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Molecular Transport Properties Through Carbon Nanotube Membranes University of Kentucky UKnowledge University of Kentucky Doctoral Dissertations Graduate School 2007 MOLECULAR TRANSPORT PROPERTIES THROUGH CARBON NANOTUBE MEMBRANES Mainak Majumder University of Kentucky, [email protected] Right click to open a feedback form in a new tab to let us know how this document benefits ou.y Recommended Citation Majumder, Mainak, "MOLECULAR TRANSPORT PROPERTIES THROUGH CARBON NANOTUBE MEMBRANES" (2007). University of Kentucky Doctoral Dissertations. 557. https://uknowledge.uky.edu/gradschool_diss/557 This Dissertation is brought to you for free and open access by the Graduate School at UKnowledge. It has been accepted for inclusion in University of Kentucky Doctoral Dissertations by an authorized administrator of UKnowledge. For more information, please contact [email protected]. ABSTRACT OF DISSERTATION Mainak Majumder The Graduate School University of Kentucky 2007 MOLECULAR TRANSPORT PROPERTIES THROUGH CARBON NANOTUBE MEMBRANES ABSTRACT OF DISSERTATION A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in the College of Engineering at the University of Kentucky By Mainak Majumder Lexington, Kentucky Director: Dr. Bruce J. Hinds, William Bryan Professor of Materials Engineering Lexington, Kentucky 2007 Copyright © Mainak Majumder 2007 ABSTRACT OF DISSERTATION MOLECULAR TRANSPORT PROPERTIES THROUGH CARBON NANOTUBE MEMBRANES Molecular transport through hollow cores of crystalline carbon nanotubes (CNTs) are of considerable interest from the fundamental and application point of view. This dissertation focuses on understanding molecular transport through a membrane platform consisting of open ended CNTs with ~ 7 nm core diameter and ~ 1010 CNTs/cm2 encapsulated in an inert polymer matrix. While ionic diffusion through the membrane is close to bulk diffusion expectations, gases and liquids were respectively observed to be transported ~ 10 times faster than Knudsen diffusion and ~ 10000-100000 times faster than hydrodynamic flow predictions. This phenomenon has been attributed to the non-interactive and frictionless graphitic interface. Functionalization of the CNT tips was observed to change selectivity and flux through the CNT membranes with analogy to ‘gate-keeper’ functionality in biological membranes. An electro-chemical diazonium grafting chemistry was utilized for enhancing the functional density on the CNT membranes. A strategy to confine the reactions at the CNT tips by a fast flowing liquid column was also designed. Characterization using electrochemical impedance spectroscopy and dye assay indicated ~ 5-6 times increase in functional density. Electrochemical impedance spectroscopy experiments on CNT membrane/electrode functionalized with charged macro-molecules showed voltage-controlled conformational change. Similar chemistry has been applied for realizing ‘voltage-gated’ transport channels with potential application in trans-dermal drug delivery. Electrically-facilitated transport ( a geometry in which an electric field gradient acts across the membrane) through the CNT and functionalized CNT membranes was observed to be electrosmotically controlled. Finally, a simulation framework based on continuum electrostatics and finite elements has been developed to further the understanding of transport through the CNT membranes. KEYWORDS: carbon nanotube membrane, nano-scale hydrodynamics, diazonium grafting, voltage- gated membrane, finite element analysis Mainak Majumder Date: 12th November, 2007 MOLECULAR TRANSPORT PROPERTIES THROUGH CARBON NANOTUBE MEMBRANE By Mainak Majumder Dr. Bruce J. Hinds Director of Dissertation Dr. Douglass Kalika Director of Graduate Studies 12th November, 2007 RULES FOR THE USE OF DISSERTATIONS Unpublished dissertations submitted for the Doctor's degree and deposited in the University of Kentucky Library are as a rule open for inspection, but are to be used only with due regard to the rights of the authors. Bibliographical references may be noted, but quotations or summaries of parts may be published only with the permission of the author, and with the usual scholarly acknowledgements. Extensive copying or publication of the dissertation in whole or in part also requires the consent of the Dean of the Graduate School of the University of Kentucky. A library that borrows this dissertation for use by its patrons is expected to secure the signature of each user. Name Date p p p p p p p p p p p DISSERTATION Mainak Majumder The Graduate School University of Kentucky 2007 MOLECULAR TRANSPORT PROPERTIES THROUGH CARBON NANOTUBE MEMBRANE DISSERTATION A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in the College of Engineering at the University of Kentucky By Mainak Majumder Lexington, Kentucky Director: Dr.Bruce J. Hinds, William Bryan Professor of Materials Engineering Lexington, Kentucky 2007 Copyright © Mainak Majumder 2007 Dedicated to my grand-father,‘dada’, who guided and inspired me during my formative years. He passed away on 25th July 2007, after a prolonged battle with Alzheimer’s disease. ACKNOWLEDGEMENTS First and foremost, I am indebted to my advisor, Professor Bruce J. Hinds, for his guidance, enthusiasm and excellent problem selection. I gratefully acknowledge the funding provided by the National Science Foundation (NSF), National Institutes of Health (NIH), ARO Advanced Carbon Nanotechnology Program and the dissertation year fellowship from the University of Kentucky. I also acknowledge Central Glass and Ceramic Research Institute, a CSIR laboratory in Kolkata, India for allowing me a leave of absence for the first two years of my Ph.D. studies. I thank Dr. Nitin Chopra, a former graduate student of our laboratory for realizing the synthesis of the CNT membranes, without which this dissertation would not have reached the present form. Other collaborators from our laboratory include Xin Zhan, Dr. Karin Keis and Xin Su. Dr. Karin Keis was particularly involved in much of the electrochemistry work discussed in Chapter 5. Undergraduate students who helped me were Corey Meadows, Jeggan Cole and Wendy Satterwhite. A person very special to my academic growth and support at the University of Kentucky is Professor Dibakar Bhattacharrya (Department of Chemical Engineering). In fact, he was responsible for recruiting me to this university and has been a strong mentor. Members of the Bachas lab (Chemistry Department, University of Kentucky), Dr. Vasilis Gavalas, Dr. Pramod Nednoor, and Professor Leonidas Bachas, are acknowledged for some very fruitful discussions. Professor Audra Stinchomb at the Department of Pharmacy, University of Kentucky, is acknowledged for some preliminary drug diffusion studies through functionalized carbon nanotube membranes. My collaborators from the Center for Applied Energy Research, Drs. Rodney Andrews and Dali Qian, are also credited for supplying the aligned carbon nanotube samples. iii My sincere thanks to Bing Hu, who often helped me in Scanning Electron Microscopy experiments and obtaining clear and beautiful pictures of the nanotubes or membranes; Professor Steven Rankin (Chemical Engineering, University of Kentucky) for using the FTIR Spectrometer (Chapter 4); Professor Todd Hastings (Electrical Engineering, University of Kentucky) for the use of EIS simulation software (Chapter 5); and Professor Pinar Menguic (Mechanical Engineering, University of Kentucky) and members of his laboratory for allowing me to use the finite element software FEMLAB (Chapter 7). The infrastructure provided by the Department of Chemical and Materials Engineering and the Center for Nano-scale Science and Engineering at the University of Kentucky is beneficial for undertaking cutting edge research and is, therefore, acknowledged. There are many friends, including Kaustav Ghosh, Dr. Sumod Kalakkunath, Dr. Venkat Koganti., Pawan Tyagi, and Saurav Dutta, who made my stay in Lexington a memorable one. My mother has been a tower of strength, braving every crisis that came my way. Her faith and devotion have strengthened me and made me what I am today. My wife, Amrita, has not only provided me emotional support, but also brought structure and enrichment to my life. iv TABLE OF CONTENTS Acknowledgements . iii Table of Contents . v List of Tables . ix List of Figures . xi Preview . xx Chapter 1: Introduction . 1 1.1 Discovery of Fullerene and Carbon Nanotubes . 1 1.2 Carbon Nanotubes as Nano-scale Containers or Mass Transport Channels . 4 1.3 Synthesis of Aligned Carbon Nanotube Structures . 7 1.4 Vertically Aligned and Ordered Membranes . 9 1.4.1 What are membranes? . 9 1.4.2 Anodization of Aluminium . 10 1.4.3 Track-etch Membranes . 12 1.4.4 Template Synthesis Approach . 14 1.4.5 Fabrication of Vertically Aligned Carbon Nanotube Membrane 15 1.5 Goals of the Dissertation . 18 Chapter 2: Experimental Methods . 20 2.1 Synthesis of CNT Membranes. 20 2.2. Ionic Transport Measurements. 20 2.3. Electrochemical Impedance Sectroscopy Measurements. 23 2.4. Liquid Transport Measurements . 23 2.5 Gas Transport Measurement . 25 2.6.KCl Diffusion Experiments for Estimation of Porosity . 27 2.7 Functionalization of CNT Membranes . 28 2.8 FTIR Studies . 30 2.9 U-tube Permeation Experiment. 30 2.10 Synthesis of 4-carboxy phenyl diazonium tetra fluoroborate . 32 2.11 Electrochemical Grafting. 32 v 2.12 Dye Adsorption-Desorption Assay . 34 2.13 Functionalization of CNT Membrane/Electrodes. 36 2.14 Estimation of Porosity of Membranes from Methyl Viologen flux . 39
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