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

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 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 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.

Os recursos cinotécnicos e a sua necessidade no Exército Português

No âmbito do Relatório Científico Final do Trabalho de Investigação Aplicada, o presente trabalho com o título “Os Recursos Cinotécnicos e a sua necessidade no Exército Português” estuda o emprego operacional atual, fruto das valências cinotécnicas existentes e as tarefas operacionais que podem, pelos referidos recursos, ser apoiadas. O autor considera também as características físicas do cão, as implicações logísticas e financeiras e a doutrina que concorrem para o referido emprego operacional, elencando lacunas existentes que, quando colmatadas poderão concorrer para um emprego operacional eficiente dos recursos cinotécnicos do Exército Português. Para obtenção de dados foi conduzida análise documental e bibliográfica e efetuados inquéritos por entrevista a comandantes de Batalhão/ Grupo com meios cinotécnicos na sua orgânica ou em apoio aos mesmos, aos comandantes das unidades cinotécnicas do Exército Português e dos restantes ramos das Forças Armadas e Forças de Segurança, ainda a comandantes da Força de Operações Especiais. O objetivo deste trabalho passa por avaliar de que forma podem os recursos cinotécnicos do Exército Português contribuir para o melhor desempenho das suas unidades operacionais. Para a consecução do mesmo o autor fez uso do método indutivo onde, com base no emprego operacional junto dos Paraquedistas e da Polícia do Exército, generalizou o que poderia ser profícuo para todas as unidades operacionais do Exército Português, bem como todas as lacunas que devem ser colmatadas para apoio ao mesmo. No âmbito da doutrina é importante o fornecimento aos comandantes das unidades apoiadas informação sobre as capacidades, limitações e regras de segurança relativos ao emprego dos binómios em apoio a cada tarefa das tipologias de operações, fornecendo informações precisas e detalhadas sobre o que cada tipo de cão consegue fazer, durante quanto tempo e em que condições ambientais pois, mesmo havendo atualmente a PDE 0-20-18, sendo a cinotecnia uma área muito técnica, a falta da referida doutrina pode se transformar numa condicionante ao emprego dos binómios. A referida PDE, atualmente, assume-se como um potenciador do emprego dos recursos cinotécnicos. No âmbito logístico pode ser pensada uma rede logística própria tendo em conta o emprego operacional e a projeção dos binómios, explícitando desde a forma de aquisição dos cães até ao suporte à sua projeção, contudo deve-se pesar, por outro lado, se o emprego dos binómios em treinos operacionais ou em missões assume um peso significativo na manobra logística global de modo a exigir criação de uma rede própria. As características naturais do cão são um potenciador da ação e sentimento de segurança, podendo, ainda, ser usadas para colmatar a falta de efetivos. Quanto ao emprego operacional importa salientar a deteção de explosivos e estupefacientes, os cães de sentinela, binómios de guarda e binómios de exploração (que em simultâneo executam patrulhas de segurança).

IMPROVED SENSITIVITY OF RESONANT MASS SENSOR BASED ON MICRO TILTING PLATE AND MICRO CANTILEVER

Vapor sensors have been used for many years. Their applications range from detection of toxic gases and dangerous chemicals in industrial environments, the monitoring of landmines and other explosives, to the monitoring of atmospheric conditions. Microelectrical mechanical systems (MEMS) fabrication technologies provide a way to fabricate sensitive devices. One type of MEMS vapor sensors is based on mass changing detection and the sensors have a functional chemical coating for absorbing the chemical vapor of interest. The principle of the resonant mass sensor is that the resonant frequency will experience a large change due to a small mass of gas vapor change. This thesis is trying to build analytical micro-cantilever and micro-tilting plate models, which can make optimization more efficient. Several objectives need to be accomplished: (1) Build an analytical model of MEMS resonant mass sensor based on micro-tilting plate with the effects of air damping. (2) Perform design optimization of micro-tilting plate with a hole in the center. (3) Build an analytical model of MEMS resonant mass sensor based on micro-cantilever with the effects of air damping. (4) Perform design optimization of micro-cantilever by COMSOL. Analytical models of micro-tilting plate with a hole in the center are compared with a COMSOL simulation model and show good agreement. The analytical models have been used to do design optimization that maximizes sensitivity. The micro-cantilever analytical model does not show good agreement with a COMSOL simulation model. To further investigate, the air damping pressures at several points on the micro-cantilever have been compared between analytical model and COMSOL model. The analytical model is inadequate for two reasons. First, the model’s boundary condition assumption is not realistic. Second, the deflection shape of the cantilever changes with the hole size, and the model does not account for this. Design optimization of micro-cantilever is done by COMSOL.

Improved Dynamic Headspace Sampling and Detection using Capillary Microextraction of Volatiles Coupled to Gas Chromatography Mass Spectrometry

Sampling and preconcentration techniques play a critical role in headspace analysis in analytical chemistry. My dissertation presents a novel sampling design, capillary microextraction of volatiles (CMV), that improves the preconcentration of volatiles and semivolatiles in a headspace with high throughput, near quantitative analysis, high recovery and unambiguous identification of compounds when coupled to mass spectrometry. The CMV devices use sol-gel polydimethylsiloxane (PDMS) coated microglass fibers as the sampling/preconcentration sorbent when these fibers are stacked into open-ended capillary tubes. The design allows for dynamic headspace sampling by connecting the device to a hand-held vacuum pump. The inexpensive device can be fitted into a thermal desorption probe for thermal desorption of the extracted volatile compounds into a gas chromatography-mass spectrometer (GC-MS). The performance of the CMV devices was compared with two other existing preconcentration techniques, solid phase microextraction (SPME) and planar solid phase microextraction (PSPME). Compared to SPME fibers, the CMV devices have an improved surface area and phase volume of 5000 times and 80 times, respectively. One (1) minute dynamic CMV air sampling resulted in similar performance as a 30 min static extraction using a SPME fiber. The PSPME devices have been fashioned to easily interface with ion mobility spectrometers (IMS) for explosives or drugs detection. The CMV devices are shown to offer dynamic sampling and can now be coupled to COTS GC-MS instruments. Several compound classes representing explosives have been analyzed with minimum breakthrough even after a 60 min. sampling time. The extracted volatile compounds were retained in the CMV devices when preserved in aluminum foils after sampling. Finally, the CMV sampling device were used for several different headspace profiling applications which involved sampling a shipping facility, six illicit drugs, seven military explosives and eighteen different bacteria strains. Successful detection of the target analytes at ng levels of the target signature volatile compounds in these applications suggests that the CMV devices can provide high throughput qualitative and quantitative analysis with high recovery and unambiguous identification of analytes.