Design, Technology and Characterization of Micromechanised Sensors and Actuators for Harsh Environments

Los sistemas micro electro mecánicos (MEMS) han demostrado ser una exitosa familia de dispositivos que pueden usarse como plataforma para el desarrollo de dispositivos con aplicaciones en óptica, comunicaciones, procesado de señal y sensorización. Los dispositivos MEMS estándar suelen estar fabricados usando tecnología de silicio. Sin embargo, el rendimiento de estos MEMS se puede mejorar si se usan otros materiales. Por ejemplo, el diamante nanocristalino (NCD) ofrece unas excelentes propiedades mecánicas, transparencia y una superficie fácil de funcionalizar. Por otro lado, el sistema de materiales (In; Ga; Al)N, los materiales IIIN, se pueden usar para producir estructuras monocristalinas con alta sensibilidad mecánica y química. Además, el AlN se puede depositar por pulverización catódica reactiva sobre varios substratos, incluyendo NCD, para formar capas policristalinas orientadas con alta respuesta piezoeléctrica. Adicionalmente, tanto el NCD como los materiales III-N muestran una gran estabilidad térmica y química, lo que los hace una elección idónea para desarrollar dispositivos para aplicaciones para alta temperatura, ambientes agresivos e incluso para aplicaciones biocompatibles. En esta tesis se han usado estos materiales para el diseño y medición de demostradores tecnológicos. Se han perseguido tres objetivos principales: _ Desarrollo de unos procesos de fabricación apropiados. _ Medición de las propiedades mecánicas de los materiales y de los factores que limitan el rendimiento de los dispositivos. _ Usar los datos medidos para desarrollar dispositivos demostradores complejos. En la primera parte de esta tesis se han estudiado varias técnicas de fabricación. La estabilidad de estos materiales impide el ataque y dificulta la producción de estructuras suspendidas. Los primeros capítulos de esta disertación se dedican al desarrollo de unos procesos de transferencia de patrones por ataque seco y a la optimización del ataque húmedo sacrificial de varios substratos propuestos. Los resultados de los procedimientos de ataque se presentan y se describe la optimización de las técnicas para la fabricación de estructuras suspendidas de NCD y materiales III-N. En un capítulo posterior se estudia el crecimiento de AlN por pulverización catódica. Como se ha calculado en esta disertación para obtener una actuación eficiente de MEMS, las capas de AlN han de ser finas, típicamente d < 200 nm, lo que supone serias dificultades para la obtención de capas orientadas con respuesta piezoeléctrica. Las condiciones de depósito se han mapeado para identificar las fronteras que proporcionan el crecimiento de material orientado desde los primeros pasos del proceso. Además, durante la optimización de los procesos de ataque se estudió un procedimiento para fabricar películas de GaN nanoporoso. Estas capas porosas pueden servir como capas sacrificiales para la fabricación de estructuras suspendidas de GaN con baja tensión residual o como capas para mejorar la funcionalización superficial de sensores químicos o biológicos. El proceso de inducción de poros se discutirá y también se presentarán experimentos de ataque y funcionalización. En segundo lugar, se han determinado las propiedades mecánicas del NCD y de los materiales III-N. Se han fabricado varias estructuras suspendidas para la medición del módulo de Young y de la tensión residual. Además, las estructuras de NCD se midieron en resonancia para calcular el rendimiento de los dispositivos en términos de frecuencia y factor de calidad. Se identificaron los factores intrínsecos y extrínsecos que limitan ambas figuras de mérito y se han desarrollado modelos para considerar estas imperfecciones en las etapas de diseño de los dispositivos. Por otra parte, los materiales III-N normalmente presentan grandes gradientes de deformación residual que causan la deformación de las estructuras al ser liberadas. Se han medido y modelado estos efectos para los tres materiales binarios del sistema para proporcionar puntos de interpolación que permitan predecir las características de las aleaciones del sistema III-N. Por último, los datos recabados se han usado para desarrollar modelos analíticos y numéricos para el diseño de varios dispositivos. Se han estudiado las propiedades de transducción y se proporcionan topologías optimizadas. En el último capítulo de esta disertación se presentan diseños optimizados de los siguientes dispositivos: _ Traviesas y voladizos de AlN=NCD con actuación piezoeléctrica aplicados a nanoconmutadores de RF para señales de alta potencia. _ Membranas circulares de AlN=NCD con actuación piezoeléctrica aplicadas a lentes sintonizables. _ Filtros ópticos Fabry-Pérot basados en cavidades aéreas y membranas de GaN actuadas electrostáticamente. En resumen, se han desarrollado unos nuevos procedimientos optimizados para la fabricación de estructuras de NCD y materiales III-N. Estas técnicas se han usado para producir estructuras que llevaron a la determinación de las principales propiedades mecánicas y de los parámetros de los dispositivos necesarios para el diseño de MEMS. Finalmente, los datos obtenidos se han usado para el diseño optimizado de varios dispositivos demostradores. ABSTRACT Micro Electro Mechanical Systems (MEMS) have proven to be a successful family of devices that can be used as a platform for the development of devices with applications in optics, communications, signal processing and sensorics. Standard MEMS devices are usually fabricated using silicon based materials. However, the performance of these MEMS can be improved if other material systems are used. For instance, nanocrystalline diamond (NCD) offers excellent mechanical properties, optical transparency and ease of surface functionalization. On the other hand, the (In; Ga; Al)N material system, the III-N materials, can be used to produce single crystal structures with high mechanical and chemical sensitivity. Also, AlN can be deposited by reactive sputtering on various substrates, including NCD, to form oriented polycrystalline layers with high piezoelectric response. In addition, both NCD and III-N materials exhibit high thermal and chemical stability, which makes these material the perfect choice for the development of devices for high temperatures, harsh environments and even biocompatible applications. In this thesis these materials have been used for the design and measurement of technological demonstrators. Three main objectives have been pursued: _ Development of suitable fabrication processes. _ Measurement of the material mechanical properties and device performance limiting factors. _ Use the gathered data to design complex demonstrator devices. In a first part of the thesis several fabrication processes have been addressed. The stability of these materials hinders the etching of the layers and hampers the production of free standing structures. The first chapters of this dissertation are devoted to the development of a dry patterning etching process and to sacrificial etching optimization of several proposed substrates. The results of the etching processes are presented and the optimization of the technique for the manufacturing of NCD and III-N free standing structures is described. In a later chapter, sputtering growth of thin AlN layers is studied. As calculated in this dissertation, for efficient MEMS piezoelectric actuation the AlN layers have to be very thin, typically d < 200 nm, which poses serious difficulties to the production of c-axis oriented material with piezoelectric response. The deposition conditions have been mapped in order to identify the boundaries that give rise to the growth of c-axis oriented material from the first deposition stages. Additionally, during the etching optimization a procedure for fabricating nanoporous GaN layers was also studied. Such porous layers can serve as a sacrificial layer for the release of low stressed GaN devices or as a functionalization enhancement layer for chemical and biological sensors. The pore induction process will be discussed and etching and functionalization trials are presented. Secondly, the mechanical properties of NCD and III-N materials have been determined. Several free standing structures were fabricated for the measurement of the material Young’s modulus and residual stress. In addition, NCD structures were measured under resonance in order to calculate the device performance in terms of frequency and quality factor. Intrinsic and extrinsic limiting factors for both figures were identified and models have been developed in order to take into account these imperfections in the device design stages. On the other hand, III-N materials usually present large strain gradients that lead to device deformation after release. These effects have been measured and modeled for the three binary materials of the system in order to provide the interpolation points for predicting the behavior of the III-N alloys. Finally, the gathered data has been used for developing analytic and numeric models for the design of various devices. The transduction properties are studied and optimized topologies are provided. Optimized design of the following devices is presented at the last chapter of this dissertation: _ AlN=NCD piezoelectrically actuated beams applied to RF nanoswitches for large power signals. _ AlN=NCD piezoelectrically actuated circular membranes applied to tunable lenses. _ GaN based air gap tunable optical Fabry-Pérot filters with electrostatic actuation. On the whole, new optimized fabrication processes has been developed for the fabrication of NCD and III-N MEMS structures. These processing techniques was used to produce structures that led to the determination of the main mechanical properties and device parameters needed for MEMS design. Lastly, the gathered data was used for the design of various optimized demonstrator devices.

Design and demonstration of an electronically scanned reflectarray antenna at 100 GHz using multiresonant cells based on liquid crystals

The design, fabrication and measured results are presented for a reconfigurable reflectarray antenna based on liquid crystals (LC) which operates above 100 GHz. The antenna has been designed to provide beam scanning capabilities over a wide angular range, a large bandwidth and reduced Side-Lobe Level. Measured radiation patterns are in good agreement with simulations, and show that the antenna generates an electronically steerable beam in one plane over an angular range of 55º in the frequency band from 96 to 104 GHz. The Side Lobes Level is lower than -13 dB for all the scan angles and -18 dB is obtained over 16% of the scan range. The measured performance is significantly better than previously published results for this class of electronically tunable antenna, and moreover verifies the accuracy of the proposed procedure for LC modeling and antenna design.

Photoconductivity and Electro-Optical Properties of Wide Band Gap Metal Oxides

The PhD activity described in this Thesis was focused on the study of metal-oxide wide-bandgap materials, aiming at fabricating new optoelectronic devices such as solar-blind UV photodetectors, high power electronics, and gas sensors. Photocurrent spectroscopy and DC photocurrent time evolution were used to investigate the performance of prototypes under different atmospheres, temperatures and excitation wavelengths (or dark conditions). Cathodoluminescence, absorption spectroscopy, XRD and SEM were used to assess structural, morphologic, electrical and optical properties of materials. This thesis is divided into two main sections, each describing the work done on a different metal-oxide semiconductor. 1) MOVPE-grown Ga2O3 thin films for UV solar-blind photodetectors and high power devices The semiconducting oxides, among them Ga2O3, have been employed for several decades as transparent conducting oxide (TCO) electrodes for fabrication of solar cells, displays, electronic, and opto-electronic devices. The interest was mainly confined to such applications, as these materials tend to grow intrinsically n-type, and attempts to get an effective p-type doping has consistently failed. The key requirements of TCO electrodes are indeed high electrical conductivity and good transparency, while crystallographic perfection is a minor issue. Furthermore, for a long period no high-quality substrates and epi-layers were available, which in turn impeded the development of a truly full-oxide electronics. Recently, Ga2O3 has attracted renewed interest, as large single crystals and high-quality homo- and hetero-epitaxial layers became available, which paved the way to novel application areas. Our research group spent the last two years in developing a low temperature (500-700°C) MOVPE growth procedure to obtain thin films of Ga2O3 on different substrates (Dept. of Physics and IMEM-CNR at UNIPR). We obtained a significant result growing on oriented sapphire epitaxial films of high crystalline, undoped, pure phase -Ga2O3 (hexagonal). The crystallographic properties of this phase were investigated by XRD, in order to clarify the lattice parameters of the hexagonal cell. First design and development of solar blind UV photodetectors based on -phase was carried out and the optoelectronic performance is evaluated by means of photocurrent spectroscopy. The UV-response is adequately fast and reliable to render this unusual phase a subject of great interest for future applications. The availability of a hexagonal phase of Ga2O3 stable up to 700°C, belonging to the same space group of gallium nitride, with high crystallinity and tunable electrical properties, is intriguing in view of the development of nitride-based devices, by taking advantage of the more favorable symmetry and epitaxial relationships with respect to the monoclinic β-phase. In addition, annealing at temperatures higher than 700°C demonstrate that the hexagonal phase converts totally in the monoclinic one. 2) ZnO nano-tetrapods: charge transport mechanisms and time-response in optoelectronic devices and sensors Size and morphology of ZnO at the nanometer scale play a key role in tailoring its physical and chemical properties. Thanks to the possibility of growing zinc oxide in a variety of different nanostructures, there is a great variety of applications, among which gas sensors, light emitting diodes, transparent conducting oxides, solar cells. Even if the operation of ZnO nanostructure-based devices has been recently demonstrated, the mechanisms of charge transport in these assembly is still under debate. The candidate performed an accurate investigation by photocurrent spectroscopy and DC-photocurrent time evolution of electrical response of both single-tetrapod and tetrapod-assembly devices. During the research done for this thesis, a thermal activation energy enables the performance of samples at high temperatures (above about 300°C). The energy barrier is related to the leg-to-leg interconnection in the assembly of nanotetrapods. Percolation mechanisms are responsible for both the very slow photo-response (minutes to hours or days) and the significant persistent photocurrent. Below the bandgap energy, electronic states were investigated but their contribution to the photocurrent are two-three order of magnitude lower than the band edge. Such devices are suitable for employ in photodetectors as well as in gas sensors, provided that the mechanism by which the photo-current is generated and gas adsorption on the surface modify the conductivity of the material are known.

Lyra: uma função de derivação de chaves com custos de memória e processamento configuráveis.

Este documento apresenta o Lyra, um novo esquema de derivação de chaves, baseado em esponjas criptográficas. O Lyra foi projetado para ser estritamente sequencial, fornecendo um nível elevado de segurança mesmo contra atacantes que utilizem múltiplos núcleos de processamento, como uma GPU ou FPGA. Ao mesmo tempo possui uma implementação simples em software e permite ao usuário legítimo ajustar o uso de memória e tempo de processamento de acordo com o nível de segurança desejado. O Lyra é, então, comparado ao scrypt, mostrando que esta proposta fornece um nível se segurança mais alto, além de superar suas deficiências. Caso o atacante deseje realizar um ataque utilizando pouca memória, o tempo de processamento do Lyra cresce exponencialmente, enquanto no scrypt este crescimento é apenas quadrático. Além disto, para o mesmo tempo de processamento, o Lyra permite uma utilização maior de memória, quando comparado ao scrypt, aumentando o custo de ataques de força bruta.

Priority realloc: um mecanismo para alocação de rotas e recursos em redes EON.

Backbone networks are responsible for long-haul data transport serving many clients with a large volume of data. Since long-haul data transport service must rely on a robust high capacity network the current technology broadly adopted by the industry is Wavelength Division Multiplexing (WDM). WDM networks enable one single ber to operate with multiple high capacity channels, drastically increasing the ber capacity. In WDM networks each channel is associated with an individual wavelength. Therefore a whole wavelength capacity is assigned to a connection, causing waste of bandwidth in case the connection bandwidth requirement is less than the channel total capacity. In the last half decade, Elastic Optical Networks (EON) have been proposed and developed based on the fexible use of the optical spectrum known as the exigrid. EONs are adaptable to clients requirements and may enhance optical networks performance. For these reasons, research community and data transport providers have been demonstrating increasingly high interest in EONs which are likely to replace WDM as the universally adopted technology in backbone networks in the near future. EONs have two characteristics that may limit its ecient resources use. The spectrum fragmentation, inherent to the dynamic EON operation, decrease the network capacity to assign resources to connection requests increasing network blocking probability. The spectrum fragmentation also intensifides the denial of service to higher rate request inducing service unfairness. Due to the fact EONs were just recently developed and proposed, the aforementioned issues were not yet extensively studied and solutions are still being proposed. Furthermore, EONs do not yet provide specific features as differentiated service mechanisms. Differentiated service strategies are important in backbone networks to guarantee client\'s diverse requirements in case of a network failure or the natural congestion and resources contention that may occur at some periods of time in a network. Impelled by the foregoing facts, this thesis objective is three-fold. By means of developing and proposing a mechanism for routing and resources assignment in EONs, we intend to provide differentiated service while decreasing fragmentation level and increasing service fairness. The mechanism proposed and explained in this thesis was tested in a EON simulation environment and performance results indicated that it promotes beneficial performance enhancements when compared to benchmark algorithms.

Mesostructured zeolites: bridging the gap between zeolites and MCM-41

Surfactant-templating is one of the most versatile and useful techniques to implement mesoporous systems into solid materials. Various strategies based on various interactions between surfactants and solid precursors have been explored to produce new structures. Zeolites are invaluable as size- and shape-selective solid acid catalysts. Nevertheless, their micropores impose limitations on the mass transport of bulky feed and/or product molecules. Many studies have attempted to address this by utilizing surfactant-assisting technology to alleviate the diffusion constraints. However, most efforts have failed due to micro/mesopore phase separation. Recently, a new technique combining the uses of cationic surfactants and mild basic solutions was introduced to synthesise mesostructured zeolites. These materials sustain the unique characteristics of zeolites (i.e., strong acidity, crystallinity, microporosity, and hydrothermal stability), including tunable mesopore sizes and degrees of mesoporosity. The mesostructured zeolites are now commercially available through Rive Technology, and show superior performance in VGO cracking. This feature article provides an overview of recent explorations in the introduction of mesoporosity into zeolites using surfactant-templating techniques. Various porous materials, preparation methods, physical and catalytic properties of mesostructured zeolites will be discussed.

Paving the way for methane hydrate formation on metal–organic frameworks (MOFs)

The presence of a highly tunable porous structure and surface chemistry makes metal–organic framework (MOF) materials excellent candidates for artificial methane hydrate formation under mild temperature and pressure conditions (2 °C and 3–5 MPa). Experimental results using MOFs with a different pore structure and chemical nature (MIL-100 (Fe) and ZIF-8) clearly show that the water–framework interactions play a crucial role in defining the extent and nature of the gas hydrates formed. Whereas the hydrophobic MOF promotes methane hydrate formation with a high yield, the hydrophilic one does not. The formation of these methane hydrates on MOFs has been identified for the first time using inelastic neutron scattering (INS) and synchrotron X-ray powder diffraction (SXRPD). The results described in this work pave the way towards the design of new MOF structures able to promote artificial methane hydrate formation upon request (confined or non-confined) and under milder conditions than in nature.

(Table 2) Concentrations of dissolved aluminum in interstitial water from sediments of the Indian Ocean

Results are presented of application of laser stepwise photoionization of atoms in combination with thermal atomization of matter in vacuum for direct determination of aluminum dissolved in sea and interstitial waters. Dry residue from evaporation of 40 ?l sea water was atomized in a crucible at 1800°C, and aluminum atoms in the beam thus formed were energized into Rydberg state in two steps by two tunable dye laser beams; the atoms were then ionized by an electric pulse and resulting ions were recorded by secondary emission electron multiplier (ion detector). Ionic signal dependence on sample vaporization time was studied. The procedure is suggested for separating out a selective signal in a single measurement. Dissolved aluminum concentrations in interstitial waters of the Indian Ocean and in waters of the river-sea zone were determined using preliminarily plotted calibration characteristics for aluminum solutions in deionized and sea waters. The minimum detectable Al concentration in seawater was 1 ?g/l that corresponds to 40 pg of Al in a sample.

Developments in the Theory of X-ray Absorption and Compton Scattering.

Thesis (Ph.D.)--University of Washington, 2016-06

Entanglement and the Einstein-Podolsky-Rosen paradox with coupled intracavity optical down-converters

We show that two evanescently coupled χ((2)) parametric down-converters inside a Fabry-Perot cavity provide a tunable source of quadrature squeezed light, Einstein-Podolsky-Rosen (EPR) correlations and quantum entanglement. Analyzing the operation in the below threshold regime, we show how these properties can be controlled by adjusting the coupling strengths and the cavity detunings. As this can be implemented with integrated optics, it provides a possible route to rugged and stable EPR sources.

Thermal and electrical currents in nanoscale electronic interferometers

We theoretically study thermal transport in an electronic interferometer comprising a parallel circuit of two quantum dots, each of which has a tunable single electronic state which are connected to two leads at different temperature. As a result of quantum interference, the heat current through one of the dots is in the opposite direction to the temperature gradient. An excess heat current flows through the other dot. Although locally, heat flows from cold to hot, globally the second law of thermodynamics is not violated because the entropy current associated with heat transfer through the whole device is still positive. The temperature gradient also induces a circulating electrical current, which makes the interferometer magnetically polarized.

Microfluidic interferometer

We present a class of compact, fluid-based, interferometric, tunable optical components: the single-beam microfluidic Mach-Zender interferometer. Phase delay is achieved through light propagation across a fluid-air interface (meniscus). The effect of meniscus curvature on the device transmission is considered using the three-dimensional beam propagation method and shown to be an important device parameter. We engineer the meniscus curvature using monomer surface chemistry, rendering it flat, and find that the experimental response corresponds well with simulation. The device has a resonance at 1.3 mum with a 25 dB extinction ratio; the latter can be adjusted by shifting the meniscus position.

Bright entanglement and the Einstein-Podolsky-Rosen paradox with coupled parametric oscillators

We show that two evanescently coupled chi((2)) parametric oscillators provide a tunable bright source of quadrature squeezed light, Einstein-Podolsky-Rosen correlations and quantum entanglement. Analysing the system in the above threshold regime, we demonstrate that these properties can be controlled by adjusting the coupling strengths and the cavity detunings. As this can be implemented with integrated optics, it provides a possible route to rugged and stable EPR sources. (C) 2005 Elsevier B.V. All rights reserved.

Bright entanglement in the intracavity nonlinear coupler

We show that the intracavity Kerr nonlinear coupler is a potential source of bright continuous variable entangled light beams which are tunable and spatially separated. We use a linearized fluctuation analysis to calculate the necessary correlations in regimes where it is valid. This means that we are treating regimes where the system exhibits Gaussian statistics so that well-known criteria are both necessary and sufficient to demonstrate entanglement. This system may be realized with integrated optics and thus provides a potentially rugged and stable source of bright entangled beams.

Systematic selection of solvents for the fabrication of 3D combined macro- and microporous polymeric scaffolds for soft tissue engineering

In this study, we investigate the fabrication of 3D porous poly(lactic-co-glycolic acid) (PLGA) scaffolds using the thermally-induced phase separation technique. The current study focuses on the selection of alternative solvents for this process using a number of criteria, including predicted solubility. toxicity, removability and processability. Solvents were removed via either vacuum freeze-drying or leaching, depending on their physical properties. The residual solvent was tested using gas chromatography-mass spectrometry. A large range of porous, highly interconnected scaffold architectures with tunable pore size and alignment was obtained, including combined macro- and microporous structures and an entirely novel 'porous-fibre' structure. The morphological features of the most promising poly(lactic-co-glycolic acid) scaffolds were analysed via scanning electron microscopy and X-ray micro-computed tomography in both two and three dimensions. The Young's moduli of the scaffolds under conditions of temperature, pH and ionic strength similar to those found in the body were tested and were found to be highly dependent on the architectures.