The current thesis focuses on the deformation behaviour and strain distribution in the microstructure of ductile iron during tensile loading. Utilizing Digital Image Correlation (DIC) and in-situ tensile test under optical microscope, a method was developed to measure high resolution strain in microstructural constitutes. In this method, a pit etching procedure was applied to generate a random speckle pattern for DIC measurement. The method was validated by benchmarking the measured properties with the material’s standard properties. Using DIC, strain maps in the microstructure of the ductile iron were measured, which showed a high level of heterogeneity even during elastic deformation. The early micro-cracks were initiated around graphite particles, where the highest amount of local strain was detected. Local strain at the onset of the micro-cracks were measured. It was observed that the micro-cracks were initiated above a threshold strain level, but with a large variation in the overall strain. A continuum Finite Element (FE) model containing a physical length scale was developed to predict strain on the microstructure of ductile iron. The materials parameters for this model were calculated by optimization, utilizing Ramberg-Osgood equation. For benchmarking, the predicted strain maps were compared to the strain maps measured by DIC, both qualitatively and quantitatively. The DIC and simulation strain maps conformed to a large extent resulting in the validation of the model in micro-scale level. Furthermore, the results obtained from the in-situ tensile test were compared to a FE-model which compromised cohesive elements to enable cracking. The stress-strain curve prediction of the FE simulation showed a good agreement with the stress-strain curve that was measured from the experiment. The cohesive model was able to accurately capture the main trends of microscale deformation such as localized elastic and plastic deformation and micro-crack initiation and propagation.

La réalisation de dispositifs à des dimensions sous-micrométriques et nanométriques demande une maîtrise parfaite des procédés de fabrication, notamment ceux de gravure. La réalisation des ces dispositifs est complexe et les exigences en termes de qualité et de géométrie des profils de gravure imposent de choisir les conditions opératoires les mieux adaptées. Les simulations de l'évolution spatio-temporelle des profils de gravure que nous proposons dans cette thèse s'inscrivent parfaitement dans ce contexte. Le simulateur que nous avons réalisé offre la possibilité de mieux comprendre les processus qui entrent en jeu lors de la gravure par plasma de profils dans divers matériaux. Il permet de tester l'influence des paramètres du plasma sur la forme du profil et donc de déterminer les conditions opératoires optimales. La mise au point de ce simulateur s'appuie sur les concepts fondamentaux qui gouvernent la gravure par plasma. À partir de l'état des lieux des différentes approches numériques pouvant être utilisées, nous avons élaboré un algorithme stable et adaptable permettant de mettre en évidence l'importance de certains paramètres clés pour la réalisation de profils de gravure par un plasma à haute densité et à basse pression. Les capacités de cet algorithme ont été testées en étudiant d'une part la pulvérisation de Si dans un plasma d'argon et d'autre part, la gravure chimique assistée par les ions de SiO2/Si dans un plasma de chlore. Grâce aux comparaisons entre profils simulés et expérimentaux, nous avons montré l'importance du choix de certains paramètres, comme la nature du gaz utilisé et la pression du plasma, la forme initiale du masque, la sélectivité masque/matériau, le rapport de flux neutre/ion, etc. Nous avons aussi lié ces paramètres à la formation de défauts dans les profils, par exemple celle de facettes sur le masque, de parois concaves, et de micro-tranchées. Enfin, nous avons montré que le phénomène de redépôt des atomes pulvérisés entre en compétition avec la charge électrique de surface pour expliquer la formation de profils en V dans le Pt pulvérisé par un plasma d'argon. / Sub-micrometer and nanometer-size device manufacturing requires perfect control of fabrication processing, in particular plasma etching. The fabrication of such devices is complex and the requirements in terms of quality and geometry of the etching profiles impose to use the best adapted operating conditions. Simulation of space and time-etching profile evolution that is proposed in this thesis addresses these issues. The simulator yields a better understanding of the fundamental mechanisms that occur during plasma etching of features in various materials. It enables to test the influence of plasma parameters on the profile shape and thus to determine the optimal operating conditions. The development of the simulator is based on the fundamental concepts in plasma etching. From thorough review of the various numerical approaches available to simulate etching profile evolution, we have developed a stable and flexible algorithm that enables to emphasize the importance of some key-parameters for the realization of etching profiles by high-density and low-pressure plasma. The capabilities of this algorithm were tested on the study of Si sputtering in an argon plasma and of ion-assisted chemical etching of SiO2/Si in a chlorine plasma. From comparisons between simulated and experimental profiles, we have shown the importance of some parameters, like the nature of the gas, the plasma pressure, the initial shape of the mask, the mask/material selectivity, the neutral/ion flux ratio, etc. We also linked these parameters to the formation of defects in the profile, for exemple mask facetting, sidewall bowing and microtrenching. Finally, we have shown that redeposition of sputtered atoms compete with electric surface charging to explain V-shape profiles observed on Pt sputtered in argon plasmas.

En lien avec l’avancée rapide de la réduction de la taille des motifs en microfabrication, des processus physiques négligeables à plus grande échelle deviennent dominants lorsque cette taille s’approche de l’échelle nanométrique. L’identification et une meilleure compréhension de ces différents processus sont essentielles pour améliorer le contrôle des procédés et poursuivre la «nanométrisation» des composantes électroniques. Un simulateur cellulaire à l’échelle du motif en deux dimensions s’appuyant sur les méthodes Monte-Carlo a été développé pour étudier l’évolution du profil lors de procédés de microfabrication. Le domaine de gravure est discrétisé en cellules carrées représentant la géométrie initiale du système masque-substrat. On insère les particules neutres et ioniques à l’interface du domaine de simulation en prenant compte des fonctions de distribution en énergie et en angle respectives de chacune des espèces. Le transport des particules est effectué jusqu’à la surface en tenant compte des probabilités de réflexion des ions énergétiques sur les parois ou de la réémission des particules neutres. Le modèle d’interaction particule-surface tient compte des différents mécanismes de gravure sèche telle que la pulvérisation, la gravure chimique réactive et la gravure réactive ionique. Le transport des produits de gravure est pris en compte ainsi que le dépôt menant à la croissance d’une couche mince. La validité du simulateur est vérifiée par comparaison entre les profils simulés et les observations expérimentales issues de la gravure par pulvérisation du platine par une source de plasma d’argon. / With the reduction of feature dimensions, otherwise negligible processes are becoming dominant in microfabricated profile evolution. Improved understanding of these different processes is essential to improve the control of the microfabrication processes and to further decrease of the feature size. To help attaining such control, a 2D feature scale cellular simulator using Monte-Carlo techniques was developed. The calculation domain is discretized in square cells representing empty space, substrate or mask of the initial system. Neutral and ion species are inserted at simulation interface from their respective angular and energy distributions functions. Particles transport to the feature surface is calculated while taking into account ion reflection on sidewall and neutral reemission. The particles-surface interaction model includes the different etching mechanisms such as sputtering, reactive etching and reactive ion etching. Etch product transport is also taken into account as is their deposition leading to thin film growth. Simulation validity is confirmed by comparison between simulated profiles and experimental observations issued from sputtering of platinum in argon plasma source.

Une étape cruciale dans la fabrication des MEMS de haute fréquence est la gravure par plasma de la couche mince d’AlN de structure colonnaire agissant comme matériau piézoélectrique. Réalisé en collaboration étroite avec les chercheurs de Teledyne Dalsa, ce mémoire de maîtrise vise à mieux comprendre les mécanismes physico-chimiques gouvernant la cinétique ainsi que la formation de dommages lors de la gravure de l’AlN dans des plasmas Ar/Cl2/BCl3. Dans un premier temps, nous avons effectué une étude de l’influence des conditions opératoires d’un plasma à couplage inductif sur la densité des principales espèces actives de la gravure, à savoir, les ions positifs et les atomes de Cl. Ces mesures ont ensuite été corrélées aux caractéristiques de gravure, en particulier la vitesse de gravure, la rugosité de surface et les propriétés chimiques de la couche mince. Dans les plasmas Ar/Cl2, nos travaux ont notamment mis en évidence l’effet inhibiteur de l’AlO, un composé formé au cours de la croissance de l’AlN par pulvérisation magnétron réactive et non issu des interactions plasmas-parois ou encore de l’incorporation d’humidité dans la structure colonnaire de l’AlN. En présence de faibles traces de BCl3 dans le plasma Ar/Cl2, nous avons observé une amélioration significative du rendement de gravure de l’AlN dû à la formation de composés volatils BOCl. Par ailleurs, selon nos travaux, il y aurait deux niveaux de rugosité post-gravure : une plus faible rugosité produite par la présence d’AlO dans les plasmas Ar/Cl2 et indépendante de la vitesse de gravure ainsi qu’une plus importante rugosité due à la désorption préférentielle de l’Al dans les plasmas Ar/Cl2/BCl3 et augmentant linéairement avec la vitesse de gravure. / A crucial step in the fabrication of high-frequency MEMS is the etching of the columnar AlN thin film acting as the piezoelectric material. Realized in close collaboration with researchers from Teledyne Dalsa, the objective of this master thesis is to better understand the physico-chemical mechanisms driving the etching kinetics and damage formation dynamics during etching of AlN in Ar/Cl2/BCl3 plasmas. In the first set of experiments, we have studied the influence of the operating parameters of an inductively coupled plasma on the number density of the main etching species in such plasmas, namely positive ions and Cl atoms. These measurements were then correlated with the etching characteristics, in particular the etching rate, the surface roughness, and the chemical properties of the AlN layer after etching. In Ar/Cl2 plasmas, our work has highlighted the inhibition effect of AlO, a compound formed during the AlN growth by reactive magnetron sputtering and not from plasma-wall interactions or from the incorporation of moisture in the columnar nanostructure of AlN. In presence of small amounts of BCl3 in the Ar/Cl2 plasma, we have observed a significant increase of the etching yield of AlN due to the formation of volatile BOCl compounds. Furthermore, our work has demonstrated that there are two levels of roughness following etching: a lower roughness produced by the presence of AlO in Ar/Cl2 plasmas which is independent of the etching rate and a larger roughness due to preferential desorption of Al in Ar/Cl2/BCl3 plasmas which increases linearly with the etching rate.

Current leakage in GaN thin films limits reliable device fabrication. A variety of Ga and N rich MBE GaN thin films grown by Rf, NH3, and Rf+ NH3, are examined with electrical measurements on NiIAu Schottky diodes and CAFM. Current-voltage (IV) mechanisms will identify conduction mechanisms on diodes, and CAFM measurements will investigate the microstructure of conduction in GaN thin films. With CAFM, enhanced conduction has been shown to decorate some extended defects and surface features, while CAFM spectroscopy on a MODFET structure indicates a correlation between extended defects and field conduction behavior at room temperature. A remedy for poor conduction characteristics is presented in molten KOH etching, as evidenced by CAFM measurements, Schottky diodes, and MODFET's. The aim of this study is to identify anomalous conduction mechanisms, the likely cause of anomalous conduction, and a method for improving the conduction characteristics. Keywords: 111-Nitride, 111-V, Gallium Nitride, GaN, Electrical Properties, Conduction, Conductivity, Mobility, Hall Measurements, Resistivity, Schottky Diode, Modulation Doped Field Effect Transistor (MODFET), Conductive Atomic Force Microscopy (AFM), Defects, Molten Potassium Hydroxide (KOH) etching, Silvaco, Atlas, and Illumination.

Die Siliciumauflösung in Flusssäure-Wasserstoffperoxid- und Flusssäure-Ozon-Lösung ist aufgrund der, aus der Oxidation des Siliciums, formal resultierenden Reaktionsprodukte Wasser und Sauerstoff interessant. Der Auflösungsprozess, speziell die Oxidation des Siliciums / Elektronenlochinjektion ins Siliciumvalenzband, wird – verglichen mit anderen Ätzsystemen für Silicium – massiv kinetisch gehemmt. Ätzprozesse auf Basis dieser Mischungen sind hinsichtlich der geringen bzw. moderaten erzielbaren Siliciumabtragsraten (rSi < 0,02 nm s-1 mit Rissaufweitung in Flusssäure-Wasserstoff-peroxid-Lösungen bzw. rSi < 0,61 nm s-1 mit Oberflächenpolitur in Flusssäure-Ozon-Lösungen) wenig effektiv. Eine Erhöhung der Siliciumabtragsraten gelingt prinzipiell durch die Erhöhung der Konzentrationen siliciumoxidierender Spezies in der Silicium / Elektrolyt-Grenzfläche oder durch Zufügen geeigneter grenzflächenaktiver Elektronenüberträgerspezies. In stark sauren Lösungen wird der Elektronentransfer zusätzlich durch stabilisierende Wasserstoffaustauschprozesse inhibiert. Die Mischungen sind zur Reinigung von Siliciumwaferoberflächen oder feinteiligem Silicium geeignet.

Devido a alterações químico-estruturais causadas pelo clareamento, os substratos dentais poderiam tornar-se mais susceptíveis a perda tecidual, principalmente se expostos a desafios erosivo/abrasivos. Desta forma, o presente estudo teve como objetivos: 1) analisar in vitro, se o esmalte e a radicular dentina clareada com diferentes agentes e concentrações, apresenta uma maior susceptibilidade ao desgaste, quando submetido a ciclos de erosão e abrasão; 2) comparar o efeito da aplicação de um agente clareador a base de peróxido de carbamida a 10% a um placebo no desgaste do esmalte e da dentina radicular, através de um modelo in situ. Os resultados do estudo in vitro mostraram que, independentemente do agente usado, o clareamento não aumentou o desgaste do esmalte frente a episódios erosivo-abrasivos. Na dentina, o desgaste foi dependente do agente clareador aplicado. Baseado no protocolo in situ adotado, o peróxido de carbamida a 10% não causou maior desgaste superficial no esmalte, mas aumentou a perda de tecido dentinário comparado ao placebo. Pode-se concluir que, em termos de desgaste superficial, o esmalte não foi afetado pelo tratamento clareador, enquanto a dentina mostrou-se mais susceptível. Assim, sugerem-se cuidados adicionais na seleção do agente clareador em situações clínicas que apresentam dentina radicular exposta. / Due to the chemical and microstructural alterations caused by bleaching, the dental substrates can become more susceptible to tissue loss, mainly if exposed to erosive/abrasive challenges. Therefore, the present study had the following objectives: 1) to analyze in vitro, if enamel and root dentin that had been bleached with different agents and concentrations, were at increased risk of wear when submitted to cycles of erosion and abrasion; 2) to compare the effect of the application of a 10% carbamide peroxide bleaching agent to a placebo on wear of enamel and root dentin, through an in situ model. The results of the in vitro study showed that independent of agent used, the bleaching demonstrated no increase in the wear of enamel when exposed to the erosive-abrasive episodes. In dentin, the wear was dependent on the bleaching agent applied. Based on the in situ protocol adopted, the 10% carbamide peroxide did not cause higher wear on the enamel, but increased the wear of the root dentin compared to the placebo. It could be concluded that in terms of superficial wear, enamel was not affected by bleaching treatment, while dentin showed to be more susceptible. Thus, additional caution is suggested in the choice of the bleaching agent when root dentin is exposed.

Novos métodos de remoção do tecido cariado tem sido propostos, entre eles a utilização de lasers, abrasão a ar e químico-mecânico. Este trabalho teve o objetivo de avaliar a influência de diferentes métodos de remoção de cárie na resistência de união de um sistema adesivo autocondicionante. Cinquenta molares humanos cariados extraídos foram desgastados para expor uma superfície plana onde a lesão de cárie se encontrava rodeada por dentina hígida. Os dentes foram divididos em 05 grupos (n=10), com um total de 50 dados, de acordo com o método de remoção do tecido cariado, como segue: G1 - sem remoção; G2 - remoção com lixa; G3 – broca de aço esférica em baixa rotação; G4 - laser de Er, Cr: YSGG e G5 - Carisolv. Procedimentos adesivos foram realizados com o sistema autocondicionante (Clearfil SE Bond – Kuraray – Japão), de acordo com as instruções do fabricante. Um cilíndro de resina composta (Z250- 3M do Brasil) foi construído sobre a superfície com o sistema adesivo e estocados em água (24 horas a 37 0 C). Os corpos de prova foram seccionados verticalmente para obtenção de fatias e em seguida confeccionadas ampulhetas em dentina infectada, afetada e sadia, com área aproximada de 1mm 2. As ampulhetas foram montadas em dispositivos de micro-tração e ensaiados na máquina de teste (Mini-Instron) com velocidade de 0,5mm/min. Os resultados obtidos mostraram que existem diferenças estatisticamente significantes entre os substratos sadio e infectado para o grupo G1e sadio e afetado para os grupos G2, G3 e G5. Em dentina sadia, o método utilizado em G3 resultou em valores de adesão superiores com relação a G4 e G2 foi estatisticamente superior com relação a todos os grupos. Os métodos de remoção de dentina infectada utilizados em G2 e G3 resultaram em valores de adesão superiores com relação a G1(dentina infectada). Desta forma podemos concluir que: o tipo de substrato influencia significativamente na resistência adesiva do sistema autocondicionante testado. A adesão à dentina sadia é mais efetiva que à dentina infectada (G1) e à dentina afetada obtida após remoção do tecido infectado com lixa (G2), broca (G3) e Carisolv (G5). Entretanto, para o laser de Er,Cr:YSGG (G4) não houve evidência amostral que sugerisse maior efetividade na adesão da dentina sadia com relação à dentina afetada. A adesão em dentina sadia mostrou-se mais efetiva quando esta foi instrumentada com lixa. Porém, trata-se de um recurso laboratorial de padronização dos espécimes. A utilização da broca de aço resultou em uma superfície mais favorável a adesão, quando comparada à obtida após irradiação com laser de Er, Cr: YSGG, em dentina sadia. A adesão em dentina infectada é pobre, ficando ressaltada a necessidade da remoção deste tipo de dentina, preferencialmente com lixa ou broca, previamente a adesão com sistema autocondicionante. Para os demais métodos de remoção da dentina infectada testados, não houve evidência amostral para se detectar a existência de diferenças significantes na resistência adesiva em dentina afetada. / New methods for carious dentine removal have been proposed, such as, lasers and chemo-mechanical. This in vitro study aimed to evaluate the influence of caries removal methods (steel burs, Er, Cr: YSGG laser and Carisolv) on microtensile bond strength of self-etching adhesive systems. 50 extracted carious human molars were ground to expose flat surfaces where caries lesion was surrounded by normal dentine. Teeth were divided into 5 groups (n=10), with 50 original data, according to the removal method used: G1 - no removal; G2 - abrasive paper, G3 - steel burs; G4 – Er, Cr: YSGG laser (79, 61 J/cm 2 ) and G5 – Carisolv. Surfaces were bonded with Clearfil SE Bond, according to manufacturers’ instructions. A crown was built up using composite resin (Z250- 3M Brasil). After storage in water (24 h, 37 0 C), teeth were vertically serially sectioned into slices and trimmed into an hourglass shape with about of 1mm 2 area at the adhesion interface, that contained either infected, caries affected and normal dentine. Samples were tested in tension in a Instron machine at 0,5mm/min. Results showed that there is a significant difference between tested groups (p< 0.005). Significantly lower results were found for caries infected dentin when compared to normal dentin values (G1). A significant difference was also found when caries affected and normal dentin were compared (G2, G3, G5). In normal dentin, G2 showed better bond strenght than another groups and G4 showed lower results than G3. G2 and G3 caries infected dentin removal methods showed better bond strength than the other groups when compared with G1 (caries infected dentin). The results indicated that: bond strength of a self-etching system to normal dentin was better than to caries infected (G1) and caries affected dentin after the use of abrasive paper (G2), round steel bur (G3) and Carisolv (G4). However, there was no difference between caries affected and normal dentin after the use of ErCr:YSGG laser (G4); abrasive paper is a laboratorial method to create smear layer and it was responsable for the best bond strength to normal dentin. The usage of Er, Cr: YSGG laser negatively altered adhesion of self-etching system on normal dentin when compared with round steel bur; infected dentin is not an adequate substrate for adhesion. Abrasive paper and round steel bur are the best caries infected dentin removal methods. There were no difference in bond strength to caries affected dentin when the other methods were used.

Este trabalho é o resultado de uma pesquisa envolvendo estudos, reflexões e experimentações poéticas que buscam problematizar a percepção visual sobre a representação bidimensional e sobre a realidade cotidiana - o conjunto aqui apresentado reúne textos reflexivos, imagens produzidas (desenhos, pinturas e gravuras) e anotações sobre o processo. Num primeiro momento, ele centra na exploração das possibilidades em torno da construção de um efeito flutuante na visualidade imagética, tentando tensionar os modos de apreender a representação bidimensional. Num segundo momento, ele acrescenta a seu quadro de reflexões uma indagação sobre a experiência visual na realidade cotidiana, mais especificamente no deslocamento diário pela cidade de São Paulo, e tenta abordar a paisagem urbana pela perspectiva da representação flutuante. Como um meio de aprofundar certas questões que permeiam o processo poético, são apresentadas três reflexões independentes sobre temas distintos: 1. a espacialidade na tradição pictórica sino-japonesa do Suibokuga; 2. a relação entre cor e linguagem na pintura de Mark Rothko; e 3. possibilidades de se orientar visualmente pela cidade de São Paulo a partir da referência a algumas características básicas compreendidas nas construções espaciais da cultura japonesa. Esses textos tem como objetivo complementar as imagens produzidas, tentando mapear o conjunto de inquietações que impulsionaram o seu desenvolvimento. / The present work is the result of a process involving studies, reflections and poetic experiments which seek to approach the visual perception of the two-dimensional representation and the everyday reality - the contents presented here gather together reflexive texts, produced images (drawings, paintings and engravings) and notes on the process. At first, the process focused on the exploration of possibilities surrounding the construction of a floating effect on visual imagery, attempting to generate discomfort and doubts on the ways of visually apprehending the two-dimensional representation. Secondly, it adds to its set of reflections an inquiry about the visual experience in everyday reality, specially in the daily routine in the city of São Paulo, and attempts to approach the urban landscape from the perspective of the floating representation. As a mean to develop certain issues that permeate the poetic process, three independent reflexive texts about distinctive themes are here presented: 1. one about spatiality in Sino-Japanese pictorial tradition of Suibokuga; 2. one about the relationship between color and language in Mark Rothko\'s paintings; and 3. one about possibilities for one to visually guide himself through the city of São Paulo from the point of view of some basic features inherent to spatial constructions of Japanese culture. These texts have the objective to supplement the images produced along the poetic process, in an attempt of mapping the set of concerns which drove its development.

O processo de criação fundamenta esta pesquisa. A vivência entre a paisagem da Praia da Daniela em Florianópolis, Santa Catarina, e o ateliê com a gravura em metal, suas especificidades e possibilidades gráficas, levaram à elaboração deste livro de artista. O que procuro são aproximações entre o estuário vivo e em constante movimento transformador da paisagem da Praia da Daniela com o meu estuário fictício, que segue na busca de um contínuo formar, desafiando o metal, provocando reações e transformações que acontecem em sua materialidade. / This is a practice-based research in which the creative process is at it\'s core. The construction of this artist\'s book is a fruit of the lived experience between two places: the landscape at the Daniela Beach, in Florianopolis, Santa Catarina, Brazil, and the printmaking studio, considering the specificities and graphic possibilities of the Etching technique. What I seek is to interweave the living and transforming estuary in constant movement of the landscape at Daniela Beach, and my own fictitious estuary, which continuously seeks to give form, defying the nature of the metal, provoking reactions and transformations that happen in its materiality.