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Assisted Development of Mesophase Pitch with Dispersed Graphene and Its Resulting Carbon Fibers

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Assisted Development of Mesophase Pitch with Dispersed Graphene and Its Resulting Carbon Fibers University of Kentucky UKnowledge Theses and Dissertations--Mechanical Engineering Mechanical Engineering 2018 ASSISTED DEVELOPMENT OF MESOPHASE PITCH WITH DISPERSED GRAPHENE AND ITS RESULTING CARBON FIBERS Aaron Owen University of Kentucky, [email protected] Author ORCID Identifier: https://orcid.org/0000-0003-0858-3151 Digital Object Identifier: https://doi.org/10.13023/etd.2018.454 Right click to open a feedback form in a new tab to let us know how this document benefits ou.y Recommended Citation Owen, Aaron, "ASSISTED DEVELOPMENT OF MESOPHASE PITCH WITH DISPERSED GRAPHENE AND ITS RESULTING CARBON FIBERS" (2018). Theses and Dissertations--Mechanical Engineering. 126. https://uknowledge.uky.edu/me_etds/126 This Master's Thesis is brought to you for free and open access by the Mechanical Engineering at UKnowledge. It has been accepted for inclusion in Theses and Dissertations--Mechanical Engineering by an authorized administrator of UKnowledge. For more information, please contact [email protected]. STUDENT AGREEMENT: I represent that my thesis or dissertation and abstract are my original work. Proper attribution has been given to all outside sources. I understand that I am solely responsible for obtaining any needed copyright permissions. I have obtained needed written permission statement(s) from the owner(s) of each third-party copyrighted matter to be included in my work, allowing electronic distribution (if such use is not permitted by the fair use doctrine) which will be submitted to UKnowledge as Additional File. I hereby grant to The University of Kentucky and its agents the irrevocable, non-exclusive, and royalty-free license to archive and make accessible my work in whole or in part in all forms of media, now or hereafter known. I agree that the document mentioned above may be made available immediately for worldwide access unless an embargo applies. I retain all other ownership rights to the copyright of my work. I also retain the right to use in future works (such as articles or books) all or part of my work. I understand that I am free to register the copyright to my work. REVIEW, APPROVAL AND ACCEPTANCE The document mentioned above has been reviewed and accepted by the student’s advisor, on behalf of the advisory committee, and by the Director of Graduate Studies (DGS), on behalf of the program; we verify that this is the final, approved version of the student’s thesis including all changes required by the advisory committee. The undersigned agree to abide by the statements above. Aaron Owen, Student Dr. Rodney Andrews, Major Professor Dr. Alexandre Martin, Director of Graduate Studies ASSISTED DEVELOPMENT OF MESOPHASE PITCH WITH DISPERSED GRAPHENE AND ITS RESULTING CARBON FIBERS THESIS A thesis submitted in partial fulfillment of the requirements for the degree of Master of Science in Mechanical Engineering in the College of Engineering at the University of Kentucky By Aaron Owen Lexington, Ky Director: Dr. Rodney Andrews, Professor of Mechanical Engineering Copyright © Aaron Owen 2018 https://orcid.org/0000-0003-0858-3151 ABSTRACT OF THESIS ASSISTED DEVELOPMENT OF MESOPHASE PITCH WITH DISPERSED GRAPHENE AND ITS RESULTING CARBON FIBERS The efficacy of dispersed reduced graphene oxide (rGO) as a nucleation site for the growth of mesophase in an isotropic pitch was investigated and quantified in this study. Concentrations of rGO were systematically tested in an isotropic petroleum and coal-tar pitch during thermal treatments and compared to pitch without rGO. The mesophase content of each thermally treated pitch was quantified by polarized light point counting. Further characterization of softening temperature and insolubles were quantified. Additionally, the pitches with and without rGO were melt spun, graphitized, and tensile tested to determine the effects of rGO on graphitized fiber mechanical properties and fiber morphology. KEYWORDS: Mesophase, Reduced graphene oxide, Melt spinning, Carbon fiber Aaron Owen December 5, 2018 Date ASSISTED DEVELOPMENT OF MESOPHASE PITCH WITH DISPERSED GRAPHENE AND ITS RESULTING CARBON FIBERS By Aaron Owen Dr. Rodney Andrews Director of Thesis Dr. Alexandre Martin Director of Graduate Studies December 5, 2018 Date ACKNOWLEDGMENTS Thank you to my patient wife who has graciously dealt with my long days and late nights throughout this process. Also, thank you to everyone in the Carbon Group at CAER that helped guide me along to be a better engineer and scientist and dealt with my constant barrage of questions. Lastly, thank you to my advisor, Rodney Andrews and co-advisor Matt Weisenberger for taking the time to guide me in my research and thesis work. iii TABLE OF CONTENTS ACKNOWLEDGMENTS ................................................................................................. iii TABLE OF CONTENTS ................................................................................................... iv LIST OF TABLES ............................................................................................................ vii LIST OF FIGURES ........................................................................................................... ix Chapter 1. BACKGROUND ...........................................................................................1 1.1 Introduction ............................................................................................................... 1 1.2 History of Pitch ......................................................................................................... 4 1.3 Petroleum Pitch Origin ............................................................................................. 6 1.4 Coal-tar Pitch Origin ................................................................................................. 7 1.5 Isotropic and Mesophase ........................................................................................ 10 1.6 Previous Pitch Improvement Methods .................................................................... 16 1.7 Fiber Processing ...................................................................................................... 18 1.7.1 Melt Spinning............................................................................................... 18 1.7.2 Oxidation...................................................................................................... 24 1.7.3 Carbonization and Graphitization ................................................................ 24 1.8 Conclusion .............................................................................................................. 27 Chapter 2. GRAPHENE AS A SEED CRYSTAL FOR MESOPHASE DEVELOPMENT ..............................................................................................................29 2.1 Introduction ............................................................................................................. 29 2.2 Experimental Materials and Methods ..................................................................... 30 2.2.1 Materials ...................................................................................................... 30 2.2.2 Experimental Methods ................................................................................. 30 2.2.3 Temperature Control .................................................................................... 33 iv 2.2.3 Heat Treatment............................................................................................. 34 2.2.4 Insoluble Testing .......................................................................................... 35 2.2.5 Dynamic Mechanical Analysis (DMA) ....................................................... 36 2.2.6 Polarized Light Microscopy ......................................................................... 37 2.3 Results ..................................................................................................................... 39 2.3.1 Petroleum Pitch ............................................................................................ 39 2.3.2 Coal-tar Pitch ............................................................................................... 49 2.3.3 Observations During Heat Treatments......................................................... 57 2.2.5 Milled Mitsubishi and THF Insolubles ........................................................ 58 2.4 Conclusion .............................................................................................................. 59 Chapter 3. MELT SPINNING .......................................................................................61 3.1 Introduction ............................................................................................................. 61 3.1.1 Wayne Extruder (WEXT) Spinning ............................................................. 63 3.1.2 Pressure Spinning Capsule ........................................................................... 67 3.1.3 Melt Pool Spinning ...................................................................................... 71 3.1.4 Lessons Learned........................................................................................... 72 3.2 Method .................................................................................................................... 73 3.3 Results ..................................................................................................................... 74 3.4 Conclusion .............................................................................................................
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