University of South Florida Scholar Commons Graduate Theses and Dissertations Graduate School 11-9-2017 Synthesis, Characterization, and Application of Molybdenum Oxide Nanomaterials Michael S. McCrory University of South Florida, [email protected] Follow this and additional works at: https://scholarcommons.usf.edu/etd Part of the Mechanical Engineering Commons Scholar Commons Citation McCrory, Michael S., "Synthesis, Characterization, and Application of Molybdenum Oxide Nanomaterials" (2017). Graduate Theses and Dissertations. https://scholarcommons.usf.edu/etd/7424 This Dissertation is brought to you for free and open access by the Graduate School at Scholar Commons. It has been accepted for inclusion in Graduate Theses and Dissertations by an authorized administrator of Scholar Commons. For more information, please contact [email protected]. Synthesis, Characterization, and Application of Molybdenum Oxide Nanomaterials by Michael S. McCrory A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy Department of Mechanical Engineering College of Engineering University of South Florida Co-Major Professor: Ashok Kumar, Ph.D. Co-Major Professor: Manoj K. Ram, Ph.D. Daniel Hess, Ph.D. Sylvia Thomas, Ph.D. Sagar Pandit, Ph.D. Date of Approval: November 2, 2017 Keywords: Battery, Decontamination, Photocatalyst, Adsorbent, Methylene Blue Copyright © 2017, Michael S. McCrory DEDICATION I’d like to dedicate this work to grandma, Janet, and my parents, Gail and James. Thank you for everything; the love, support, encouragement, etc. I’d also like to dedicate this work to my soon-to-be wife, Courtney. Words just cannot describe my feelings here, so I’ll simply say thank you for everything and I love you. ACKNOWLEDGMENTS I would like to thank Dr. Ashok Kumar for his support throughout my time at USF. I would also like to thank Dr. Manoj Ram for all of his support and guidance; he worked countless hours with me (and other students), and without him I surely would not be graduating. I’d like to thank all of the committee members, Dr. Daniel Hess, Dr. Sylvia Thomas, and Dr. Sagar Pandit for taking time out of their busy schedules to be on my defense committee. I owe a special thanks to Dr. Hess for all of his support over the past 4+ years. It was an absolute pleasure and honor to work for him. I’d also like to thank my defense chair, Dr. Arash Takshi, for not only taking time to be here, but leading me through the final presentation I will make as a student at USF. I’d like to thank Dr. Rajiv Dubey, department chair, and Dr. Rasim Guldiken, graduate advisor, for their continued advice and support throughout my time here at USF, including allowing me to TA for all of these years. I’d like to thank Dr. Jose Zayas-Castro, and the rest of the College of Engineering, for their support over the years. I’d also like to thank Robert Tutfs, Jay Bieber, Richard Everly and Yusuf Emirov for all of their support and guidance in learning the characterization equipment in NREC. Finally I’d like to thank all of my lab mates (current and former). We always had some great discussions, both educational and personal. You guys were great, and I wish you all the best in your future endeavors. TABLE OF CONTENTS LIST OF TABLES ......................................................................................................................... iii LIST OF FIGURES ....................................................................................................................... iv ABSTRACT .................................................................................................................................. vii CHAPTER 1: INTRODUCTION ....................................................................................................1 1.1 Problem Description and Motivation .............................................................................1 1.2 Organization of the Dissertation ....................................................................................2 CHAPTER 2: LITERATURE REVIEW .........................................................................................4 2.1 Introduction ....................................................................................................................4 2.2 Use of MoO2 in the Decontamination of Water.............................................................4 2.3 Use of MoO2 in Li-Ion Batteries ....................................................................................8 2.4 Conclusion ...................................................................................................................19 CHAPTER 3: SYNTHESIS AND CHARACTERIZATION OF MoO2 NANOPARTICLES AND THEIR ABILITY TO DECONTAMINATE WATER ..................................................21 3.1 Introduction ..................................................................................................................21 3.2 Experimental ................................................................................................................21 3.2.1 Synthesis .......................................................................................................21 3.2.1.1 Synthesis of Nanostructured Molybdenum Trioxide (AM-MoO3)...........................................................................22 3.2.1.2 Synthesis of Molybdenum Dioxide (MoO2) ..................................22 3.2.2 Characterization ............................................................................................23 3.2.3 Water Decontamination Setup ......................................................................23 3.3 Results and Discussion ................................................................................................24 3.3.1 Electron Microscopy .....................................................................................24 3.3.2 X-ray Diffraction (XRD) ..............................................................................27 3.3.3 Decontamination ...........................................................................................29 3.4 Conclusion ...................................................................................................................35 CHAPTER 4: MORPHOLOGY CONTROLLED SYNTHESIS OF MoO2 NANOSTRUCTURES AND THEIR ABILITY TO DECONTAMINATE WATER ............37 4.1 Introduction ..................................................................................................................37 4.2 Experimental ................................................................................................................37 4.2.1 Synthesis of Molybdenum Dioxide (MoO2) .................................................38 4.2.2 Characterization ............................................................................................38 i 4.2.3 Water Decontamination Setup ......................................................................38 4.3 Results and Discussion ................................................................................................39 4.3.1 Electron Microscopy .....................................................................................39 4.3.2 X-ray Diffraction (XRD) ..............................................................................44 4.3.3 Decontamination ...........................................................................................46 4.4 Conclusion ...................................................................................................................49 CHAPTER 5: HYDROTHERMAL SYNTHESIS OF MoO2 NANOPARTICLES DIRECTLY ONTO A COPPER SUBSTRATE AND THEIR ABILITY TO DECONTAMINATE WATER ................................................................................................50 5.1 Introduction ..................................................................................................................50 5.2 Experimental ................................................................................................................51 5.2.1 Synthesis of Molybdenum Dioxide (MoO2) onto a Copper Substrate .........51 5.2.2 Characterization ............................................................................................51 5.2.3 Water Decontamination Setup ......................................................................52 5.3 Results and Discussion ................................................................................................52 5.3.1 Scanning Electron Microscopy .....................................................................53 5.3.2 X-ray Diffraction (XRD) ..............................................................................54 5.3.3 Decontamination ...........................................................................................55 5.4 Conclusion ...................................................................................................................56 CHAPTER 6: CONCLUSION ......................................................................................................57 6.1 Future Work .................................................................................................................58 REFERENCES ..............................................................................................................................60 APPENDIX A: COPYRIGHT PERMISSIONS FOR MATERIAL USED IN CHAPTER 5 .......................................................................................................................76 APPENDIX