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Tin Dioxide Nanowires and Carbon Nanotubes Portland State University PDXScholar Dissertations and Theses Dissertations and Theses Winter 2-12-2016 One-Dimensional Nanostructure and Sensing Applications: Tin Dioxide Nanowires and Carbon Nanotubes Hoang Anh Tran Portland State University Follow this and additional works at: https://pdxscholar.library.pdx.edu/open_access_etds Part of the Chemistry Commons, Materials Science and Engineering Commons, and the Nanoscience and Nanotechnology Commons Let us know how access to this document benefits ou.y Recommended Citation Tran, Hoang Anh, "One-Dimensional Nanostructure and Sensing Applications: Tin Dioxide Nanowires and Carbon Nanotubes" (2016). Dissertations and Theses. Paper 2689. https://doi.org/10.15760/etd.2685 This Dissertation is brought to you for free and open access. It has been accepted for inclusion in Dissertations and Theses by an authorized administrator of PDXScholar. Please contact us if we can make this document more accessible: [email protected]. One-Dimensional Nanostructure and Sensing Applications: Tin Dioxide Nanowires and Carbon Nanotubes by Hoang Anh Tran A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Chemistry Dissertation Committee: Shankar Rananavare, Chair Carl Wamser Albert Benight Raj Solanki Erik Sanchez James Blackwell Portland State University 2016 Abstract The key challenge for a nanomaterial based sensor is how to synthesize in bulk quantity and fabricate an actual device with insightful understanding of operational mechanisms during performance. I report here effective, controllable methods that exploit the concepts of the “green approach” to synthesize two different one-dimensional nanostructures, including tin oxide nanowires and carbon nanotubes. The syntheses are followed by product characterization and sensing device fabrications as well as sensor performance understanding at the molecular level. Sensor-analyte response and recovery kinetics are also presented. The first part of the thesis describes bulk-scale synthesis and characterization of tin oxide nanowires by the molten salt synthetic method and the nanowire doping with antimony (n-types) and lithium. The work builds on the success of using n-doped SnO2 nanoparticles to selectively detect chlorine gas at room temperature. Replacing n-doped nanoparticles with n-doped nanowires reduces the number of inter-particle electron hops between sensing electrodes. The nanowire based sensors show unprecedented 5 ppb detectability of corrosive Cl2 gas concentration in air. At the higher range, 10 ppm of Cl2 gas leads to a 250 fold increase in the device resistance. During sensor recovery, FT-IR studies show that dichlorine monoxide (Cl2O) and chlorine dioxide (ClO2) are the desorbing species. Long term stability of devices is affected by lattice oxygen vacancies replaced by chlorine atoms. Bulk-scale synthesis of multiwall carbon nanotube (MWCNTs) was achieved by a novel inexpensive synthetic method. The green chemistry method uses the non-toxic i and easy to handle solid carbon source naphthalene. The synthesis is carried out by simply heating naphthalene and organometallic precursors as catalysts in a sealed glass tube. Synthesis at 610º C leads to MWCNTs of 50 nm diameter and lengths exceeding well over microns. MWCNT doping is attempted with nitrogen (n-type) and boron (p- type) precursors. Palladium nanoparticles decorated on as-synthesized MWCNTs are employed for specific detection of explosive hydrogen gas with concentrations far below the explosive concentration limits. During performance, the sensor exhibits abnormal response behaviors at hydrogen gas concentrations higher than 1%. A model of charge carrier inversion, brought about by reduction of MWCNT by hydrogen molecules dissociated by Pd nanoparticles is proposed. ii To my beloved Dad, I miss you here on Earth. This dissertation is dedicated to you. iii Acknowledgements It gives me a pleasure to gratefully and sincerely thank my advisor, Professor S.B Rananavare. I have been extremely fortunate to have an exceptional advisor who gave me invaluable guidance, constant inspiration and continued support during my academic career at Portland State University. All that has been achieved in this thesis was made possible by him. I am also grateful to Professors Carl Wamser, Albert Benight, Raj Solanki, and Erik Sanchez for their time and invaluable inputs in my dissertation committee. I also would like to express my gratitude to Dr. James Blackwell for not only serving in my dissertation committee but also giving me a chance to work with different collaborators and sponsoring me through Intel‟s funding. I am indebted to Professor Andrea Goforth for photoluminescence analysis, Professor Andres La Rosa for the usage of the Raman system. Especially, I am thankful to Dr. Daner Abdulla for his intellectual help on Raman spectroscopy as well as uncountable advice on my thesis. Many thanks go to Dr. Joo Chan and Dr. Allen Chapadraza for the treasure of knowledge I had inherited when I was still an undergraduate student. I also would like to thank Professor Rananavare‟s research group Ryan Lerud, Srikar Rao, Kayode Morakinyo, Sayan just to mention a few, for their support and help during my PhD studies. Most importantly, none of this would have been possible without the support, love patience of my family. I would like to take this opportunity to thank my uncle Le‟s iv family, who has given me all the supports and foundation in this country. Without them I would not be the person that I am today. To my wife Leyna, I know you suffer from my imperfections and my shortcomings largely during the challenging moments. Your sweetness, your kindness, the beauty of your heart and your thoughtfulness never cease to amaze me. You are the motivation of my life. To my mom, I know I owe you everything that I am. I could not ask for a better mom than you. Thank-you mom for your patience, your wisdom and most important, your love. v Table of Contents Abstract ............................................................................................................................... i Dedication ......................................................................................................................... iii Acknowledgements ........................................................................................................... iv List of Tables .......................................................................................................................x List of Figures .................................................................................................................... xi CHAPTER 1. SENSOR BASED ON ONE DIMENSIONAL NANOMATERIALS .........1 1.1 General Introduction Nanomaterials .............................................................................1 1.2 Electronic Properties of Bulk and Nanomaterials .........................................................2 1.3 One Dimensional Nanomaterials for Sensing Applications .........................................6 1.3.1 Chlorine Sensor ..............................................................................................7 1.3.2 Hydrogen Sensor ............................................................................................9 CHAPTER 2. INSTRUMENTATION, DEVICE CHARACTERIZATION AND NANOSTRUCTURE SYNTHESIS ..................................................................................13 2.1 Synthesis and Sensor Fabrication ................................................................................13 2.1.1 Sample Preparation for SnO2 NWs ...............................................................13 2.1.2 Sample Preparation for CNTs .......................................................................15 2.2 Electron Microscopy ....................................................................................................21 2.3 Physical Vapor Deposition (PVD) ...............................................................................22 2.4 Infrared Spectroscopy (FTIR) ......................................................................................22 2.5 UV-Visible Spectroscopy (UV-Vis) ............................................................................22 2.6 Photoluminescence Spectroscopy (PL)........................................................................22 vi 2.7 Raman Spectroscopy ....................................................................................................23 2.8 Sensor Testing System .................................................................................................25 CHAPTER 3. TIN OXIDE NANOWIRES (SnO2 NWs) ................................................28 3.1 Background and Significance .....................................................................................28 3.1.1 Crystal Structure ...........................................................................................28 3.1.2 Stoichiometry, Defect Structure and Conductivity ......................................29 3.1.3 Raman Active Vibrational Modes of SnO2 Rutile Structure ........................31 3.1.4 Growth of SnO2 NWs ..................................................................................33 3.1.5 SnO2 NWs as Sensing Material ....................................................................35 3.2 Results and Discussion ................................................................................................39 3.2.1 Electron Microscopy .....................................................................................39
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