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Design, Fabrication, and Characterization of Carbon Nanotube Field Emission Devices for Advanced Applications

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Design, Fabrication, and Characterization of Carbon Nanotube Field Emission Devices for Advanced Applications Design, Fabrication, and Characterization of Carbon Nanotube Field Emission Devices for Advanced Applications by Erich Justin Radauscher Department of Electrical and Computer Engineering Duke University Date:_______________________ Approved: ___________________________ Jeffrey T. Glass, Supervisor ___________________________ Brian R. Stoner ___________________________ Adrienne D. Stiff-Roberts ___________________________ Aaron D. Franklin ___________________________ Martin A. Brooke Dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in the Department of Electrical and Computer Engineering in the Graduate School of Duke University 2016 i v ABSTRACT Design, Fabrication, and Characterization of Carbon Nanotube Field Emission Devices for Advanced Applications by Erich Justin Radauscher Department of Electrical and Computer Engineering Duke University Date:_______________________ Approved: ___________________________ Jeffrey T. Glass, Supervisor ___________________________ Brian R. Stoner ___________________________ Adrienne D. Stiff-Roberts ___________________________ Aaron D. Franklin ___________________________ Martin A. Brooke An abstract of a dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in the Department of Electrical and Computer Engineering in the Graduate School of Duke University 2016 Copyright by Erich Justin Radauscher 2016 Abstract Carbon nanotubes (CNTs) have recently emerged as promising candidates for electron field emission (FE) cathodes in integrated FE devices. These nanostructured carbon materials possess exceptional properties and their synthesis can be thoroughly controlled. Their integration into advanced electronic devices, including not only FE cathodes, but sensors, energy storage devices, and circuit components, has seen rapid growth in recent years. The results of the studies presented here demonstrate that the CNT field emitter is an excellent candidate for next generation vacuum microelectronics and related electron emission devices in several advanced applications. The work presented in this study addresses determining factors that currently confine the performance and application of CNT-FE devices. Characterization studies and improvements to the FE properties of CNTs, along with Micro-Electro-Mechanical Systems (MEMS) design and fabrication, were utilized in achieving these goals. Important performance limiting parameters, including emitter lifetime and failure from poor substrate adhesion, are examined. The compatibility and integration of CNT emitters with the governing MEMS substrate (i.e., polycrystalline silicon), and its impact on these performance limiting parameters, are reported. CNT growth mechanisms and kinetics were investigated and compared to silicon (100) to improve the design of CNT iv emitter integrated MEMS based electronic devices, specifically in vacuum microelectronic device (VMD) applications. Improved growth allowed for design and development of novel cold-cathode FE devices utilizing CNT field emitters. A chemical ionization (CI) source based on a CNT- FE electron source was developed and evaluated in a commercial desktop mass spectrometer for explosives trace detection. This work demonstrated the first reported use of a CNT-based ion source capable of collecting CI mass spectra. The CNT-FE source demonstrated low power requirements, pulsing capabilities, and average lifetimes of over 320 hours when operated in constant emission mode under elevated pressures, without sacrificing performance. Additionally, a novel packaged ion source for miniature mass spectrometer applications using CNT emitters, a MEMS based Nier-type geometry, and a Low Temperature Cofired Ceramic (LTCC) 3D scaffold with integrated ion optics were developed and characterized. While previous research has shown other devices capable of collecting ion currents on chip, this LTCC packaged MEMS micro-ion source demonstrated improvements in energy and angular dispersion as well as the ability to direct the ions out of the packaged source and towards a mass analyzer. Simulations and experimental design, fabrication, and characterization were used to make these improvements. Finally, novel CNT-FE devices were developed to investigate their potential to perform as active circuit elements in VMD circuits. Difficulty integrating devices at v micron-scales has hindered the use of vacuum electronic devices in integrated circuits, despite the unique advantages they offer in select applications. Using a combination of particle trajectory simulation and experimental characterization, device performance in an integrated platform was investigated. Solutions to the difficulties in operating multiple devices in close proximity and enhancing electron transmission (i.e., reducing grid loss) are explored in detail. A systematic and iterative process was used to develop isolation structures that reduced crosstalk between neighboring devices from 15% on average, to nearly zero. Innovative geometries and a new operational mode reduced grid loss by nearly threefold, thereby improving transmission of the emitted cathode current to the anode from 25% in initial designs to 70% on average. These performance enhancements are important enablers for larger scale integration and for the realization of complex vacuum microelectronic circuits. vi Dedicated to my dearest wife, Rebecca To my beloved parents, Erich and Sandra, and brother, Matthew And To my amazing baby boy, Aiden vii Table of Contents Abstract ......................................................................................................................................... iv Table of Contents ...................................................................................................................... viii List of Tables ...............................................................................................................................xiv List of Figures .............................................................................................................................. xv List of Symbols and Abbreviations ........................................................................................ xxii Acknowledgements ................................................................................................................ xxiii 1. General Introduction ................................................................................................................ 1 1.1 Electronic Materials for Cold Cathode Field Emission ............................................... 2 1.2 Vacuum Microelectronics Overview ............................................................................. 7 1.3 Motivation and Objectives of this Research................................................................ 11 1.4 Dissertation Outline ....................................................................................................... 12 2. Background - Carbon Nanotubes (CNT), Field Emission (FE), FE Vacuum Microelectronic Devices (FE-VMDs), and Mass Spectrometry (MS) ................................... 15 2.1 Introduction ..................................................................................................................... 15 2.2 Carbon Nanotubes ......................................................................................................... 15 2.2.1 Significance of CNT Research .................................................................................. 16 2.2.2 Structure ..................................................................................................................... 17 2.2.3 Growth Mechanisms of CNTs ................................................................................. 19 2.2.4 Properties of CNTs .................................................................................................... 21 2.2.4.1 Mechanical .......................................................................................................... 21 2.2.4.2 Electronic ............................................................................................................. 22 viii 2.2.5 CNT Applications ...................................................................................................... 24 2.3 Field Emission Fundamentals ....................................................................................... 25 2.3.1 Electron Emission ...................................................................................................... 26 2.3.1.1 Probability of Escape ......................................................................................... 26 2.3.1.2 Emission Processes ............................................................................................ 28 2.3.1.3 Emission Metrics Specific to FE ....................................................................... 31 2.3.2 The Fowler-Nordheim Theory ................................................................................ 32 2.3.2.1 Correction to the F-N Equation ........................................................................ 37 2.3.3 Field Emission from CNTs ....................................................................................... 38 2.3.3.1 Unique FE Properties of CNTs ......................................................................... 38 2.4 Field Emission Devices .................................................................................................
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