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NANOPOROUS Sio2/VYCOR MEMBRANES for AIR SEPARATION

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NANOPOROUS Sio2/VYCOR MEMBRANES for AIR SEPARATION Copyright Warning & Restrictions The copyright law of the United States (Title 17, United States Code) governs the making of photocopies or other reproductions of copyrighted material. Under certain conditions specified in the law, libraries and archives are authorized to furnish a photocopy or other reproduction. One of these specified conditions is that the photocopy or reproduction is not to be “used for any purpose other than private study, scholarship, or research.” If a, user makes a request for, or later uses, a photocopy or reproduction for purposes in excess of “fair use” that user may be liable for copyright infringement, This institution reserves the right to refuse to accept a copying order if, in its judgment, fulfillment of the order would involve violation of copyright law. Please Note: The author retains the copyright while the New Jersey Institute of Technology reserves the right to distribute this thesis or dissertation Printing note: If you do not wish to print this page, then select “Pages from: first page # to: last page #” on the print dialog screen The Van Houten library has removed some of the personal information and all signatures from the approval page and biographical sketches of theses and dissertations in order to protect the identity of NJIT graduates and faculty. ABSTRACT NANOPOROUS SiO2/VYCOR MEMBRANES FOR AIR SEPARATION by Mihir Tungare Porous Vycor tubes with 40Å initial pore diameter were modified using low pressure chemical vapor deposition (LPCVD) of silicon dioxide (Si0 2). Diethylsilane (DES) in conjunction with nitrous oxide (N20) was used as a precursor to synthesize these SiO 2 films. The aim of this study was to obtain a considerable selectivity between species of comparable size and hence N20 was used. The use of N20 was believed to make the process self-limiting. DES was allowed to flow through the tube and N20 on the outside in the chamber at 550°C in a counter-flow mechanism. This deposition geometry provided an optimum pore narrowing rate and eliminated the possibility of film cracking. The pore size of the Vycor tube was reduced with successive depositions and the stage at which maximum selectivity between oxygen and nitrogen was obtained was recorded. The value of selectivity was confirmed using mass spectroscopy and reproducing the results using another Vycor tube. The temperature dependence on selectivity was also studied. Characterization of the Vycor membranes was carried out to observe the Si02 coating. Calculation of permeability was done using ASTM standards. NANOPOROUS SiO2/VYCOR MEMBRANES FOR AIR SEPARATION by Mihir Tungare A Thesis Submitted to the Faculty of New Jersey Institute of Technology in Partial Fulfillment of the Requirements for the Degree of Master of Science in Materials Science and Engineering Interdisciplinary Program in Materials Science and Engineering August 2000 APPROVAL PAGE NANOPOROUS SiO2/VYCOR MEMBRANES FOR AIR SEPARATION Mihir Tungare Dr. Roland A. Levy, Thesis Advisor Date Distinguished Professor of Physics, NJIT Dr. James M. Grow, Committee Member Date Professor of Chemical Engineering, Chemistry, and Environmental Science, NJIT Dr. Trevor A. Tyson, Committee Member Date Assistant Professor of Physics, NJIT BIOGRAPHICAL SKETCH Author: Mihir Tungare Degree: Master of Science in Materials Science and Engineering Date: August 2000 Undergraduate and Graduate Education: • Master of Science in Materials Science and Engineering, New Jersey Institute of Technology, Newark, NJ, 2000 • Bachelor of Engineering in Metallurgy, Govt. College of Engineering, Pune, India, 1999 Major: Materials Science and Engineering iv To my parents, Mama and Baba, and my brother, Subeer v ACKNOWLEDGMENT I would like to express my sincerest gratitude to Dr. Roland A. Levy, for his advice, guidance, and encouragement. Those hard pats on my back surely boosted my confidence. His knowledge and experience helped me deal with various problems in the CVD research lab. I am thankful to Dr. James M. Grow and Dr. Trevor A. Tyson for reviewing my thesis and providing me with some enlightening discussions. Special thanks to Dr. Peter C. Foller and PPG industries for discussing their concerns and having faith in me. Their valuable comments were of great help. I am grateful to Dr. Date for encouraging me in pursuing a higher degree and for all those cheers and good wishes. I would like to express my appreciation to my CVD lab-mates Narahari Ramanuja and Dian Hong Luo for their support, helpful discussions and companionship. The jokes and humor filled conversations helped ease the burden of work and academics. I thank Narahari, my lab partner, in guiding me during the initial stages of my research and wish him luck as he steps into his future at Intel. Thanks to Kenneth J. O'Brien for his technical assistance with equipment and his entertaining conversations. I am also grateful to my friends Anto, Bhavin, Lim, Yew Fong, Kunal, Animesh, Tushar, Nimish, Chetan, Ravinder, Pawan, and many others who were always there when I needed them. I thank Mama, Baba, Subeer, Aba, Nanchi, and Shonu for their love and that long-distance support and inspiration. I am grateful to Sandhya aunty and Ashok uncle for all the help they provided. ...and to all whom I failed to mention who were instrumental for the completion of this endeavor, I express my sincerest thanks. vi TABLE OF CONTENTS Chapter Page 1 INTRODUCTION 1 1.1 Air Separation Sparks Ceramic Membrane Technology 1 1.2 Development in Ceramic Membranes 5 1.3 Ceramic Membrane Materials and Applications 6 1.4 SiO 2 as a Membrane Layer 8 1.5 Use of DES as a Precursor Gas 9 2 SYNTHESIS OF CERAMIC MEMBRANES 12 2.1 Sol-Gel Technique 13 2.2 Slip Casting 14 2.3 Acid Leaching 15 2.4 Dense Membranes 16 2.5 Track Etch Method 17 2.6 Pyrolysis 17 2.7 Thin Film Deposition Methods 18 2.7.1 Physical Vapor Deposition 19 2.7.2 Chemical Vapor Deposition 22 2.7.2.1 Overview of the Chemical Vapor Deposition Process 22 2.7.2.2 CVD Reactor Systems 23 2.7.2.3 Nucleation and Growth 25 2.7.2.4 Chemical Reactions and Kinetics 26 2.7.2.5 Transport Phenomena 26 3 MEMBRANE CHARACTERIZATION AND GAS SEPARATION MECHANISMS 28 3.1 Pore Characterization 28 vii TABLE OF CONTENTS (Continued) Chapter Page 3.1.1 Mercury Porosimetry 28 3.1.2 Nitrogen Adsorption/Desorption 29 3.1.3 Nuclear Magnetic Resonance 30 3.1.4 Permporometry 30 3.2 Characterization of the Structural Integrity of the Membrane 31 3.3 Gas Separation Mechanisms and Transport Phenomena 33 3.3.1 Gas Separation by Knudsen Diffusion 33 3.3.2 Gas Separation by Surface Diffusion 35 3.3.3 Gas Separation by Capillary Condensation 37 3.3.4 Gas Separation by Molecular Sieving 37 3.4 Entropic and Energetic Selectivity in Air Separation 39 4 EXPERIMENTAL PROCEDURE 42 4.1 Modified LPCVD Reactor 42 4.2 Si02/Vycor Membrane Fabrication 44 4.2.1 Predeposition Procedure 44 4.2.2 Si02 Deposition 45 4.3 Permeability and Selectivity Measurements 46 5 RESULTS AND DISCUSSION 47 5.1 Virgin Vycor Tube Measurements 47 5.2 Deposition of SiO 2 at 550°C 47 5.2.1 Membrane I 49 5.2.2 Membrane II 52 5.2.2.1 Characterization of Membrane II 56 viii TABLE OF CONTENTS (Continued) Chapter Page 5.3 Effect of Temperature on Permeability 59 5.4 Calculation of Permeability 62 6 CONCLUSIONS 65 REFERENCES 67 ix LIST OF TABLES Table Page 1.1 Commercial ceramic membranes 4 1.2 Properties of Silica 10 1.3 Properties of DES 11 2.1 Evaporation vs. Sputtering 21 5.1 Viscosity of Oxygen as a Function of Temperature 60 LIST OF FIGURES Figure Page 1.1 Part of ceramic membranes in market 3 2.1 Schematic showing the transport and reaction processes underlying CVD 23 2.2 LPCVD Reactor 24 3.1 Schematic of bubble point test apparatus 32 3.2 Potential energy (Er) along the permeation path of two molecules of different sizes, representing hydrogen and methane 38 4.1 LPCVD reactor for the synthesis of Si02 films on Vycor tubes 42 5.1 Plot of Permeability (across Membrane I) as a function of 1/Square root of Molecular Weight 48 5.2 Plot of Permeability as a function of 1/Square root of Molecular weight 49 5.3 Permeability as a function of Deposition time for Membrane I 50 5.4 Selectivity of Membrane I as a function of Deposition time 51 5.5 Linear dependence of dP/dt on Pressure difference for determination of Permeability for Membrane I 51 5.6 Permeability as a function of Deposition time for Membrane II 52 5.7 Selectivity of Membrane II as a function of Deposition time 53 5.8 Linear dependence of dP/dt on Pressure difference for determination of Permeability for Membrane II 53 5.9 Outgassing species within the tube 54 5.10 Gas sample from the tube with oxygen in the chamber 55 5.11 Gas sample from the tube with nitrogen in the chamber 56 5.12 Exterior surface of Vycor tube at a Magnification of 26X 57 5.13 Exterior surface of Vycor tube at a Magnification of 54X 57 xi LIST OF FIGURES (Continued) Figure Page .4 Intrr rf f r tb t Mnftn f 4 8 . Cr tn f r tb t Mnftn f 4 8 .6 Cr tn f r tb t Mnftn f 4 59 . prtr dpndn f rblt 6 x CHAPTER 1 INTRODUCTION 1.1 Air Separation Sparks Ceramic Membrane Technology Gas separation is important in processes involving oxygen enrichment, inert gas generation, air dehumidification, pollution control as well as hydrogen, helium, and hydrocarbon recovery ,2 .
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