This dissertation explores the different ways to create thin film-based biosensors that are capable of rapid and label-free detection of cortisol, a non-specific biomarker closely linked to stress, within the physiological range of 10pM to 10 uM. Increased cortisol levels have been linked to stress-related diseases, such as chronic fatigue syndrome, irritable bowel syndrome, and post-traumatic stress disorder. It also plays a role in the suppression of the immune system as well. Therefore, accurate measurement of cortisol in saliva, serum, plasma, urine, sweat, and hair, is clinically significance to predict physical and mental diseases. In this dissertation, thin film-based electrochemical immunosensors were fabricated using a self-assembled monolayer (SAM) functionalized by cortisol specific antibodies to detect cortisol at 10 pM level sensitivities in the presence of a redox probe. The fabricated electrochemical cortisol immunosensors were able to detect cortisol in human saliva samples and the outcomes were validated using the standard Enzyme Linked Immuno Sorbent Assay (ELISA) technique. With the aim of improving signal amplification and label-free cortisol detection, copper nanoparticles were incorporated on screen-printed carbon electrodes (SPCE) for the fabrication of electrochemical cortisol immunosensor. This SPCE-based sensor showed a sensitivity of 4.21µA/M and the limit of detection 6.6nM. Both the SAM and SPCE-based immunosensors were not thermally stable due to the instability of antibodies at room temperature. To address this issue, an antibody-free immunosensor was fabricated. Molecular Imprinted Polymer (MIP) was used to template the target cortisol molecule. The MIP-based sensing platform was prepared using polypyrrole, a thermally stable conducting polymer. The conductivity of the polymer ensured good electrical performance. The polypyrrole-based MIP was synthesized by means of electrochemical polymerization and was used to detect cortisol within the physiological range at room temperature. MIP-based sensors exhibited the detection limit of 1 pM, and were cost-effective, easy to fabricate, temperature stable, and reusable. The sensing performance of the resulting sensors was comparable to those of commercially available technologies, such as ELISA. Aiming to perform cortisol sensing at point-of-care (POC), an Extended Gate Field Effect Transistor (EGFET) was integrated with a developed MIP cortisol sensor. The as developed MIP-EGFET sensor was used to detect the cortisol concentration in the range of 1 pM to 100 nM. A few of the major advantages of the developed sensor are its ability to provide a direct readout and simpler electronic systems, which are necessary for miniaturized Point of Care devices.

L’un des enjeux relatif au déploiement des piles à combustible à oxyde solide comme système de production d’une énergie propre relève de la température de fonctionnement qui est actuellement autour de 1000°C. Abaisser cette température tout en préservant les performances afin de réduire les coûts de fabrication et d’augmenter la durée de vie des systèmes a été l’objectif dece travail de doctorat.Un coeur de pile à combustible (anode-électrolyte-cathode) élaboré avec des procédés physiques de dépôts (projection par plasma atmosphérique et pulvérisation cathodique magnétron) a été développé et optimisé sur un support métallique poreux. Les matériaux étudiés ont été un cermet en Nickel-Zircone stabilisée à l’Ytttrium (Ni-YSZ) pour l’anode, un électrolyte en YSZ avec ou sans couche de cérine gadoliniée (GDC) et les nickelates de terres rares comme cathode. La maitrise des procédés de revêtements a permis de réduire les épaisseurs de chaque couche et d’assurer la cohésion de l’ensemble des 3 couches avec des caractéristiques cristallographiques, microstructurales et de porosité adaptées. . Les performances électrochimiques ont été étudiées pour chaque élément du coeur de pile puis pour l’ensemble du système élaboré sur métal poreux. Même si les performances atteintes ne sont pas encore suffisantes, les procédés de revêtements optimisés pour recouvrir un support métallique poreux ont confirmé leur potentiel. / Energy production by a clean and environmental processes is a real challenge. Fuel cell technology is good candidate to answer this objective. The major problem of the Solid Oxide Fuel Cell is their high operating temperature (around 1000°C) for a massive industrialisation. Decreasing these temperature at 700°C allows a reduction of cost manufacturing and increase the lifetime, in this case the new challenge is to avoid the performances losses.During this phD work, dry surface treatment processes are employed for produce the fuel cell core. The thickness reduction of each part limit the performances decreasing generate by the modification of the temperature. The materials used is a Ni-Yttria stabilised zirconia cermet (Ni-YSZ) for the anode, YSZ with or without gadolinnia doped ceria (GDC) for electrolyte and rare earth nickelate for the cathode component. All material are a usual employed in the SOFC technology. All coating are synthesized and characterised separately. After a third generation of fuel cell is realized on ITM porous metal support produced by PLANSEE. The anode has been deposit by atmospheric plasma spray, the electrolyte and cathode have been synthesised by reactive magnetron sputtering.

This thesis discusses the growth of thin-film silicon layers suitable for solar cells using liquid phase epitaxy and the behaviour of oxide LPCVD silicon nitride stacks on silicon in a high temperature ambient.¶ The work on thin film cells is focussed on the characteristics of layers grown using liquid phase epitaxy. The morphology resulting from different seeding patterns, the transfer of dislocations to the epitaxial layer and the lifetime of layers grown using oxide compared with carbonised photoresist barrier layers are discussed. The second half of this work discusses boron doping of epitaxial layers. Simultaneous layer growth and boron doping is demonstrated, and shown to produce a 35um thick layer with a back surface field approximately 3.5um thick.¶ If an oxide/nitride stack is formed in the early stages of cell processing, then characteristics of the nitride may enable increased processing flexibility and hence the realisation of novel cell structures. An oxide/nitride stack on silicon also behaves as a good anti- reflection coating. The effects of a nitride deposited using low pressure chemical vapour deposition on the underlying wafer are discussed. With a thin oxide layer between the silicon and the silicon nitride, deposition is shown not to significantly alter effective life-times.¶ Heating an oxide/nitride stack on silicon is shown to result in a large drop in effective Lifetimes. As long as at least a thin oxide is present, it is shown that a high temperature nitrogen anneal results in a reduction in surface passivation, but does not significantly affect bulk lifetime. The reduction in surface passivation is shown to be due to a loss of hydrogen from the silicon/silicon oxide interface and is characterised by an increase in Joe. Higher temperatures, thinner oxides, thinner nitrides and longer anneal times are all shown to result in high Joe values. A hydrogen loss model is introduced to explain the observations.¶ Various methods of hydrogen re-introduction and hence Joe recovery are then discussed with an emphasis on high temperature forming gas anneals. The time necessary for successful Joe recovery is shown to be primarily dependent on the nitride thickness and on the temperature of the nitrogen anneal. With a high temperature forming gas anneal, Joe recovery after nitrogen anneals at both 900 and 1000oC and with an optimised anti-reflection coating is demonstrated for chemically polished wafers.¶ Finally the effects of oxide/nitride stacks and high temperature anneals in both nitrogen and forming gas are discussed for a variety of wafers. The optimal emitter sheet resistance is shown to be independent of nitrogen anneal temperature. With textured wafers, recovery of Joe values after a high temperature nitrogen anneal is demonstrated for wafers with a thick oxide, but not for wafers with a thin oxide. This is shown to be due to a lack of surface passivation at the silicon/oxide interface.

<p>Idag används guld som kontaktmaterial på elektriska kontakter för lågströmstillämpningar. Guldhar emellertid låg nötningsbeständighet, är dyrt och miljömässigt påfrestande att utvinna. Ettalternativt kontaktmaterial till guld är nanokomposit Ti-Si-C-Ag belagt medlikströmsmagnetronsputtring. Nanokomposit Ti-Si-C-Ag har hittills belagts med sammansatt Ti-Si-C sputterkälla och separat silverkälla.</p><p>I detta arbete har filmer belagts från tre olika sammansatta Ti-Si-C-Ag-källor med tre olikakolhalter. Filmerna har belagts i två olika beläggningssystem: Ett konventionellt batchladdat ochett sekventiellt med sluss.</p><p>Filmernas fas- och ämnessammansättning har studerats med XRD och EDX. Tjocklek ochmikrostruktur har analyserats med SEM. Vidhäftning och resistivitet har analyserats medRockwellindentation och ytresistansmätning med fyrpunktsprob. Kontaktresistansen har ävenstuderats i begränsad mån.</p><p>Arbetet visar att ökat kolinnehåll i källan ger kolrikare filmer med större titankarbidkorn.Resistiviteten ökar p.g.a. tilltagen amorf fas mellan kornen men kontaktresistansen sjunker givetduktilare film.</p> / <p>Today gold is used as contact material on electric contacts for low current applications. Gold, however,has low wear resistance, is expensive and environmentally stressful to produce. An alternative contactmaterial to gold is nano composite Ti-Si-C-Ag deposited with DC-magnetron sputtering. Nanocomposite Ti-Si-C-Ag has so far been deposited by a compound Ti-Si-C sputter source with a separateAg source.</p><p>In this work films have been deposited by three different compound Ti-Si-C-Ag sources with threedifferent carbon contents. The films have been deposited in two separate PVD systems: Oneconventional batch loaded and one sequential with a load-lock.</p><p>The phase- and elemental composition of the films has been studied with XRD and EDX respectively.Thickness and microstructure have been analysed with SEM. Adhesion and resistivity has beenanalysed with Rockwell indentation and surface resistivity measurement with four point probe. Contactresistance has also been studied to a limited extent.</p><p>The work shows that the increment of carbon content in the source yields more carbon rich films withlarger titanium carbide crystallites. The resistivity is increasing due to an increased amorphous phasebetween the crystallites but the contact resistance is decreasing due to a more ductile film.</p>

<p>The high pressure and high temperature (HPHT) behavior of Ti_1-xAl_xN coatings on cutting tool inserts have been of interest for this diploma work. A literature study of HPHT techniques as well as measurement methods has been done. A diamond anvil cell (DAC) would be a good device to achieve high pressure and high temperature conditions on small samples. Another way to obtain these conditions would be a cutting test, which has been performed on a Ti_1-xAl_xN coated cutting tool insert with x = 0.67. Also a cubic press could be used to apply HPHT on a     Ti_1-xAl_xN sample or a large volume press on a whole cutting tool insert. To measure hardness on thin coatings a nanoindentor could be used, which have been done on heat-treated Ti_0.33Al_0.67N and TiN samples. X-ray diffraction (XRD) is a suitable method to measure phase composition of a sample and was performed on the cutting tested insert as well as on an untreated reference insert. Three ways to continue this project have been outlined all starting with more comprehensive cutting tests.</p>

Characterization of local boiling trends, in addition to the typically reported area-averaged trends, is essential for the robust design and implementation of phase change technologies to sensitive heat transfer applications such as electronics cooling. Obtaining the values of heat fluxes corresponding to locally varying surface temperatures has been a challenge limiting most investigations to area-averaged results. This thesis illustrates the importance of a spatially local heat transfer analysis during boiling. Pool and submerged jet impingement boiling scenarios on a silicon surface are considered at the macroscale (27.5 mm heater with multiple nucleation sites) and microscale (1000 ��m heater for isolated bubble generation), by the use of two thin film serpentine heater geometries. The macroscale heater highlights the effect of spatial variations in imposed heat flux on boiling heat transfer with a circumferentially uniform but radially non-uniform heat flux distribution. The microscale heater simulates a local hot-spot for spot cooling on an electronic device. Spatial variation in boiling heat transfer and bubble dynamics with and without a jet flow are documented using thin film voltage sensors along with qualitative and quantitative high speed imaging and infra-red thermography. Unique to this study is the documentation of local boiling curves for different radial locations on the heat transfer surface and their comparison with the corresponding area-averaged representations. It is shown here that sectionally averaged representations of boiling curves over regions of like-imposed heat flux can substantially simplify the interpretation of data while retaining important information of the local variations in heat transfer. The radial influence of the convective jet flow on the bubble dynamics and boiling heat transfer is assessed for a single circular submerged jet configuration. Varied parameters include jet exit Reynolds numbers, nozzle geometry, test fluid (deionized water and FC-72), fluid subcooling and the supplied heat flux. Distinct modifications of the surface temperature distribution imposed by the impinging jet flow are highlighted by comparing radial temperature profiles during pool and jet impingement boiling. It is demonstrated that in contrast with pool boiling, thermal overshoots during jet impingement boiling for a highly wetting fluid like FC-72 are highest in regions farthest from the impingement point. The effect of jet inertia on bubble departure characteristics are compared with pool boiling under subcooled conditions for FC-72. Qualitative high speed visualization indicates the presence of two modes of bubble generation during jet impingement boiling (a) bubble departure from the surface and (b) bubble separation from the source resulting in sliding bubbles over the surface. The effect of jet flow on bubble entrainment is depicted. Quantitative results indicate that in general departure diameters for pool and jet impingement boiling increase and plateau at a maximum value with increasing power input while no notable trends were observed in the corresponding departure frequencies. The largest departure diameters for jet impingement boiling at fixed fluid subcoolings of 10��C and 20��C were found to be smaller than that for the corresponding pool boiling test by a factor of 1.6 and 2.3, respectively. / Graduation date: 2013

The fields of health care and environment control have an increasing demand for sensors able to detect low concentrations of specific molecules in gaseous or liquid samples. The recent introduction of microfabricated devices in these fields gave rise to sensors with attractive properties. A cutting edge technology is based on guided acoustic waves, which are perturbed by events occurring at the nanometer scale. A first part of the thesis investigates the Love mode waveguide, a versatile structure in which a thin film is guiding the acoustic wave generated in a piezoelectric substrate. A systematic analysis of its sensitivity was obtained using a transmission line model generalized to discriminate the rigid or viscous nature of the probed layers. We developed a novel integrated combination of the Love mode device with a Surface Plasmon Resonance optical sensor to quantify the thickness and the composition of soft layers. The electromagnetic interferences in the recorded signal were modeled to determine the phase velocity in the sensing area and to provide new mechanisms for an enhanced sensitivity. The experimental aspects of this work deal with the fabrication, the important issue of the packaging and the sensitivity calibration of the Love mode biosensor. A second part of the thesis investigates nanocrystalline diamond under the form of a thin film membrane suspended to a rigid silicon frame. The high mechanical and chemical resistance of nanocrystalline diamond, close to single-crystal diamond, open ways to membrane based acoustic sensors such as Flexural Plate Wave and thin Film Bulk Acoustic Resonators (FBAR). A novel dynamic characterization of the thin film is reported and the properties of composite FBAR devices including a diamond thin film membrane and a piezoelectric aluminum nitride layer are assessed using the perturbation theory. This study is applied to evaluate the high sensing potential of the first prototype of an actual diamond-based composite FBAR.

The characterization and fabrication of active matrix thin film transistors (TFTs) has been studied for an addressable microfluidic electrowetting channel device as application. A new transparent semiconductor material, Amorphous Indium Gallium Zinc Oxide (a-IGZO), is used for TFT, which shows high electrical performance rather than amorphous silicon based TFT; higher mobility and even higher transparency. The purpose of this dissertation is to optimize each TFT process including the optimization of a-IGZO properties to achieve robust device for application. To minimize hysteresis of TFT curves, the gate dielectric is discussed extensively in this dissertation. By optimizing gas ratio of NH3SiH4, it is found that the TFT with NH3 rich SiNx gate dielectric deposited with NH3/SiH4 =5.1 and stoichiometric SiO2 demonstrates best condition to reduce hysteresis. a-IGZO films is investigated as a function of power and substrate bias effect which affects to electrical performance; the higher power and substrate bias increase the carrier density in the film and mainly cause threshold voltage(VT) to shift in the negative gate voltage direction and mobility to increase, respectively. In addition, the powerful method to estimate the electrical properties of a-IGZO is proposed by calculating O2 and IGZO flux during sputtering in which the incorporation ratio with O2/IGZO ≈1 demonstrates the optimized a-IGZO film for TFT. It is confirmed that both physical and chemical adsorption affects the electrical property of a-IGZO channel by studying TFT-IV characteristics with different pressure and analyzing X-ray photoelectron spectroscopy (XPS), which mainly affects the VT instability. The sputtered SiO2 passivation shows better electrical performance. To achieve electrically compatible (lower back channel current) a-IGZO film to SiO2 sputter passivated device, a-IGZO TFTs require oxygen rich a-IGZO back channel by employing two step a-IGZO deposition process (2nd 10nm a-IGZO with PO2 = 1.5mTorr on 1st 40nm a-IGZO with PO2=1mTor). Electrowetting microfluidic channel device as application using a-IGZO TFTs is studied by doing preliminary test. The electrowetting channel test using polymer post device platform is candidate for addressable electrowetting microfluidic channel device driven by active matrix type a-IGZO TFT.

Ph.D. / Electrical Engineering / A novel combinatory on-line technique coupling Electrochemistry (EC) with Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) for in-situ quantitative determination of the corrosion mechanism in magnetic thin film structures has been developed in this research. Detailed construction of a system and a comprehensive methodology was described in this dissertation. Uniformly coated multi-layer magnetic thin film samples with multi-elemental alloys containing CoCrPtB and CrMo/Cr on the Ni/P substrate were used in this research for demonstrations. In-situ quantifications conducted in a series of experiments revealed that elemental dissolution was a predominant mechanism during corrosion courses of metallic thin film materials. At the microscopic scale, using results from depletion rate determination as well as cross-sectional analyses of microstructures and magnetic features, elemental passivity was observed to occur, depending on corrosion conditions. Without external influences, surface topographic measurements indicated that passive film could be produced at the macro-scale. The dependence of the dissolution rate of each metallic ion of alloys on electrolyte concentration, potential bias, scanning rate, and corrosion duration suggested that the most critical influential factor in corrosion mechanisms was epitaxial microstructures with strongly-oriented arrangements of grains and grain boundaries. Through the use of cross-sectional microstructural analysis, including high resolution TEM micrography, electron FFT diffraction, and nano-probe with EDS profiling, variations of elemental spatial distributions at grains and grain boundaries due to the corrosion phenomena were discovered, which provided a comprehensive understanding of occurrences of micro-corrosion in thin film structures. Because of the unique magnetic property of magnetic thin films, extensive studies of field strengths from the surface were also performed in this research. Important magnetization variations were noticed when cross-sectional images were obtained. Finally, models of corrosion kinetics in the multiple layers of magnetic thin film structures were proposed.

The fields of health care and environment control have an increasing demand for sensors able to detect low concentrations of specific molecules in gaseous or liquid samples. The recent introduction of microfabricated devices in these fields gave rise to sensors with attractive properties. A cutting edge technology is based on guided acoustic waves, which are perturbed by events occurring at the nanometer scale. A first part of the thesis investigates the Love mode waveguide, a versatile structure in which a thin film is guiding the acoustic wave generated in a piezoelectric substrate. A systematic analysis of its sensitivity was obtained using a transmission line model generalized to discriminate the rigid or viscous nature of the probed layers. We developed a novel integrated combination of the Love mode device with a Surface Plasmon Resonance optical sensor to quantify the thickness and the composition of soft layers. The electromagnetic interferences in the recorded signal were modeled to determine the phase velocity in the sensing area and to provide new mechanisms for an enhanced sensitivity. The experimental aspects of this work deal with the fabrication, the important issue of the packaging and the sensitivity calibration of the Love mode biosensor. A second part of the thesis investigates nanocrystalline diamond under the form of a thin film membrane suspended to a rigid silicon frame. The high mechanical and chemical resistance of nanocrystalline diamond, close to single-crystal diamond, open ways to membrane based acoustic sensors such as Flexural Plate Wave and thin Film Bulk Acoustic Resonators (FBAR). A novel dynamic characterization of the thin film is reported and the properties of composite FBAR devices including a diamond thin film membrane and a piezoelectric aluminum nitride layer are assessed using the perturbation theory. This study is applied to evaluate the high sensing potential of the first prototype of an actual diamond-based composite FBAR.