La demande croissante d’électricité, notamment renouvelable, entraîne une croissance de l’éolien avec l’utilisation de pales en composite de plus en plus grandes. Pour réduire le cout de maintenance de ces structures composites, le suivi de santé structurel (SHM) au cours du temps permet d’évaluer le comportement de la structure, d’anticiper les dégradations et la maintenance. Dans ce cadre, le développement de capteurs, à base de résine époxy et de nanotubes de carbone, appelés Quantum Resistive Sensor (QRS), est présenté. Les QRS peuvent être attachés à la surface de la structure ou intégrés à cœur durant la séquence de drapage. Durant la polymérisation de la résine, le comportement électrique du QRS traduit l’évolution de la réticulation et de la température dans la structure. Suite au processus de fabrication, l’influence des paramètres extérieurs (température, humidité, vitesse de déformation, coefficient de Poisson…) sur les caractéristiques des QRS a été étudiée. Durant l’utilisation de la structure composite, les QRS ont également permis la détection et la propagation d’endommagements jusqu’à la fracture ultime. Les QRS représentent donc une solution potentielle comme capteurs SHM non intrusifs, permettant un suivi de la structure, de sa fabrication jusqu’à sa dégradation finale. / The growing demands for electrical energy, especially renewable, is boosting the development of wind turbines equipped with longer composite blades. To reduce the maintenance cost of such huge composite parts, the structural health monitoring (SHM) is an approach to anticipate and/or follow the structural behaviour along time. To do so, a proper instrumentation is necessary and has to be as less intrusive as possible. To this end, the development of carbon nanotube- epoxy Quantum Resistive Sensor (QRS) is presented. QRS can be as well glued on the surface or embedded in the core of the composite structure during the stacking sequence. During manufacturing, both the temperature and resin crosslinking can be detected with the change in the QRS electrical characteristics. Once the structural part is made, the effect of the external parameters (strain rate, temperature, humidity, Poisson ratio…) on the electrical characteristics of QRS has been studied. During the composite life, the QRS electrical behaviour has also demonstrate its capability to detect the initiation and propagation of damage until final failure. A non-intrusive monitoring with QRS of the structure life cycle, from manufacturing until final breakage is therefore possible.

Orientador: Luis Vicente de Andrade Scalvi / Banca: Margarida Juri Saeki / Banca: Tomaz Catunda / O Programa de Pós-Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi da Unesp / Resumo: A proposta deste trabalho é a investigação das propriedades elétricas e ópticas de filmes finos de dióxido de estanho (Sn'O IND. 2') obtidos via sol-gel e por solução alcoólica depositados via dip-coating, e, filmes de alumina ('Al IND. 2''O IND. 3') obtidos por deposição de filmes de alumínio (Al) via evaporação resistiva e tratamento térmico em diferentes ambientes, para promover a oxidação de Al. A investigação individual quanto às propriedades ópticas e elétricas desses materiais conhecer seu comportamento na forma de filmes, e estudar a região interfacial de Sn'O IND. 2' e 'Al IND. 2''O IND. 3'. As caracterizações estruturais dos filmes foram feitas por difração de raios-X (DRX), e, no caso dos filmes de alumina, utilizou-se também microscopia eletrônica de varredura (MEV) e microscopia óptica. Nas caracterizações ópticas foram utilizadas técnicas de espectroscopia na região do ultravioleta e no infravermelho próximo (UV-Vis-Nir). Tanto os filmes obtidos por meio alcoólico como obtidos via SGDC foram caracterizados como sendo de Sn'O IND. 2' de estrutura tetragonal do tipo rutilo, sendo que os filmes obtidos via processo alcoólico apresentaram condutividade elétrica maior do que os filmes obtidos via SGDC. Os resultados referentes aos filmes finos de alumínio indicam que independentemente da quantidade de camadas de alumínio depositadas e da atmosfera de tratamento térmico, tem-se a oxidação do alumínio à alumina ('Al IND. 2''O IND. 3'), sendo que a estrutura dominante depende da atmosfera de tratamento. A sua utilização como camada isolante no gate em dispositivo metal-óxido-semicondutor é viável, pois a corrente fonte-dreno apresenta valores significativamente maiores do que a corrente fonte-gate. / Abstract: The main goal of this work is the investigation of properties of tin dioxide (Sn'O IND. 2') and alumina ('Al IND. 2''O IND. 3) thin films. The first one was obtained through the sol-gel process as well as alcoholic solution, via dip-coating. The alumina thin films were obtained by resistive evaporation of aluminum (Al) followed by thermal annealing in distinct atmospheres, to promote the Al oxidation. The individual investigation of optical and electrical properties of these materials aims the knowledge of their behavior as thin films, which allows studying the interface layer of the heterojunction Sn'O IND. 2' e 'Al IND. 2''O IND. 3'. Structural characterization of films was carried out by X-ray diffraction (XRD) technique and particularly on the alumina films, scanning electron microscopy (SEM) and optical microscopy were done. For the optical characterization, wide spectra were obtained, with spectroscopy from ultraviolet to near infrared (UV-Vis-Nir). Either the films obtained in the alcoholic solution as well as via SGDC, where characterized as Sn'O IND. 2' of tetragonal structure of rutile type, and the films obtained through alcoholic process present electrical conductivity higher than the films obtained via SGDC. Results on aluminum thin films indicate that independent on the amount of deposited aluminum and thermal annealing atmosphere, the oxidation of aluminum to alumina ('Al IND. 2''O IND. 3) takes place, but the dominant alumina structure depends on the thermal annealing atmosphere. Besides, its utilization as insulating layer at the gate of a metal-oxide semicondutor device is achievable, because the source-drain current is significantly higher than the source-gate current. / Mestre

In recent years there has been an increased drive towards point of care testing (POCT), in which assays are performed at the site of the patient. This has many benefits, critically; the time for a result to be obtained will be significantly reduced, allowing for greater and more effective decision making. Many currently used bioassay methods are not affordable in resource poor areas where infectious disease is most prevalent, in order to combat this issue many research groups are attempting to miniaturise equipment for portability and make assays more affordable and therefore more accessible. With the aims of generating a new assay platform which is highly portable and affordable, the work in this thesis presents the development of several generic methods utilising nano- and micro-scale beads coated with aptamer which are then monitored interacting with target proteins with Tunable Resistive Pulse Sensing (TRPS). Aptamers are short oligonucleotide sequences which are capable of binding to a wide range of targets with high selectivity and comparable affinity to antibodies while possessing greater stability and have begun to challenge the role of antibodies. When aptamers bind a target, they often undergo a conformational change. In the assays described herein, this conformational change is key to the observed signal changes. TRPS is a pore-based system in which beads moving through a pore cause a measurable increase in resistance which can be used to derive particle size, concentration, and mobility. During the course of this thesis several template TRPS aptasensors have been developed. TRPS was successfully used to confirm the successful coating of nano- and micro-scale beads with DNA aptamers by monitoring an increase in electrophoretic mobility when the negatively charged DNA is added to the surface. Following on from this, TRPS was used to monitor the interaction of aptamer tagged beads with thrombin protein enabling thrombin detection down to 1.4 nM and the comparison of several thrombin-aptamers with results comparable to previously published SPR data. Thrombin was postulated to shield the negative DNA, resulting in a decrease in mobility, and the magnitude of this charge shielding was found to depend upon the binding mechanism of the aptamer used. This effect is not thought to be specific to our system nor to thrombin, the principles outlined here may be applied to other RPS technologies, or by interchanging of the aptamer, different proteins. In later chapters, this method is expanded to include multiplexed detection of growth factors and a significant improvement in signal. vi Following on from this, the controlled aggregation of avidin coated beads in the presence of biotinylated-BSA was explored. Factors impacting upon this assay were discussed including magnetic separation, particle size and particle concentration, and different methods of data interpretation were presented. This aggregation study identified several key parameters in the use of TRPS in aggregation assays. Using the methods outlined by the study of aggregates, a dispersion assay was then designed in which the interaction of thrombin proteins with clusters of particles brought about the release of many small particles by the disruption of double stranded DNA linkages. This dispersion assay incorporated magnetic separation to simplify the read-out and relied on measuring particle concentration rather than mobility, enabling the use of additional pressure to increase speed and ease of use. Using this method, thrombin was able to be detected down to 100 fM, a significant advancement in TRPS aptasensors.

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Integrating nanometer-sized pores into low-k ILD films is one of the approaches to lower the RC signal delay and thus help sustain the continued scaling of microelectronic devices. While increasing porosity of porous dielectrics lowers the dielectric constant (k), it also creates many reliability and implementation issues. One of the problems is the little understood metal ion diffusion and drift in porous media. Here, we present a rigorous simulation method of Cu diffusion based on Master equation with elementary jump probabilities within the contiguous dielectric film, along the pore boundary, from the dielectric matrix to the pore boundary, and from the pore boundary to the matrix material. In view of the diffusional jump distance being as large as 2 nm, the nano-pores being on a similar length scale, and the film thickness being only a few tens of nanometers, the conventional diffusion equation in differential equation form is grossly inadequate and elementary jump frequencies are required for a proper description of the Cu diffusion in porous dielectric. The present atomistic approach allows a consistent implementation of Cu ion drift in electric field by lowering and raising of the diffusion barriers along the field direction. This will help understand the behavior of Cu interconnects under thermal or electric stress at an atomistic level. Another approach to lower the increasing RC delays is to bring memory and logic closer by integrating memory in the BEOL. Resistive RAM is one such memory is not transistor based and thus, does not require a silicon substrate. Thus, it offers the possibility of integration directly into the back-end reducing memory to logic distance from 1000s of µm to a 10s of nm. This 3D integration also allows for increased density as well. However, one barrier in the implementation of RRAM in the back end is the use of expensive as well as non-BEOL native material in conventional Cu/TaOx/Pt resistive devices. In this thesis, we present our research about functionality of RRAM with porous low-k dielectrics (which are a candidate for CMOS ILD), and through the similar elementary jump simulations, discuss the impact of porosity in dielectrics on the functionality of RRAM. Lastly, we present a cheaper replacement for Pt as the counter electrode in RRAM and show that it functions as good as Pt. This work addresses following three areas: 1. Modeling of diffusion in porous dielectrics through elementary jump based simulation. The model is based on random walk theory of elementary particle jumps. Initially, qualitative simulations are conducted without actual parameters. It is shown that Cu diffusion in porous dielectrics decreases quasi-linearly with porosity. Furthermore, it is shown that morphology of the pores may have a greater effect on diffusivity compared to porosity. The simulations are then calibrated with parameters, and the result is shown to yield a similar diffusivity times as actual process time. 2. Modeling of Cu ions drift in porous dielectrics under electric stress. First, the model is explained, and then qualitative simulation results are presented for porous dielectrics with varied porosities and morphologies. 3. Research to find a suitable replacement for Pt as the counter electrode in RRAM devices. The research methodology is discussed and a much cheaper Rh is selected as the potential replacement for Pt. Successful functionality of Rh based resistive devices is presented. / Master of Science

In an effort to lower interconnect time delays and power dissipation in highly integrated logic and memory nanoelectronic products, numerous changes in the materials and processes utilized to fabricate the interconnect have been made in the past decade. Chief among these changes has been the replacement of aluminum (Al) by copper (Cu) as the interconnect metal and the replacement of silicon dioxide (SiO2) by so called low dielectric constant (low-k) materials as the insulating interlayer dielectric (ILD). Cu/low-k structure significantly decreases the RC delay compared with the traditional interconnect (Al/SiO₂). Therefore, the implementation of low-k dielectric in Cu interconnect structures has become one of the key subjects in the microelectronics industry. Incorporation of pores into the existing low-k dielectric is a favorable approach to achieve ultra low-k ILD materials. To bring memory and logic closer together is an effective approach to remove the latency constraints in metal interconnects. The resistive random access memories (RRAM) technology can be integrated into a complementary metal-oxide-semiconductor (CMOS) metal interconnect structure using standard processes employed in back-end-of-line (BEOL) interconnect fabrication. Based on this premise, the study of this thesis aims at assessing a possible co-integration of resistive switching (RS) cells with current BEOL technology. In particular, the issue is whether RS can be realized with porous dielectrics, and if so, what is the electrical characterization of porous low-k/Cu interconnect-RS devices with varying percentages of porosity, and the diffusive and drift transport mechanism of Cu across the porous dielectric under high electric fields. This work addresses following three areas: 1. Suitability of porous dielectrics for resistive switching memory cells. The porous dielectrics of various porosity levels have been supplied for this work by Intel Inc. In course of the study, it has been found that Cu diffusion and Cu+ ion drift in porous materials can be significantly different from the corresponding properties in non-porous materials with the same material matrix. 2. Suitability of ruthenium as an inert electrode in resistive switching memory cells. Current state-of-the-art thin Cobalt (Co)/Tantalum Nitride (TaN) bilayer liner with physical vapor deposited (PVD) Cu-seed layer has been implemented for BEOL Cu/low-k interconnects. TaN is used for the barrier and Co is used to form the liner as well as promoting continuity for the Cu seed. Also, the feasibility of depositing thin CVD ruthenium (Ru) liners in BEOL metallization schemes has been evaluated. For this study, Ru is used as a liner instead of Ta or Co in BEOL interconnects to demonstrate whether it can be a potential candidate for replacing PVD-based TaN/Ta(Co)/Cu low-k technology. In this context, it is of interest to investigate how Ru would perform in well-characterized RS cell, like Cu/TaOx/Ru, given the fact that Cu/TaOx/Pt device have been proven to be good CBRAM device due to its excellent unipolar and bipolar switching characteristics, device performance, retention, reliability. If Cu/TaOx/Ru device displays satisfactory resistive switching behavior, Cu/porous low-k dielectric/Ru structure could be an excellent candidate as resistive switching memory above the logic circuits in the CMOS back-end. 3. Potential of so-called covalent dielectric materials for BEOL deployment and possibly as dielectric layer in the resistive switching cells. The BEOL reliability is tied to time dependent failure that occurs inside dielectric between metal lines. Assessing the suitability of covalent dielectrics for back-end metallization is therefore an interesting topic. TDDB measurements have been performed on pure covalent materials, low-k dielectric MIM and MI-semiconductor (MIS) devices supplied by Intel Inc. / Master of Science

Current research has developed a fully predictive model of an electrically heated common residential oven. This system was modeled using a fully explicit approach and, where applicable, considered natural convective correlations, various radiation networks, and conduction relations. Two oven configurations were modeled, a conventional (unmodified) residential oven and a modified design. By comparing the theoretical results obtained through modeling with experimental results, verification of the modeling assumptions and results has been achieved. This research has produced an analytical design tool for predictive modeling of time dependant surface temperatures, maximum expected temperatures, and the baking performance of various oven designs. Thus this software package can be used to predict the overall feasibility of an oven design prior to fabrication.

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