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Solid-State Potentiometric Sensors for Nitrogen Monoxide, Nitrogen Dioxide, and Carbon Monoxide

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Solid-State Potentiometric Sensors for Nitrogen Monoxide, Nitrogen Dioxide, and Carbon Monoxide SOLID-STATE POTENTIOMETRIC SENSORS FOR NITROGEN MONOXIDE, NITROGEN DIOXIDE, AND CARBON MONOXIDE By BRIGGS MCKENNEY WHITE A DISSERTATION PRESENTED TO THE GRADUATE SCHOOL OF THE UNIVERSITY OF FLORIDA IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY UNIVERSITY OF FLORIDA 2007 1 © 2007 Briggs Mckenney White 2 To My Parents 3 ACKNOWLEDGMENTS A researcher develops only if those around him and those that have passed before him are of ample quality and agreeable predisposition. I thank Vincenzo Esposito, Suman Chatterjee, and Keith Duncan, for their help, advice, and inspiration. I thank Bryan Blackburn, Martin Van Assche, and Laure Chevallier for their enthusiasm and support in the laboratory. I acknowledge the efforts of the many students in the research groups at the University of Florida and The University of Rome “Tor Vergata” for making this Ph.D. enjoyable and productive. I thank my advisor, Eric Wachsman, for the resources, motivation, recognition, advice, and responsibility that helped me to develop as a scientist and thinker. I also thank my Italian co- advisor, Enrico Traversa, for his friendship, scientific philosophy, and technical instruction. Both Eric Wachsman and Enrico Traversa afforded me with the possibility to do many great things in the laboratory and also to go learn and speak in Lindau (Germany), Quebec City (Canada), Genoa (Italy), Villa Adrianna (Italy), Los Angeles, and Cancun (Mexico). I thank my committee of Mark Orazem, Anthony Brennen, Amelia Dempere, and Daryll Butt for their scientific/technical discussions. I acknowledge the Major Analytical Instrumentation Center, the Engineering Research Center, and the Italian Center of National Research at Tor Vergata for use of the facilities. Several researchers directly assisted me by either preparing materials or executing experiments on my behalf. Sean Bishop, Eric Armstrong and Alberto Reiner pressed the Zirconia pellets used in the three electrode cells (Chapter 6). Martin Van Assche and Jiho Yoo completed all temperature programmed desorption (TPD) and temperature programmed reaction (TPR) experiments (Chapter 4). Suman Chatterjee participated heavily in all phases of the La2CuO4 synthesis, La2CuO4 sensor fabrication and sensor response (OCP) characterization 4 (Chapter 3). Eric Macam fabricated and characterized the sensors that were prepared with the auto-ignition fuel-lean La2CuO4 and the co-precipitated La2CuO4 (Chapter 3). A researcher, like any professional, needs a clear view of reality and a strong sense of self- confidence so that he/she can rationally select ambitious goals from the multitude available without fear of failure. To my parents, I owe a debt of gratitude for their persistant love, guidance, and support. They assisted me more than anyone else in the development of my personal skill set which ultimately enabled me to achieve this doctoral degree. I thank Tony, Kerry, Dan, and John for opening their hearts and home to me. They made my last year in Gainesville my most productive and enjoyable. 5 TABLE OF CONTENTS Page ACKNOWLEDGMENTS ...............................................................................................................4 LIST OF TABLES...........................................................................................................................9 LIST OF FIGURES .......................................................................................................................10 ABSTRACT...................................................................................................................................16 CHAPTER 1 INTRODUCTION ..................................................................................................................18 1.1 Why Do We Need Sensors for NO or NO2?.....................................................................18 1.2 Why Use Solid-State Potentiometric NOX Sensors? ........................................................19 1.3 Why Aren’t We Already Using Solid-State Potentiometric Sensors to Monitor NOX? ...................................................................................................................................20 1.4 Summary...........................................................................................................................20 2 BACKGROUND ....................................................................................................................22 2.1 Nernstian and Non-Nernstian Sensors..............................................................................22 2.2 Sensor Materials ...............................................................................................................24 2.3 Background Information on La2CuO4 ..............................................................................28 2.4 Homogeneous Gas Phase NOX and CO Chemistry..........................................................30 2.5 Sensing Mechanisms ........................................................................................................32 2.5.1 Introduction ............................................................................................................32 2.5.2 Mixed Potential Theory Discussion .......................................................................33 2.6 Summary...........................................................................................................................36 3 EFFECT OF ELECTRODE MICROSTRUCTURE ON SENSITIVITY AND RESPONSE TIME..................................................................................................................44 3.1 Introduction.......................................................................................................................44 3.2 Experimental.....................................................................................................................47 3.2.1 Powder Synthesis....................................................................................................47 3.2.2 Powder Characterization ........................................................................................48 3.2.3 Sensor Fabrication..................................................................................................48 3.2.4 Electrical Characterization .....................................................................................50 3.3 Results and Discussion .....................................................................................................50 3.3.1 Powder Synthesis....................................................................................................50 3.3.2 Effect of Synthesis Technique on Sensor Electrode Microstructure......................51 3.3.3 Effect of Sintering Temperature and Time on Sensor Electrode Microstructure...51 3.3.4 Open-Circuit Potential Responses to Changes in NO Concentration ....................52 3.4 Summary...........................................................................................................................56 6 4 EVIDENCE THAT NOX AND CO SHIFT THE FERMI LEVEL OF La2CuO4 ..................66 4.1 Introduction.......................................................................................................................66 4.2 Background.......................................................................................................................66 4.3 Experimental.....................................................................................................................68 4.3.1 Powder Preparation and Characterization ..............................................................68 4.3.2 Potentiometric Sensor Fabrication and Voltage Monitoring..................................69 4.3.3 Resistance-type Sensor Fabrication and Electrical Characterization .....................69 4.3.4 Mass Spectrometry .................................................................................................70 4.4 Results...............................................................................................................................70 4.4.1 DTA-TGA, X-Ray Diffraction and FE-SEM Results of Calcined La2CuO4 Powder .........................................................................................................................70 4.4.2 Potentiometric Sensor.............................................................................................72 4.4.3 Resistance-type Sensor...........................................................................................73 4.5 Summary...........................................................................................................................75 5 INVESTIGATION OF SENSORS WITH ELECTROCHEMICAL IMPEDANCE SPECTROSCOPY..................................................................................................................87 5.1 Introduction.......................................................................................................................87 5.2 Experimental.....................................................................................................................89 5.3 Results and Discussion .....................................................................................................90 5.3.1 High Frequency ......................................................................................................90 5.3.1.1 La2CuO4 conduction mechanism .................................................................92 5.3.1.2 Effect of NOX
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