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High Yield Solvothermal Synthesis of Hexaniobate Based Nanocomposites Via the Capture of Preformed Nanoparticles in Scrolled Nanosheets

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High Yield Solvothermal Synthesis of Hexaniobate Based Nanocomposites Via the Capture of Preformed Nanoparticles in Scrolled Nanosheets University of New Orleans ScholarWorks@UNO University of New Orleans Theses and Dissertations Dissertations and Theses Fall 12-20-2013 High Yield Solvothermal Synthesis of Hexaniobate Based Nanocomposites via the Capture of Preformed Nanoparticles in Scrolled Nanosheets Shivaprasad Reddy Adireddy University of New Orleans, [email protected] Follow this and additional works at: https://scholarworks.uno.edu/td Part of the Inorganic Chemistry Commons, and the Materials Chemistry Commons Recommended Citation Adireddy, Shivaprasad Reddy, "High Yield Solvothermal Synthesis of Hexaniobate Based Nanocomposites via the Capture of Preformed Nanoparticles in Scrolled Nanosheets" (2013). University of New Orleans Theses and Dissertations. 1726. https://scholarworks.uno.edu/td/1726 This Dissertation-Restricted is protected by copyright and/or related rights. It has been brought to you by ScholarWorks@UNO with permission from the rights-holder(s). You are free to use this Dissertation-Restricted in any way that is permitted by the copyright and related rights legislation that applies to your use. For other uses you need to obtain permission from the rights-holder(s) directly, unless additional rights are indicated by a Creative Commons license in the record and/or on the work itself. This Dissertation-Restricted has been accepted for inclusion in University of New Orleans Theses and Dissertations by an authorized administrator of ScholarWorks@UNO. For more information, please contact [email protected]. High Yield Solvothermal Synthesis of Hexaniobate Based Nanocomposites via the Capture of Preformed Nanoparticles in Scrolled Nanosheets A Dissertation Submitted to the Graduate Faculty of the University of New Orleans in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Chemistry By Shivaprasad Reddy Adireddy B.S. Osmania University, 2005 M.S. University of New Orleans, 2011 Copyright 2012, Shivaprasad Reddy Adireddy ii To The People Who Make This World A Better Place iii Acknowledgements Along the journey of my Ph.D. I have been helped by several people. First I wish to express my deep gratitude and sincere thank you to my research advisor Professor John B. Wiley for his cooperation, constructive criticism, encouragement and valuable guidance during the course of my study. After joining the group, I always received enormous amount of help from my adviser in choosing my project and setting up my work space. I am truly grateful for his keen interest, responsive action, remarkable feedback and extreme support throughout the course of my research. I also would like to thank my dissertation committee members, Prof. Mathew Tarr, Prof. Leszek Malkinski, and Prof. Steven Rick, for helpful discussions and suggestions. I am also thankful to each and every member of Department of Chemistry and Advanced Materials Research Institute for their help and support throughout my PhD. They are also acknowledged for providing an academically stimulating environment in the department. I am thankful to my present and past group members, namely Dr. Yuan Yao, Dr. Elisha Josepha, Dr. Debasish Mohanty, Dr. Girija S. Chaubey, Mohammad Montasserasadi, Jagnyaseni Tripathy, Lea Gustin, Cecilia Carbo, Taha Rostamzade, Treva Brown, Mayra Franco and Sara Tefaghi. I remember all the great moments that I had with my group members, I am thankful for their time, and great friendship. It was an honor and great pleasure to be a part of the Wiley group. The project work would not have been possible without the friendly support and timely help of my colleagues and friends, especially Prof. Leonard Spinu, Dr. Jose Vargas, Dr. Avijit Biswas, Dr. Jiajun Chen, Dr. Kai Wang, Dr. Bao Bao Cao, Sarah Wozny, Pramathesh Maji, Sanjeeva Dodlapati, Abhishek Srivastava, Satish Rai, Sudhendu Azad, Pinkesh Attarwala, iv Sravan Burla, Vempati Satheesh, Deepak Mudili, Thilo Buck, Curt Click, Vijay Burla, Rupal Shah, Jenny Martin, Aubrie Pfirman, Jugal Shah, Thilo Buck, Rajesh Komatineni, Meet Singh, Rupa Biradar, and Sandeep Bandi. I also want to thank my grandparents, family friends and relatives for their wishes, blessings, and help; and last, but not least, my parents, for their endless love, support, and encouragement. Financial support from the Louisiana Board of Regents Post-Katrina Support Fund Initiative (PKSFI) is gratefully acknowledged. v Table of Contents List of Figures .................................................................................................................. viii List of Tables ................................................................................................................... xiii Abstract ............................................................................................................................ xiv Chapter 1 Introduction........................................................................................................1 1.1 Nanotechnology ....................................................................................................1 1.2 Nanomaterials .......................................................................................................2 1.2.1 Zero-Dimensional (OD) Nanostructures...............................................6 1.2.2 One-Dimensional (1D) Nanostructures ..............................................16 1.3 Layered Inorganic Materials ...............................................................................19 1.3.1 K4Nb6O17.............................................................................................22 1.3.2 Hexaniobate Based Nanocomposites ..................................................25 1.3.3 Peapods ...............................................................................................27 1.4 References ...........................................................................................................29 Chapter 2 Rapid Large-scale Fabrication of Hexaniobate Nanoscrolls ...........................41 2.1 Introduction .........................................................................................................41 2.2 Experimental .......................................................................................................43 2.2.1 Preparation of Niobate Nanoscrolls ....................................................44 2.2.2 Characterization ..................................................................................45 2.3 Results .................................................................................................................46 2.3.1 Solvothermal Synthesis .......................................................................47 2.3.2 Factors Influencing Nanoscroll Formation and Architecture .............51 2.3.3 Other Intercalants ................................................................................54 2.3.4 Dispersion in Different Solvents .........................................................56 2.3.5 Bulk and Surface Characterization .....................................................57 2.4 Discussion ...........................................................................................................61 2.5 Conclusions .........................................................................................................65 2.6 References ...........................................................................................................66 Chapter 3 High Yield Solvothermal Synthesis of Magnetic Peapod Nanocomposites via the Capture of Preformed Nanoparticles in Scrolled Nanosheets .............71 3.1 Introduction .........................................................................................................71 3.2 Experimental .......................................................................................................73 3.2.1 Niobate Nanosheets ............................................................................73 3.2.2 Magnetic Nanoparticle Synthesis .......................................................74 3.2.3 Synthesis of Magnetic NP@hexaniobate Nanopeapods .....................75 3.2.4 Characterization ..................................................................................76 3.3 Results .................................................................................................................76 3.4 Discussion ...........................................................................................................88 3.5 Conclusions .........................................................................................................93 3.6 References ...........................................................................................................93 vi Chapter 4 A General Method for the Fabrication of Hexaniobate-Based Nanocomposites .............................................................................................101 4.1 Introduction .......................................................................................................101 4.2 Experimental .....................................................................................................103 4.2.1 Niobate Nanosheets ..........................................................................104 4.2.2 Nanoparticles ....................................................................................105 4.2.3 Synthesis of Nanopeapods with Various NPs ...................................107 4.2.4 Modification of Nanosheets and Nanoscrolls ...................................107 4.2.5 Gold Insertion into
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