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2-DIMENSIONAL INTERCALATED CYANO-METALLATE COMPLEXES- APPROACH to ULTRAFILTRATION by Babatunde Mattew Adebiyi, B.S., M.S. a Diss

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2-DIMENSIONAL INTERCALATED CYANO-METALLATE COMPLEXES- APPROACH TO ULTRAFILTRATION by Babatunde Mattew Adebiyi, B.S., M.S. A dissertation submitted to the Graduate Council of Texas State University in partial fulfillment of the requirements for the degree of Doctor of Philosophy with a Major in Material Science, Engineering, and Commercialization May 2019 Committee Members: Gary W. Beall, Chair Kevin Lewis Benjamin R. Martin William Chittenden Alex Zakhidov COPYRIGHT by Babatunde Mattew Adebiyi 2019 FAIR USE AND AUTHOR’S PERMISSION STATEMENT Fair Use This work is protected by the Copyright Laws of the United States (Public Law 94-553, section 107). Consistent with fair use as defined in the Copyright Laws, brief quotations from this material are allowed with proper acknowledgement. Use of this material for financial gain without the author’s express written permission is not allowed. Duplication Permission As the copyright holder of this work I, Babatunde Mattew Adebiyi, authorize duplication of this work, in whole or in part, for educational or scholarly purposes only. DEDICATION I dedicate this work to my late cousin, Segun Ogunleye, rest on. ACKNOWLEDGEMENTS I would like to thank my advisor, Dr. Gary Beall for his guidance and relentless effort and input in making sure the research is completed. I would like to thank Dr. Clois Powel (Rtd) for his insights, Dr. Ben Martin and my dissertation committee members for their inputs and positive criticism that brought me up to speed. To Dr. Shazly and Dr. Michael Opoku for their assistance in proffering solutions to my several questions. I would like to thank my wife, Victoria for her support and understanding during my program. I would also like to appreciate my parents and my sisters; Keji, Funmilola, Taiwo and Kehinde Adebiyi for believing in me and for their prayers and patience without which I will not be able to achieve this feat. To my friends Mr. and Mrs. Olanrewaju Ogedengbe, and Mr. and Mrs. Bolaji Adesanya, I say a big Thank you. The financial support for this work by Graduate School Fellowship and MSEC program is highly appreciated. v TABLE OF CONTENTS Page ACKNOWLEDGEMENTS ............................................................................................... .vvi LIST OF TABLES………………………………………………………………………..ix LIST OF FIGURES .............................................................................................................x ABSTRACT .......................................................................................................................xv CHAPTER 1. INTRODUCTION ...........................................................................................................1 1.1 Background .......................................................................................................... 1 1.2 Review of The Literature ..................................................................................... 3 1.2.1 Nature of Transition Metal in 3D Metal Framework .................................... 3 1.2.2 Fe, Ni, Mn and Co Transition Metal ............................................................. 4 1.2.3 Preceding Background Work ........................................................................ 6 1.2.4 Potential Applications ................................................................................. 14 1.3 Dissertation Effort and Research Objectives ..................................................... 16 2. EXPERIMENTAL METHODS.....................................................................................19 2.1 Preparation of Divalent Transition Metal Powder Complexes .......................... 19 2.1.1 Treatment of samples with DDP ................................................................. 21 2.1.2 Preparation of Powder Complex for SEM Imaging .................................... 21 2.1.3 X-Ray Diffraction Analysis ........................................................................ 22 2.1.4 Thermo Graph Analysis .............................................................................. 22 2.1.5 Raman Scattering ........................................................................................ 22 2.1.6 Transmission Electron Microscopy ............................................................ 22 2.1.7 Vibrating Sample Magnetometry ................................................................ 23 2.2. Divalent Transition Metal Growth Method on Microporous Membranes ......... 23 2.2.1 Na Ion Selectivity ....................................................................................... 26 3. RESULTS AND DISCUSSIONS ..................................................................................30 3.1 FeNi(CN)4 and Derivative .................................................................................. 30 3.1.1 X-Ray Diffraction ....................................................................................... 30 vi 3.1.2 SEM and EDAX for Fe Transition Metal Complex ................................... 33 3.1.3 TEM Imaging for the Fe Transition Metal Complex .................................. 36 3.1.4 Raman Scattering for Fe Transition Metal Complex .................................. 40 3.1.5 TGA for Fe Transition Metal Complex ...................................................... 42 3.1.6 VSM for Fe Transition Metal Complex ...................................................... 43 3.2 MnNi(CN)4 and Derivative ................................................................................ 44 3.2.1 X-Ray Diffraction ....................................................................................... 44 3.2.2 SEM and EDAX for Mn Transition Metal Complex .................................. 45 3.2.3 TEM Imaging for Mn Transition Metal Complex ...................................... 47 3.2.4 Raman Scattering for Mn Transition Metal Complex ................................ 52 3.2.5 TGA for Mn Transition Metal Complex ..................................................... 53 3.2.6 VSM for Mn Transition Metal Complex .................................................... 54 3.3 Ni2(CN)4 and Derivative .................................................................................... 55 3.3.1 X-Ray Diffraction ....................................................................................... 55 3.3.2 SEM and EDAX for Ni Transition Metal Complex ................................... 56 3.3.3 TEM Imaging for Ni Transition Metal Complex ........................................ 58 3.3.4 Raman Scattering for Ni Transition Metal Complex .................................. 61 3.3.5 TGA for Ni Transition Metal Complex ...................................................... 62 3.3.6 VSM for Ni Transition Metal Complex ...................................................... 63 3.4 CoNi(CN)4 and Derivative ................................................................................. 64 3.4.1 X-Ray Diffraction ....................................................................................... 65 3.4.2 SEM and EDAX for Co Transition Metal Complex ................................... 66 3.4.3 TEM Imaging for Co Transition Metal Complex ....................................... 67 3.4.4 Raman Scattering for Co Transition Metal complex .................................. 71 3.4.5 TGA for Co Transition Metal Complex...................................................... 72 3.4.6 VSM for Co Transition Metal Complex ..................................................... 72 3.5 Filtration Results of Transition Metal Complex on Microporous Fiber ............ 73 3.6 BET Surface Area Results and Analysis ............................................................ 78 4. RECOMMENDATION AND CONCLUSION .............................................................79 4.1 Recommendation for Future Work .................................................................... 79 4.2 Conclusions ........................................................................................................ 79 5. SYNTHESIS OF NICKEL FERRITE-GRAPHITIC LAYERS NANOCOMPOSITE WITH INVERTED MAGNETIC HYSTERESIS .............................................................82 5.1 Introduction ........................................................................................................ 82 5.2 Experimental work ............................................................................................. 83 5.3 Characterizations ................................................................................................ 83 5.4 Results and Discussions ..................................................................................... 84 vii 5.4.1 X-ray Diffraction ........................................................................................ 84 5.4.2 Scanning Electron Microscopy ................................................................... 85 5.4.3 Transmission Electron Microscopy ............................................................ 86 5.4.4 Raman Spectroscopy ................................................................................... 87 5.4.5 Magnetic Properties .................................................................................... 88 5.5 Proposed Mechanism of Nickel Ferrite Formation ............................................ 90 5.5.1 Conclusions ........................................................................................................ 92 APPENDIX SECTION ......................................................................................................94
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