Les systèmes intelligents sont le résultat combiné de différentes avancées en microélectronique et en particulier de l’augmentation des puissances de calcul, la diminution des consommations d’énergie, l'ajout de nouvelles fonctionnalités et de moyens de communication et en particulier à son intégration et application dans notre vie quotidienne. L'évolution du domaine des systèmes intelligents est prometteuse, et les attentes sont élevées dans de nombreux domaines : pour la surveillance dans l'industrie, les transports, les infrastructures et l'environnement, ainsi que dans le logement, l'électronique grand public et les services de soins de santé, mais aussi dans les applications pour la défense et l’aérospatial. Aujourd’hui, l'intégration de plus en plus de fonctions dans les systèmes intelligents les conduisent vers un problème énergétique où l'autonomie devient le principal problème. Par conséquent, il existe un besoin croissant en capteurs autonomes et sources d'alimentation. Le développement de dispositifs de récupération d’énergie et de capteurs autoalimentés est une façon de répondre à ce problème énergétique. Parmi les technologies étudiées, la piézoélectricité a l'avantage d'être compatible avec l'industrie des MEMS. De plus elle génère des tensions élevées et elle possède un fort couplage direct entre les physiques mécaniques et électriques. Parmi les matériaux piézoélectriques, les nanofils (NFs) semi-conducteurs piézoélectriques pourraient être une option prometteuse car ils présentent des propriétés piézoélectriques plus importantes et une plus grande gamme de flexion.Parmi les différents NFs piézoélectriques, les NFs de ZnO et de GaN sont les plus étudiés. A l'échelle nanométrique leurs propriétés piézoélectriques sont plus que doublées. Ils ont l'avantage d'être compatible avec l’industrie microélectronique et raisonnablement synthétisable par des approches top-down et bottom-up. En particulier, nous avons étudié la croissance par voie chimique de NFs de ZnO. Pour les utiliser correctement, nous avons étudié le comportement des NFs de ZnO. Nous avons effectué une étude analytique et des simulations par éléments finis (FEM) d'un NF de ZnO en flexion. Ces études décrivent la distribution du potentiel piézoélectrique en fonction de la force et permettent d’établir les règles d'échelle et de dimensionnement. Ensuite, nous avons développé la caractérisation mécanique par AFM du module de Young de NFs de ZnO et de GaN, puis nous avons effectué des caractérisations piézoélectriques par AFM de ces NFs pour vérifier leur comportement sous des contraintes mécaniques de type flexion. Une fois leur comportement physique compris, nous discutons des limites de notre modèle de NFs piézoélectriques en flexion et nous développons un modèle plus réaliste et plus proche des configurations expérimentales. En utilisant ce nouveau modèle, nous avons évalué le potentiel des NFs de ZnO pour les capteurs de force et de déplacement en mesurant le potentiel généré sous une contrainte, puis, sur la base d’expériences, nous avons évalué l'utilisation de NFs de GaN pour les capteurs de force en mesurant le courant au travers des NFs contraints. De même, nous avons évalué le potentiel de ces NFs pour les applications de récupération d'énergie liées aux capteurs autonomes. Pour bien comprendre la problématique, nous avons étudié l’état de l’art des nano générateurs (NG) et leurs architectures potentielles. Nous analysons leurs avantages et inconvénients, afin de définir une structure de NG de référence. Après une brève étude analytique de cette structure pour comprendre son fonctionnement et les défis, nous avons effectué plusieurs simulations FEM pour définir des voies d'optimisation pour les NG utilisé en mode de compression ou de flexion. Enfin la fabrication de prototypes et leurs caractérisations préliminaires sont présentées. / Smart systems are the combined result of different advances in microelectronics leading to an increase in computing power, lower energy consumption, the addition of new features, means of communication and especially its integration and application into our daily lives. The evolution of the field of smart systems is promising, and the expectations are high in many fields: Industry, transport, infrastructure and environment monitoring as well as housing, consumer electronics, health care services but also defense and space applications. Nowadays, the integration of more and more functions in smart systems is leading to a looming energy issue where the autonomy of such smart systems is beginning to be the main issue. Therefore there is a growing need for autonomous sensors and power sources. Developing energy harvesters and self-powered sensors is one way to address this energy issue. Among the technologies studied, piezoelectricity has the advantage to be compatible with the MEMS industry, it generates high voltages and it has a high direct coupling between the mechanic and electric physics. Among the piezoelectric materials, semiconductor piezoelectric nanowires (NWs) could be a promising option as they exhibit improved piezoelectric properties and higher maximum flexion.Among the different piezoelectric NWs, ZnO and GaN NWs are the most studied, their piezoelectric properties are more than doubled at the nanoscale. They have the advantage of being IC compatible and reasonably synthesizable by top-down and bottom-up approaches. Especially we studied the hydrothermal growth of ZnO NWs. In order to use them we studied the behavior of ZnO NWs. We performed analytical study and FEM simulations of a ZnO NW under bending. This study explains the piezoelectric potential distribution as a function of the force and is used to extract the scaling rules. We have also developed mechanical AFM characterization of the young modulus of ZnO and GaN NWs. Following we perform piezoelectric AFM characterization of these NWs, verifying the behavior under bending stresses. Once physics understood, we discuss limitation of our piezoelectric NWs models and a more realistic model is developed, closer to the experimental configurations. Using this model we evaluated the use of ZnO NW for force and displacement sensors by measuring the potential generated, and from experiments, the use of GaN NW for force sensor by measuring the current through the NW. But energy harvesting is also necessary to address the energy issue and we deeper investigate this solution. To fully understand the problematic we study the state of the art of nanogenerator (NG) and their potential architectures. We analyze their advantages and disadvantages in order to define a reference NG structure. After analytical study of this structure giving the basis for a deeper understanding of its operation and challenges, FEM simulations are used to define optimization routes for a NG working in compression or in bending. The fabrication of prototypes and theirs preliminary characterization is finally presented.

Nous utilisons un microscope combinant microscopie à force atomique (AFM) et microscopie à effet tunnel (STM) à très basse température (~100 mK) afin d'étudier des nanocircuits mésoscopiques. Pour effectuer l'AFM dans ces conditions, nous utilisons un diapason en quartz recouvert de deux électrodes sur l'une desquelles est collée la pointe. Lorsque le diapason vibre on peut alors localiser en AFM un échantillon conducteur sur un substrat isolant, puis stopper les vibration pour réaliser des spectroscopies tunnel le long de la partie conductrice. Nous utilisons des pointes de platine-iridium ce qui nous permet de mesurer la densité d'états électronique locale. Nous nous sommes intéressés aux jonctions Josephson hybrides composées d'un îlot d'environ 1 µm de métal normal (cuivre) séparant deux supraconducteurs (aluminium). Ces échantillons sont réalisées par lithographie électronique et évaporation sous angle.Les courbes courant-tension de ces jonctions deviennent hystérétiques à très basse température ce qui est vraisemblablement dû à la dissipation thermique dans la partie normale. Nous avons pu localiser de manière fiable des échantillons uniques et effectuer simultanément des mesures en transport et des spectroscopies locales. Nous avons vu que la densité d'états du supraconducteur varie continuement à proximité du métal normal. Nous avons également observé un chauffage du supraconducteur avec le courant traversant la jonction. La mesure de la densité d'états du supraconducteur permet alors d'estimer la température électronique dans l'échantillon. La comparaison avec notre modèle thermique montre que l'énergie thermique produite dans le métal normal semble être évacuée mieux que prévu. / We use a microscope combining atomic force microscopy (AFM) and scanning tunneling microscopy (STM) at very low temperature (~100 mK) to study mesoscopic nanocircuits. To perform AFM measurements, we use quartz tuning forks covered with metallic electrodes on which we glue the tip. By using the tuning fork as a dynamic force sensor, we can localize the sample. Then, switching off the oscillation, we can perform local spectroscopies along the conductive part. We use platinum-iridium coated tips to measure the local density of states. This work is focused on hybrid Josephson junctions composed of a normal metal (copper) island of approximately 1 µm separating two superconductors (aluminium). These samples are made by electronic lithography and shadow evaporation.The current-voltage characteristics of these junctions become hysteretic at very low temperature because of thermal dissipation in the normal part. We achieved the localization of a unique sample and performed simultaneously transport measurements and local spectroscopies. We observed that the density of states of the superconductor varies continuously close to the normal metal. We also observed heating in the superconductor when the junction is current biased. The measure of the density of states of the superconductors gives an estimation of the electronic temperature in the sample. The comparison with our thermal model shows that the energy produced in the normal metal seems to be evacuated better than expected.

Esta tese apresenta o estudo do efeito do solvente acetato de etila e acetona no comportamento em solução dos polímeros acetato butirato celulose (CAB) e acetato butirato carboximetil celulose (CMCAB) e nas características dos seus filmes finos obtidos pela técnica de revestimento rotacional ou por adsorção. As medidas de viscosidade e espalhamento de raio-X a baixo ângulo (SAXS) mostraram que o acetato de etila é um melhor solvente para CAB e CMCAB do que a acetona. A caracterização dos filmes foi feita através de medidas de elipsometria, microscopia de força atômica (AFM), espectrocospia vibracional por geração de soma de freqüências (SFG) e medidas de ângulo de contato. Os filmes de CMCAB obtidos por revestimento rotacional são mais espessos quando preparado em acetona do que em acetato de etila. Imagens de AFM mostraram que os filmes de CMCAB oriundos de soluções em acetato de etila são mais homogêneos e lisos do que aqueles preparados a partir de acetona. Medidas de SFG comprovaram a forte afinidade da acetona com SiO2/Si, mostrando que esse solvente cria uma nova camada para os filmes de CAB e CMCAB. Os valores de energia superficial calculados para CAB e CMCAB foram semelhantes ~ (49,0 ± 0,5) mJ/m², sendo a contribuição da componente dispersiva maior que a da componente polar. A adsorção das proteínas lisozima, albumina do soro bovino (BSA), concanavalina A e jacalina foram mais pronunciadas sobre os filmes de CMCAB do que sobre CAB. Indicando que a presença do grupo carboximetil (CM) contribui significativamente no processo de adsorção das biomoléculas. O efeito da rugosidade dos filmes de CAB e CMCAB sobre o processo de adsorção das proteínas foi estudado. No caso do CMCAB, a adsorção das proteínas foi mais pronunciada sobre o filme rugoso do que sobre o filme mais liso. Entretanto, para os filmes de CAB a rugosidade não teve um efeito significativo na adsorção das proteínas / The effect of ethyl acetate and acetone on the solution behavior of cellulose acetate butyrate (CAB) and carboxymehtylcellulose acetate butyrate (CMCAB) and on the characteristics of films obtained either by spin coating or adsorption was investigated. Viscosity and small angle X-ray scattering (SAXS) measurements showed that ethyl acetate is a better solvent than acetone for CAB e CMCAB. Films were characterized by means of ellipsometry, atomic force microscopy (AFM), sum frequency generation (SFG) and contact angle measurements. Spin-coated films of CMCAB from ethyl acetate solutions were thicker than those deposited from acetone solutions. AFM images revealed that CMCAB spin coated films from ethyl acetate solutions were homogeneous and flat. However, films obtained from solutions in acetone were very rough. SFG spectra showed that acetone binds strongly to SiO2/Si wafers, creating a new surface for CAB and CMCAB films. Surface energy values determined for spin-coated CAB and CMCAB were similar ~ (49,0 ± 0,5) mJ/m² with the dispersive component larger than the polar component. The adsorption of lysozyme, bovine serum albumin (BSA), concanavalin A and jacalin was more pronounced onto CMCAB films than that onto CAB films. Indicating that carboxymethyl group favored the adsorption process. The influence of surface roughness of CAB and CMCAB on protein adsorption has been investigated. In the case of CMCAB, protein adsorption was morepronounced onto rough films than that onto flat films. However, the roughness of CAB films exerted no significant influence on proteins adsorption

FundaÃÃo Cearense de Apoio ao Desenvolvimento Cientifico e TecnolÃgico / As estruturas a base de carbono tem um papel de grande importÃncia nos campos da ciÃncia e da tecnologia. Isso graÃas à versatilidade do elemento carbono, pilar da quÃmica orgÃnica, que consegue formar uma diversidade de estruturas (cerca de 10 milhÃes de compostos), alÃm de ser um constituinte bÃsico de toda forma de vida conhecida. Dependendo das condiÃÃes de formaÃÃo, este fenomenal elemento, pode se apresentar em diversas formas alotrÃpicas: desde um material extremamente frÃgil, como o grafite, atà materiais incrivelmente resistentes como o diamante, nanotubos de carbono e o grafeno. Esses materiais grafÃticos tÃm sido extensivamente estudados, apresentando propriedades Ãnicas e grande potencial em aplicaÃÃes tecnolÃgicas. Dentre eles, o grafeno ocupa, atualmente, a posiÃÃo de maior destaque por possuir propriedades mecÃnicas e eletrÃnicas diferenciadas. O Ãxido de grafeno à uma classe de estruturas grafÃticas constituÃda basicamente de uma camada de grafeno decorada com grupos epÃxido e hidroxila na superfÃcie e grupos carboxÃlicos e carbonila nas bordas. A sua estequiometria depende fortemente do mÃtodo de obtenÃÃo. Esse material, alÃm de ser uma das principais rotas para a obtenÃÃo em larga escala do grafeno, tambÃm apresenta diversas propriedades interessantes, que possibilitam, por exemplo, aplicaÃÃes biolÃgicas, uma vez que seus grupos funcionais o tornam bastante reativo alÃm de ser facilmente dispersado em Ãgua. Muitas questÃes relacionadas ao Ãxido de grafeno ainda nÃo estÃo bem esclarecidas, como sua prÃpria estrutura, processo de formaÃÃo e mecanismos de interaÃÃo. Nesse sentido, foi utilizada, como principal ferramenta, a microscopia de forÃa elÃtrica (EFM) para estudar propriedades eletrostÃticas de uma amostra de Ãxido de grafeno obtida utilizando-se um mÃtodo de Hummer modificado. Por meio de um modelo simplificado, foi possÃvel desenvolver um mÃtodo para anÃlise das mediÃÃes de EFM e assim determinar a presenÃa e o sinal da carga lÃquida da amostra. AlÃm de ser possÃvel esclarecer a origem do fenÃmeno de borda observado nos experimentos de EFM. / Carbon-based structures have played a major role in scientific and technological fields. This is due to the versatility of the element carbon, the pillar of organic chemistry, which can form a variety of structures (about 10 million compounds), besides being a basic constituent of all known life forms. Depending on the conditions, this phenomenal element can occur in several allotropic forms: from an extremely brittle material, such as graphite, so incredibly resistant materials such as diamond, carbon nanotubes and graphene. These graphitic materials have been studied extensively, and present unique properties and great potential for technological applications. Among these materials, graphene currently occupies the most prominent position by having special electronic and mechanical properties. The graphene oxide is a class of graphitic structure consisting essentially of a graphene layer decorated with epoxide and hydroxyl groups on the surface and carboxyl and carbonyl groups on the edges. Its stoichiometry depends strongly on the method of production. In addition the graphene oxide is one of the main routes for obtaining large-scale graphene also it has several interesting properties, which allow, for example, biological applications, since their functional groups make it very reactive, besides being easily dispersed in water. Many issues related to graphene oxide are yet unclear, as also its structure, training procedure and mechanisms of interaction. Thus, the electric force microscopy (EFM) was used as the main tool to study electrostatic properties of a graphene oxide sample obtained by a modified Hummer method. By means of a simplified model, it was possible to develop a method for the analysis of the EFM measurements and so determine the presence and the sign of the net charge of the sample. Furthermore it is possible to clarify the origin of the edge phenomenon observed in EFM experiments.

A Na, K-ATPase (NKA) é uma proteína de membrana encontrada em organismos eucariotos multicelulares cuja atividade e funções já são amplamente discutidas na literatura. Sua unidade funcional corresponde a um heterodímero formado por duas subunidades , com regiões transmembrana. Espécies multiméricas como dímeros e tetrâmeros dessa enzima também são conhecidos por exercer atividade enzimática. As interações lipídio-proteína são intrínsecas para a NKA, por tal motivo, proteolipossomos constituídos de DPPC e DPPC:DPPE foram preparados por co-solubilização. Como controle, lipossomos de mesma composição foram produzidos por extrusão e/ou sonicação. Para as imagens de AFM, as amostras foram fixadas com glutaraldeído, para proteção mecânica e contra desidratação das vesículas. Para lipossomos de DPPC as imagens topográficas de AFM das vesículas apresentaram formato oval, superfície perfeitamente lisa e diâmetro médio de 151 + 46 nm, enquanto as vesículas de composição DPPC:DPPE, apesar de lisas, tiveram cantos pontiagudos e diâmetro médio de 98 + 28 nm. Imagens de fase de ambas as composições não apresentaram qualquer indicativo de diferenças na composição química, provavelmente devido à natureza de carga neutra dos dois fosfolipídios. As imagens de fase por AFM para os proteolipossomos tanto de DPPC-NKA, quanto DPPC:DPPE-NKA, revelaram resultados inéditos na literatura, onde a inserção da NKA aparece como nítidas regiões transições de fase de composição química distinta quando comparadas com os lipossomos. No entanto, as mudanças de fase são diferentes entre as composições estudadas, aparecendo como manchas escuras circulares para DPPC-NKA e mais visíveis como interstícios brilhantes para composição de DPPC:DPPE-NKA. As vesículas de DPPC-NKA apresentaram diâmetro médio de 390 + 326 nm e, nas imagens de topografia tridimensionais, protusões de 38 a 115 nm correspondentes às regiões de mudanças de fase, que, indicaram o diâmetro dos microdomínios relacionados à proteína. Já nas imagens para DPPC:DPPE-NKA o diâmetro médio dos proteolipossomos foi de 189 + 156 nm, e as protusões apareceram entre os interstícios, variando de 20 a 66 nm. O estudo de DSC dos lipossomos revelou que a concentração de glutaraldeído nas condições das análises de AFM, em torno de 5% (v/v), afetam as características físico-químicas para as composições com DPPE. A AFM foi eficiente para confirmar a reinserção da NKA em proteolipossomos pelas imagens de fase, e, para medir o diâmetro dos microdomínios pelas imagens de topografia. / Na, K-ATPase (NKA) is a membrane protein present in eukaryotic multicellular organisms. Its functions and activity are already widely described in the literature. Its minimal functional structure is a heterodimer of two main subunits , with transmembrane domains. However, dimers and tetramers of the enzyme are also known to have enzymatic activity. Since there are intrinsic lipid-protein interactions, NKA proteoliposomes composed of DPPC and DPPC:DPPE (1:1 molar ratio) were prepared by the co-solubilization method and liposomes of the same compositions were obtained by extrusion and/or sonication to be used as control. The samples to the AFM study were prepared using glutaraldehyde to protect the vesicles from mechanical shocks and dehydration. Liposomes composed of DPPC and DPPC:DPPE (1:1 molar ratio) were prepared by extrusion and sonication, respectively, as control. The topographical images for DPPC liposomes showed vesicles with an oval shape and smoothed surfaces with a mean diameter of 151 + 46 nm. DPPC:DPPE vesicles also presented smoothed surfaces, but with pointed corners and mean diameter of 98 + 28 nm. Phase images for both lipid compositions showed no differences in chemical composition. For DPPC:DPPE samples, this can be explained by the neutral net charge of both lipids. The proteoliposomes observed in the AFM phase images showed darker and large circular spots in the vesicles. These spots represent delays in the phase oscillation of the AFM probe and are associated with different chemical composition. The phase changes showed the reconstitution of the NKA in the proteoliposomes. When compared with topographical images, this spots matched protrusions. The mean diameter of DPPC-NKA proteoliposomes determined by AFM was 390 + 326 nm. In the three-dimensional topographical images of composition, protrusions from 38 to 115 nm near the areas of different phases indicate the diameters of the NKA microdomains. The phase changes for DPPC:DPPE-NKA appeared as bright interstices with the protrusions of the topographical images in between them. The size of these protrusions ranged from 20 to 66 nm and the mean diameter of the proteoliposomes was 189 + 156 nm. The DSC liposomes data showed that the glutaraldehyde concentration used in the AFM analysis affect the physical chemistry properties of the samples with DPPE. AFM proved to be an efficient method to confirm the reconstitution of into proteoliposomes with phase images and to determine the diameter of the protein microdomains with the topographical images.

Esta tese aborda a aplicação de técnicas avançadas de processamento e análise de imagens em problemas originais envolvendo imagens de microscopia de força atômica. Para isso, foi desenvolvida uma série de algoritmos para a caracterização e o entendimento do processo de formação de novos materiais poliméricos com perspectivas de inúmeras aplicações tecnológicas. As análises envolveram a determinação da orientação da morfologia de substratos para alinhamento de cristais líquidos, contagem e estimativa dos raios de domínios em filmes automontados POMA/PVS, análise do aumento da fotoluminescência em filmes PPV e estudos da curvatura espontânea de macromoléculas de polímeros. Dentre os algoritmos principais podemos citar a determinação da inclinação dos autovalores da matriz de covariância das coordenadas dos pontos da forma, aplicação da técnica dos máximos regionais e diagramas de Voronoi, filtros passabanda 2D através da transformada de Fourier e extração da curvatura multiescala. A implementação destes algoritmos envolveu algoritmos básicos de análise de imagens tais como esqueletização, dilatações exatas e extração do contorno de formas. A principal contribuição deste trabalho foi a implementação do software denominado SPIA (Scanning Probe Image Analysis) que possui ferramentas para análise e processamento de imagens incluindo todas as que foram utilizadas no decorrer deste trabalho além de outras ferramentas. Este software foi desenvolvido em ambiente Delphi sob o paradigma da orientação a objetos para plataformas Windows NT/9X/2000/XP. Possui uma interface amigável e semelhante a outros softwares dedicados a processamento de imagens. Todas as técnicas aplicadas foram testadas extensivamente e os resultados que corroboram sua eficiência são mostrados ao longo da tese / This thesis address the application of advanced techniques of processing and analysisof images in original problems involving images of atomic force microscopy. For this, a series of algorithms for characterization and understanding of process of formation of new polymeric materials was developed and implemented, with perspectives of many technological applications. The analysis was applied to the determination of orientation of the morphology of substrates for alignment of liquid crystals, counting and estimative of radiuses of granules in layer-by-layer polymer films, analysis of enhancement of photoluminescence in PPV cast films, as well as the study of curvature spontaneous of macromolecules. The principal algorithms included are determination of inclination of eigenvectors of matrix of covariance of coordinates of points of shape,application of regional maxima technique and Voronoi diagrams, passband filters 2D through Fourier Transform and curvature multiscale. The implementation of these algorithms involved a series of image analysis algorithms such as squeletonization, exact dilations and extracting of contour of shapes. The principal contribution of this work was to develop a software called SPIA (Scanning Probe Image Analysis) that includes tools for analysis of processing of images including that were used in this work. This software was developed in Delphi under object orientation paradigm to Windows NT/9X/2000/XP. It has a friendly interface similar to other image processing softwares. All this techniques were tested extensively and the results that corroborate the robustness of the algorithms are included throughout the thesis

Orientador: Jacobus Willibrordus Swart / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Elétrica e de Computação / Made available in DSpace on 2018-08-24T14:49:15Z (GMT). No. of bitstreams: 1 Garcia_AlissonSoares_M.pdf: 5063750 bytes, checksum: 2502df6540499f8d119aa5b993966ec5 (MD5) Previous issue date: 2014 / Resumo: Filmes ultrafinos (espessuras inferiores a 20 nm) de nitreto de titânio (TiN) para serem usados como eletrodos de porta para tecnologia CMOS (Complementary Metal Oxide Semicon-duc-tor) foram obtidos. Estes filmes ultrafinos foram obtidos através da evaporação por feixe de elétrons de camadas ultrafinas (de 1 ou 2 nm de espessura) de titânio (Ti) com posterior ni-tretação por plasma ECR (Electron Cyclotron Resonance) de nitrogênio (N2). Após a deposição e nitretação do titânio, a fim de evitar a oxidação dos filmes, no mesmo reator ECR da nitreta-ção, executou-se a deposição CVD (Chemical Vapor Deposition) de filmes de a-Si:H (silício amorfo hidrogenado) usando plasma de SiH4/Ar. Estes filmes de a-Si:H foram implantados com fósforo (P+) e recozidos por processamento térmico rápido para torná-los dopados n+ e policris-talinos. Assim, foram formados eletrodos de porta (Metal Gate) MOS com estruturas Poli-Si n+/TiN e esta dissertação apresenta as seguintes contribuições científicas: ¿ Obtenção de eletrodos de porta Poli-Si n+/TiN que suportam processos RTA em alta tempe-ratura de 1000 ºC. Esta característica foi observada por análises Raman, que identificaram picos relativos ao TiN dos modos TA (~195 cm-1) e LA (~315 cm-1) e ao Si cristalino (~ 521 cm-1); ¿ Obtenção de filmes ultrafinos de TiN, com espessuras menores que 20 nm e contínuos. Qua-tro amostras apresentaram espessuras menores que 10 nm, que é um valor desejado para ob-ter eletrodos de porta MOS que caibam nos dispositivos fabricados para nós tecnológicos com dimensões menores que 22 nm. Esta característica foi identificada por imagens SEM (microscopia eletrônica de varredura); ¿ Obtenção de eletrodos de porta Poli-Si n+/TiN do tipo midgap, pois os valores de VFB estão entre -0,31 V e -0,48 V. Estas características foram extraídas de medidas de Capacitância¿Tensão (C-V); Portanto, eletrodos de Poli-Si n+/TiN do tipo midgap, com espessuras menores que 10 nm, resistentes a processos de alta temperatura e que podem ser usados em dispositivos fabrica-dos para nós tecnológicos com dimensões menores que 22 nm, foram obtidos / Abstract: Ultrathin films (thickness of less than 20 nm) of titanium nitride (TiN) to be used as gate electrodes for CMOS (Complementary Metal Oxide Semiconductor) technology were obtained. These ultrathin films were obtained by electron beam evaporation of ultrathin layers (1 or 2 nm thick) of titanium (Ti) followed by ECR (Electron Cyclotron Resonance) plasma nitriding of nitrogen (N2). After deposition and nitriding of the titanium, in order to prevent oxidation of the films, in the same nitriding ECR reactor, a-Si:H (hydrogenated amorphous silicon) films were deposited by CVD (Chemical Vapor Deposition) using SiH4/Ar plasma. These films of a-Si:H were implanted with phosphorus (P+) and annealed by rapid thermal annealing to turn them n+ dopped and polycrystalline. Thus, MOS metal gate electrodes were formed with Poly-Si n+/TiN structures and this dissertation presents the following scientific contributions: ¿ Gate electrodes of Poly-Si n+/TiN that support RTA processes in high temperature of 1000 ºC were obtained. This characteristic was observed by Raman analysis, that identified peaks associated to TiN at TA mode (~195 cm-1) and LA mode (~315 cm-1), and related to the crys-talline Si at (~ 521 cm-1); ¿ Ultrathin films of TiN, less than 20 nm thick and continuous, were obtained. Four samples were less than 10 nm thick, which represents a thickness that is desirable to obtain MOS gate electrodes that fit devices manufactured for technological nodes with dimensions smaller than 22 nm. This feature was identified by SEM images (Scanning Electron Micros-copy); ¿ Midgap metal gate electrodes Poly-Si n+/TiN were obtained, as VFB values are between -0.31 V and -0.48 V. These features were extracted from measurements of capacitance-voltage (C-V); Therefore, midgap electrodes of Poly-Si n+/TiN, less than 10 nm thick, resistant to high temperature processes and that can be used in devices manufactured for technological nodes with dimensions smaller than 22 nm were obtained / Mestrado / Eletrônica, Microeletrônica e Optoeletrônica / Mestre em Engenharia Elétrica

Les sondes basées sur des résonateurs en quartz sont des capteurs disposant d'une autonomie en termes d'excitation et d'acquisition, et à cet égard présentent de nombreux avantages par rapport aux poutres cantilever qui ont jusqu'à présent dominé dans les applications de micro-caractérisation directe. Un de ces avantages est qu'elles peuvent êtres embarquées et calibrées sans recours à un système de déflection laser. Ces outils plus compacts et autosuffisants peuvent en conséquence être aisément intégrés et contrôlés au sein d'un microscope électronique à balayage, qui permet une observation globale rapide souvent privilégiée dans la recherche en micro-robotique. Le développement de ces sondes est de plus avantagé de par le fait qu'elles sont constituées de composants électroniques standards répandus dans le commerce, et qu'elles peuvent être adaptées à des usages spécifiques par l'ajout d'une micro-pointe. Les sondes de quartz dans la littérature sont cependant souvent basées sur des composants à fréquence d'oscillation limitée, et une plus grande vitesse d'opération serait utile à l'ensemble de leurs applications. C'est dans ce contexte que nous nous intéressons à des composants à plus haute fréquence, et au contrôle de sondes dans un microscope électronique propre à leur utilisation ciblée en micro-robotique et en imagerie. Les propriétés de ces sondes sont tout d'abord examinées dans le but de pouvoir évaluer et exploiter des résonateurs à plus haute fréquence; nous montrons ensuite que des sondes basées sur des résonateurs à cisaillement d'épaisseur atteignent de plus hautes vitesses en imagerie, ce qui les rend prometteuses pour des applications rapides ne requérant pas une haute résolution. Enfin, nous intégrons une sonde diapason dans un MEB, et établissons ainsi une preuve de concept pour la cartographie en raideur de micro-membranes fragiles. / As self-sensing and self-exciting tools, quartz probes present many advantages over the heretofore dominant silicon cantilevers for mechanical micro-sensing applications. One of these advantages is that they can be embedded and calibrated without the need for a laser deflection setup. The more compact and self-sufficient tools can therefore be readily integrated and controlled with Scanning Electron Microscopy, which is favoured at the smaller scales of micro-robotic research. More generally, the development and use of quartz probes is bolstered by the fact that they can be fabricated from widely commercialized quartz components and customised through the addition of a microtip. The quartz probes found in the literature are however largely based on components with limited oscillation frequencies, and could benefit from higher operating speeds. In this context, we address the frequency improvement and embedded control of AFM probes with regard to their use in targeted micro-robotics and imaging. The properties of quartz probes are first covered towards the evaluation and use of higher frequency components; we next demonstrate that faster scanning can be achieved with quartz probes made from thickness shear resonators, making them suitable for fast applications which do not require high sensitivity. Lastly, we integrate a tuning fork probe inside a SEM, and establish through it a proof of concept for the non-destructive stiffness mapping of fragile micro-membranes.

Le développement récent de la nanofluidique pose de nombreuses questions concernant les lois et longueurs caractéristiques qui régissent l’hydrodynamique et le mouillage à l’échelle du nanomètre. Pour aborder ce sujet, nous avons utilisé des techniques de microscopies avancées en sondant l’interface liquide/air à l’aide de pointes non conventionnelles. L’AFM utilisé dans le mode oscillant modulation de fréquence (FM-AFM) donne accès, de manière indépendante, à la force exercée par le liquide pendant une approche-retrait, et aux composantes conservatives et dissipatives de l’interaction pointe-ménisque. Des expériences complémentaires menées en microscopie électronique (MEB) permettent de visualiser le nanoménisque créé et de mesurer la force capillaire résultante. La couche visqueuse entraînée par l’oscillation de la pointe est d’abord étudiée. Le coefficient de friction et la masse ajoutée sont mesurés par FM-AFM en fonction de la viscosité des liquides et de la fréquence d’excitation. Un modèle basé sur une description classique rend compte quantitativement de l’ensemble des résultats expérimentaux permettant ainsi une évaluation du champ de vitesse entraîné par la nanosonde.Les méthodes développées ont permis d’étudier les caractéristiques de l’interface liquide. Le profil du nanoménisque est modélisé et validé grâce aux observations MEB. La raideur du ménisque mesurée expérimentalement par FM-AFM et décrite théoriquement démontre une dépendance logarithmique avec l’extension latérale du ménisque.Des résultats préliminaires sont également obtenus avec des pointes de carbone sur lesquelles glisse la ligne de contact, donnant accès à la dissipation dans le nanoménisque et à la ligne de contact, ainsi qu’à l’ancrage sur des défauts uniques, un des problèmes ouverts de la physique du mouillage.Cette étude démontre que le FM-AFM et le MEB sont des outils pertinents pour sonder quantitativement les propriétés des liquides à l’échelle nanométrique, ouvrant la voie à des études systématiques sur le mouillage à l’échelle nanométrique / The recent development of nanofluidic raises many issues about laws and characteristic lengths governing hydrodynamics and wetting at the nanometer scale. To address this issue, we used advanced microscopy techniques to probe the liquid/air interface with unconventional tips. The oscillating frequency modulation mode (FM-AFM) of the Atomic Force Microscope (AFM) gives independent access to the force applied by the liquid during an approach-withdrawal ramp, and to the conservative and dissipative components of the tip-meniscus interaction. Additional experiments conducted by electron microscopy (SEM) helped visualizing the shape of nanomeniscus to measure the resulting capillary force.The viscous layer set in motion by the oscillation of the tip is studied first. The friction coefficient and the added mass are measured by AFM-FM as a function of the viscosity of the liquid and of the excitation frequency. A model based on a classical description reflects quantitatively all experimental results enabling an evaluation of the velocity field caused by the nanoprobe.The developed methods also served to study the properties of the liquid interface. Nanomeniscus profile is modeled and validated through SEM observations. The stiffness measured experimentally by FM-AFM and described theoretically shows a logarithmic dependence with the lateral extension of the meniscus.Preliminary results are also obtained with carbon tips on which the contact line slides, giving access to the energy dissipation in the nanomeniscus and at the contact line, as well as to the anchoring of single defaults, an open issue of wetting physics.This study demonstrates that FM-AFM and SEM are relevant tools to probe quantitatively the properties of liquids at the nanoscale, opening the way for systematic studies on wetting at the nanoscale

Les prothèses diaphragmatiques en ePTFE utilisées dans la hernie diaphragmatique congénitale à large défect ont une faible étirabilité, ce qui entrainera des récidives herniaires au cours de la croissance de l’enfant. En effet, l’analyse en imagerie montre que la surface du diaphragme grandit de 4-5 fois jusqu’à l’adolescence. De plus, les mesures de rigidité des surfaces de prothèses explantés, montrent l’influence des contraintes mécaniques appliquées sur la structure des matrices extracellulaires néoformées. Afin de favoriser l’intégration tissulaire du ePTFE, nous avons testé un moyen de fonctionnaliser le ePTFE avec la polydopamine sur une seule face. Le revêtement nanoscopique favorise la colonisation cellulaire. Enfin, ce travail de thèse présente une méthode originale de réalisation d’une nouvelle membrane bicouche avec des propriétés mécaniques conformes aux exigences chirurgicales. Ce biomatériau innovant et prometteur fait actuellement l’objet d’une Déclaration d’invention. / Electron microscopy assessments of ePTFE prosthesis explants for diaphragmatic congenital hernia repair strongly suggest that the tissue responses are directly related to the surface microstructure of the biomaterial. AFM measurements (Young moduli) emphasize the influence of the mechanical stress applied to the implant on the mechanical properties of the newly formed extracellular matrices. In order to guide the host responses, we undertook to functionalize with polydopamine the ePTFE biomaterial. Electron microscopy investigations reveal the interest of that surface treatment regarding cell colonization of implant. To optimize that approach, we developed an original method aimed to coat only one face of the biomaterial. After determination of the growth rate of the diaphragm from birth to adolescence, we explored the possibility to design a new double-faced mesh able to follow body growth. From this point of view, the initial prototypes are promising and under patent application.