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Ce travail a été effectué dans le cadre d’études de la miniaturisation d’un cryo-réfrigérateur de type tube à gaz pulsé (TGP) et particulièrement pour mieux comprendre l’écoulement et le transfert de chaleur dans un régénérateur, l’élément clé du TGP.Nous présentons les études numérique et expérimentale du facteur de frottement et du nombre de Nusselt pour les écoulements stationnaires et continus à nombre de Reynolds modéré O(1 − 100) au sein d’un régénérateur micro-fabriqué. L’influence de la porosité et de la géométrie est étudiée. La micro-structure précisément contrôlée représente des canaux incurvés de largeur de 10, 20 et 40 μm et de profondeur de 100 à 300 μm qui forment un réseau de colonnes ayant des profiles de losanges ou sinusoïdaux. Les micro-canaux sont gravés sur un substrat de silicium par la technologie DRIE. Une technologie d’implantation de thermomètres à l’intérieur de la micro-structure de régénérateur a été développée et mise en œuvre. Les performances des micro-régénérateurs ont été étudiées selon deux approches : la première se base sur le rapport des pertes de charges dans l’écoulement et de l’efficacité du transfert thermique (NPH/NTU) ; la deuxième, sur le coefficient de transfert de chaleur globale proposé par Bejan. L’étude numérique de ces deux critères montre tout le potentiel des micro-structures proposées. / This research is done in the framework of miniaturisation of pulse tube cryocoolers studies and especially to gain a better understanding of the mass flow and heat transfert in the regenerator, which is a crucial component of these type of cryocoolers.In this work we present a numerical and experimental study of the Darcy-Weisbach friction factor and Nusselt number for a continuous and steady flow at moderate Reynolds number O(1−100) in a micro-machined regenerators. The influence of porosity from 40 to 80 % and of the geometry parameters are studied. Well-controlled microstructures represent convoluted channels of 10, 20 or 40 μm width and 100 or 300 μm depth generated by rhombic- or sinusoidal-shaped columns.The channels are etched in Silicon wafers using DRIE MEMS technology. The thermometers are integrated inside the regenerator’s micro-structure to measure the temperature evolution. The efficiency of the regenerators is estimated using two different approaches : the first, as a ratio of pressure drop losses and heat transfer efficiency (NPH/NTU) ; the second, as a volumetric heat transfer density coefficient proposed by Bejan. The numerical study of the efficiency shows theinterest of proposed micro-structures.

Novel processes were developed that resulted in a self-packaged device during the system integration, along with a transparent lid for inspection or optical probing. A new process was developed for improving the verticality in Micro Electro Mechanical Systems (MEMS) structures using Deep Reactive Ion Etching (DRIE). A self-pattered, mask-less photolithography technique was developed to metallize these vertical structures while maintaining a transparent window, for packaging of various MEMS devices. The verticality and metallization coverage were evaluated by incorporating the MEMS structures into an optical Corner Cube Retroreflector (CCR). A low temperature, hermetic sealing technique was also developed using In-Au thermo-compression bonding at 160°C. Cross-shaped 550um deep vertical mirrors, with sidewall angles of 90.08° were etched with this new DRIE technique. This is the best reported sidewall angle for such deep structures. The typical scalloped DRIE sidewall roughness was reduced to 40nm using wet polishing. A bonded Pyrex wafer was used as the handle wafer during DRIE; it eventually forms the package window after DRIE. The metallized, vertical mirrors were bonded to a MEMS device chip to assemble and package the CCR. The MEMS device chip consisted of an array of torsion mirrors. The mirrors were designed to modulate at 6Vp-p - 20Vp-p, with the resonant frequencies ranging from 25 KHz - 50 KHz. The design and simulation results are presented. To test the hermetic seal, helium leak tests were performed on the packaged device. Leak rates of as low as 2.8x10-8 atm cc/s air were detected, which is better than the MIL-STD-883G of 5x10-8 atm cc/s air for a package volume of 7.8x10-3 CC. A microprocessor and temperature/humidity sensor was then integrated with the CCR to assemble a passive optical digital data communicator. A flexible circuit design and a folded packaging scheme were utilized to minimize the overall form factor. Flat, flexible polymer batteries were incorporated to reduce the thickness of the package to a few millimeters. The fully packaged sensor system was about 30mmx30mmx6mm. Recorder sensor data was transmitted to a remote location using the CCR, and those results are presented.

Hollow biocompatible microneedle arrays were designed and fabricated using two different bulk micromachining techniques-Deep Reactive Ion Etching and Coherent Porous Silicon technology to investigate their reliability for transdermal applications. An in-house experimental setup was developed for microneedle fracture and split thickness penetration force measurements. Out of plane needle array configurations (100and#956;m needle length) with intra array geometric variations including needle shape, diameter, intra-array pitch and density (1a 625) were characterized on cadaver skin to predict skin barrier penetration without fracture. Use of microneedle array as transdermal patch necessitates reliable penetration and not just pushing against stratum corneum like a bed of nails. Critical in plane fracture tests were conducted on single microneedle columns with different geometry to validate the failure mechanism with force quantification relations. Preliminary penetration characterization was performed on skin like polymer followed by direct testing on cryogen preserved cadaver skin. Compressive and indentation test were performed on both excised skin and polymer to analyze their mechanical behavior on loading and establish a mechanical correlation. Finite element modeling using ANSYS was done to examine the effect of shear loading on the needles due to lack of experimental verification.

Patch-based transdermal drug delivery offers a convenient way to administer drugs without the drawbacks of standard hypodermic injections relating to issues such as patient acceptability and injection safety. However, conventional transdermal drug delivery is limited to therapeutics where the drug can diffuse across the skin barrier. By using miniaturized needles, a pathway into the human body can be established which allow transport of macromolecular drugs such as insulins or vaccines. These microneedles only penetrate the outermost skin layers, superficial enough not to reach the nerve receptors of the lower skin. Thus, microneedle insertions are perceived as painless. The thesis presents research in the field of microneedle-based drug delivery with the specific aim of investigating a microneedle-based transdermal patch concept. To enable controllable drug infusion and still maintain an unobtrusive and easy-to-use, patch-like design, the system includes a small active dispenser mechanism. The dispenser is based on a novel thermal actuator consisting of highly expandable microspheres. When actuated, the microspheres expand into a liquid reservoir and, subsequently, dispense stored liquid through outlet holes. The microneedles are fabricated in monocrystalline silicon by Deep Reactive Ion Etching. The needles are organized in arrays situated on a chip. To allow active delivery, the microneedles are hollow with the needle bore-opening located on the side of the needle. This way, the needle can have a sharp and well-defined needle tip. A sharp needle is a further requirement to achieve microneedle insertion into skin by hand. The thesis presents fabrication and evaluation of both the microneedle structure and the transdermal patch as such. Issues such as penetration reliability, liquid delivery into the skin and microneedle packaging are discussed. The microneedle patch was also tested and studied in vivo for insulin delivery. Results show that intradermal administration with microneedles give rise to similar insulin concentration as standard subcutaneous delivery with the same dose rate. / QC 20100623

Thesis (Ph. D.)--Universiteit van Amsterdam, 1983. / Includes bibliographical references.

A novel micromachining technology on SOI substrates is presented that is capable of producing on-chip high-Q resonators and resonator arrays equipped with high aspect-ratio (30:1) microstructures and nano-gap capacitive transducers filled with high-k dielectrics. The newly developed IC-compatible MEMS microfabrication process consists of merely three standard photolithography steps, which is much simpler than the other SOI-based resonator device technologies. In order to achieve the optimum performance and yield of the resonators and resonator arrays, this SOI-based fabrication process has been carefully designed and investigated step by step. For capacitively-transduced extensional mode (e.g., radial-contour and wine-glass mode) resonators, formation of nano-scale capacitive gaps and large resonator-to-electrode overlap area is essential for reducing the motional resistance Rx and DC bias voltage by strengthening the capacitive transduction. Atomic Layer Deposition (ALD) technology with superb conformability and uniformity as well as outstanding thickness controllability is used to deposit the ultra-thin layer (~10 nm) of high-k dielectric material that acts as the solid capacitive gaps, which allows the mass production of on-chip capacitively-transduced resonators and resonator arrays with greatly enhanced electromechancial coupling coefficient, and thus lower motional resistance and DC bias voltage. Using this technique, high-Q micromechanical resonators and resonator arrays on SOI substrates operating at ultra-high frequencies (UHF) have been developed. The ultimate goal of this project is to implement on-chip narrow-band micromechanical filters with unprecedented frequency selectivity and ultra-low insertion loss. By fine-tuning the nonlinear characteristics of the capacitive transducers enabled by the new SOI technology, novel on-chip mechanical signal processors for frequency manipulation, such as mixer and multiplier, will be investigated.

Microelectromechanical systems (MEMS) technology allows the realization of mechanical parts, sensors, actuators and electronics on silicon substrate. An attractive utilization of MEMS is to develop micro instruments for chemical analysis. An example is gas chromatography (GC) which is widely used in food, environmental, pharmaceutical, petroleum/refining, forensic/security, and flavors and fragrances industries. A MEMS-based micro GC (µGC) provides capabilities for quantitative analysis of complex chemical mixtures in the field with very short analysis time and small amounts of consumables. The aim of this research effort is to enhance the sensitivity and selectivity of µGC instruments by implementing chemical amplification method known as preconcentration. A micro preconcentrator (µPC) extracts the target analytes from the sample matrix, concentrates them, and injects them into the separation column for analysis. This work resulted in the development of silicon-glass bonded chips consisting of 7 mm x 7 mm x 0.38 mm multiport cavity with thousands of embedded 3D microstructures (to achieve high surface-to-volume ratio) coated with polymeric thin film adsorbents. Deep reactive ion etching (DRIE) was the enabling technology for the realization of µPCs. Several coating methods, such as inkjet printing of polymers and polymer precipitation from solution have been utilized to coat complex geometrical structures. One major outcome was the development of cobweb adsorbent structure. Moreover, the porous polymeric adsorbent Tenax TA in the film form was characterized, for the first time, for μPC application and shown to have similar properties to that of the granular form. Several μPC designs were experimentally evaluated for their performance in concentrating volatile organic compounds, including cancer biomarkers, Propofol (anesthetic agent), environmental pollutants, and chemical warfare simulants. The possibility of utilizing the μPCs in practical applications such breath analysis was also demonstrated. / Ph. D.

L’imagerie multispectrale permet d’améliorer la détection et la reconnaissance de cibles dans les applications de surveillance. Elle consiste à analyser des images de la même scène acquises simultanément dans plusieurs bandes spectrales grâce à un filtrage. Cette thèse étudie la possibilité de réaliser une matrice de 4 filtres Fabry Pérot (FP) intégrés 3D et ajustables par actionnement électrostatique dans le domaine visible-proche infrarouge. Les miroirs fixes des filtres FP sont des multicouches ZnS/YF₃ déposés sur un wafer de borosilicate, et les miroirs mobiles sont des membranes multicouches PECVD SiNH/SiOH encastrées sur une structure mobile très compacte micro-usinée dans un wafer en silicium. Les performances optiques des filtres FP ont été optimisées en prenant en compte la dissymétrie et le déphasage à la réflexion des miroirs. La structure mobile a été modélisée par éléments finis pour minimiser ses déformations lors de l’actionnement. Les étapes critiques des procédés de fabrication des miroirs mobiles en technologie Si ou SOI ont été mises au point : i) la fabrication et la libération par gravures profondes DRIE et XeF₂ des membranes multicouches avec une contrainte résiduelle ajustée par recuit et une réflectance voisine de 50% dans une large gamme spectrale, ii) le contrôle des vitesse de la gravure DRIE avec des motifs temporaires permettant la gravure simultanée de motifs de largeur et de profondeur variables, et iii) la délimitation de motifs sur surfaces fortement structurées à l’aide de pochoirs alignés mécaniquement ou de films secs photosensibles. Ces travaux ouvrent la voie vers une réalisation complète d’une matrice de filtres FP intégrés 3D. / Multispectral imaging is used to improve target detection and identification in monitoring applications. It consists in analyzing images of the same scene simultaneously recorded in several spectral bands owing to a filtering. This thesis investigates the possibility to realize, an array of four 3D integrated Fabry-Perot (FP) filters that are tunable in the visible-near infrared range by electrostatic actuation. The fixed mirrors of the FP filters are ZnS/YF₃ multilayers deposited on a borosilicate wafer, and the movable mirrors are PECVD SiNH/SiOH multilayer membranes clamped in a very compact movable structure micromachined in a Si wafer. A 3rd glass wafer is used for filters packaging. Optical performances of the FP filters have been optimized by taking into account the asymmetry and the reflection phase shift of the mirrors and the mobile structure has been modeled by finite elements analysis notably to minimize its deformation during actuation. The critical steps of the movable mirrors fabrication process in Si or SOI technology have been developed : i) the fabrication and the release by DRIE and XeF₂ etching of 8 or 12 layers membranes with a residual stress tunable by annealing and a reflectance close to 50% in broad wavelength range (570-900nm), ii) the control with temporary patterns of the simultaneous deep etching of patterns with different widths and depths, and iv) various patterning techniques on highly structured surfaces based on shadow masks (with mechanical alignment) or laminated photosensitive dry films. These results open the way towards the full realization of an array of 3D integrated FP filters.

L'utilisation de la microscopie de champ proche optique SNOM reste très limitée dû aux difficultés de mise en œuvre instrumentale. La sonde de champ proche est le cœur du microscope et la maîtrise de son utilisation (suppression d'un certain nombre de réglages optiques) constitue la clé technique de l'accès de cette méthode à un plus grand nombre d'utilisateurs. Ces travaux de thèse s'effectuent dans le contexte d'un projet qui consiste à réaliser la preuve de concept d'une sonde novatrice en matériau hybride organique/minéral, de type levier, intégrant une fonction optique. Dans la première partie, une étude bibliographique retrace l'historique des microscopies et donne le principe du champ proche optique. Ensuite, les différentes sondes commerciales de type fibre optique ou cantilever, à ouverture ou sans ouverture, ou autre, leurs avantages et inconvénients, leurs techniques de fabrication et les principaux matériaux utilisés sont présentés. En se basant sur cette étude bibliographique, on propose une nouvelle sonde à pointe pleine en matériau hybride qui associe les avantages de chaque type de sonde. Les raisons du choix du matériau hybride comme matériau de base de la sonde et ses caractéristiques sont aussi présentées dans cette partie. Dans une deuxième partie on détaille le procédé de fabrication du matériau (synthèse) ainsi que le rôle des différentes étapes dans ce procédé et les changements réalisées suite à des modifications des paramètres de la synthèse. Une caractérisation de ce matériau est aussi réalisée dans cette partie en mesurant son indice de réfraction et son module d'Young. La troisième partie est consacrée à la détermination des dimensions de la sonde qui permettent de maximiser le transfert de puissance optique en émission et réception. Ceci est fait en se basant sur une étude plus théorique au travers de simulations. L'effet de plusieurs paramètres sur la propagation de la lumière dans la sonde est étudié (longueur, largeur, épaisseur et raideur du levier ainsi qu'ouverture à l'extrémité de la pointe). La quatrième partie est dédié à la réalisation des sondes "micropoutres sol-gel" et aux caractérisations mécaniques et optiques associées. Elle présente le procédé de fabrication optimisé de sondes optiques couplant la définition des sondes par méthode de masquage et leur libération par gravure réactive ionique et gravure au fluorure de xénon "DRIE + XeF2". A partir de ce procédé, des guides d'ondes optiques ont été réalisés et caractérisés permettant la détermination des pertes optiques et donc du coefficient d'absorption du matériau hybride développé. La conclusion présente les perspectives ouvertes et en cours de ce travail dans le cadre d'un projet plus global. . / .The use of near-field optical microscopy SNOM is still very limited due to difficulties in instrumental work. The probe is the heart of the microscope and control its use (removal of optical settings number) is the technique key to access this method to a larger number of users. This thesis work is realized in the context of a project to achieve a concept proof for an innovative probe organic / inorganic hybrid material, lever type, incorporating an optical function. In the first part, the history of microscopy and the principle of the optical near field are described in a literature study. Then, the various commercial probes of optical fiber or cantilever type, with aperture or apertureless, or otherwise, their advantages and disadvantages, their manufacturing techniques and the main materials used are presented. Based on this literature study, we propose a new probe full tip hybrid material that combines the advantages of each type of probe. The choice reasons of the hybrid material as base material of the probe and its characteristics are also presented in this part. In the second part we detail the manufacturing process of the material (synthesis) as well as each step role in this process and changes made in response to changes in the synthesis parameters. Characterization of this material is also carried out in this part by measuring its refractive index and its Young's modulus. The third part is devoted to the determination of the probe dimensions to maximize the optical transmission and collection power based on a theoretical study through simulations. Several parameters effect on the light propagation in the probe is also studied (length, width, thickness and stiffness of the lever and aperture towards the end of the tip). The fourth part is dedicated to the probe achievement in hybrid material and associated mechanical and optical characterizations. It presents the manufacturing optimized process of optical probes coupling masking defining method probes and releasing method by reactive ion etching and etching xenon fluoride "DRIE + XeF2". Using this process, optical waveguides were realized and characterized for the determination of optical losses and therefore the absorption coefficient of the developed hybrid material. The conclusion presents open perspectives as part of a larger project.