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Relations Structure/Composition/Propriétés de revêtements électrodéposés de nickel de taille de grain nanométrique / Relations between structure, composition and properties of electrodeposited nickel coatings with nanometric grain sizeGodon, Aurélie 03 December 2010 (has links)
Les travaux présentés dans ce mémoire ont pour but de mieux comprendre les relations entre la microstructure des revêtements métalliques nanocristallisés et leurs propriétés électrochimiques et mécaniques. Les dépôts de nickel sont élaborés par électrodéposition en courant continu et en courant pulsé dans un bain au sulfamate de nickel avec des sels de haute pureté, sans additif afin de minimiser les risques de contamination. Une caractérisation précise des états métallurgiques développés est réalisée au moyen de diverses techniques (MEB, MET, DRX, AFM, EBSD, SIMS, GDOES) afin d’évaluer la microstructure à différentes échelles (taille de grain, texture, contraintes internes, type de joints de grains) et d’identifier les contaminants. Trois types de texture ont été développés, associés à différentes tailles d’hétérogénéités structurales allant du micromètre à quelques dizaines de nanomètres. Une loi dite “d’échelle” a été mise en évidence, permettant de corréler les résultats obtenus par les diverses méthodes d’analyse. L’affinement de la taille de grain se traduit par une augmentation de la contamination dans les dépôts et entraîne une augmentation de la microdureté. La loi de Hall-Petch est influencée par l’orientation cristallographique ce qui a pu être relié à la nature des joints de grains et à la contamination des revêtements. Une étude préliminaire de la réactivité électrochimique en milieu acide a montré le rôle marqué des effets de surface (contamination et rugosité de surface). La réalisation d’un polissage électrolytique sur les revêtements a permis d’étudier l’influence des paramètres métallurgiques (taille de grain, contamination, nature des joints de grains) sur la réactivité. Les courbes de polarisation dans le domaine anodique et dans le domaine cathodique ont été simulées à l’aide de modèles cinétiques. Les résultats obtenus suggèrent que les joints de grains ont un effet qui peut être activant ou désactivant suivant l’étape considérée, ces effets pouvant être atténués par la présence d’impuretés. Les modifications de propriétés mécaniques et électrochimiques des revêtements ne peuvent être attribuées à une diminution de la taille de grain seule. / The purpose of the work presented in this manuscript is to better understand the relations between the microstructure of nanocrystallized metal coatings and their electrochemical and mechanical properties. Nickel deposits are elaborated by electrodeposition using direct current and pulse current in a nickel sulphamate bath with salts of high purity and without additive, in order to minimize the risks of contamination. A precise characterization of the developed metallurgical states is carried out by means of various techniques (SEM, TEM, XRD, AFM, EBSD, SIMS, GDOES) in order to evaluate the microstructure on various scales (grain sizes, textures, internal stresses, type of grain boundaries) and to identify contaminants. Three types of texture were developed associated with various sizes of structural heterogeneities from about one micrometer to a few dozens of nanometers. A “scale” law, allowing to correlating the results obtained by the various methods of analysis was shown. The grain size refinement results in an increase of contamination in the deposits and involves an increase of microhardness. The Hall-Petch law is influenced by the crystallographic orientation which could be connected to the nature of grain boundaries and the contamination of the coatings. A preliminary study of the electrochemical reactivity in acidic media showed the marked role of the surface effects (contamination and roughness of surface). Electrolytic polishing of the coatings highlights the influence of the metallurgical parameters (grain size, contamination, nature of grains boundaries) on the reactivity. The polarization curves in anodic domain and cathodic domains were simulated using kinetic models. The obtained results suggest that grain boundaries can either activate or deactivate the electrochemical kinetics according to the considered stage, these effects being able to be constrained by the presence of impurities. The modifications of mechanical and electrochemical properties of the coatings cannot be ascribed to a reduction of the grain size alone.
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Pollutant and Inflammation marker detection using low-cost and portable microfluidic platform, and flexible microelectronic platformLi-Kai Lin (6863093) 02 August 2019 (has links)
Existing methods for pathogen/pollutant detection or wound infection monitoring employ high-cost instruments that could only be operated by trained personnel, and costly device-based detection requires a time-consuming field-to-lab process. This expensive process with multiple prerequisites prolongs the time that patients must wait for a diagnosis. Therefore, improved methods for point-of-care biosensing are necessary. In this study, we aimed to develop a direct, easy-to-use, portable, low cost, highly sensitive and selective sensor platform with the goal of pollutant detection and wound infection/cancer migration monitoring. This study has two main parts, including microfluidic, electrical, and optical sensing platforms. The first part, including chapters 2, 3, and 4, focuses on Bisphenol A (BPA) lateral flow assay (LFA) detection; the second part, including chapter 5 focuses on the electrical sensing platform fabrication for one of the markers of inflammation, matrix metalloproteinases-9 (MMP-9), monitoring/detection. In chapters 2, 3, and 4, we found that the few lateral flow assays (LFAs) established for detecting the endocrine-disrupting chemical BPA have employed citrate-stabilized gold nanoparticles (GNPs), which have inevitable limitations and instability issues. To address these limitations, in chapter 2, a more stable and more sensitive biosensor is developed by designing strategies for modifying the surfaces of GNPs with polyethylene glycol and then testing their effectiveness and sensitivity toward BPA in an LFA. In chapter 3, we describe the development of a new range-extended bisphenol A (BPA) detection method that uses a surface enhanced Raman scattering lateral flow assay (SERS-LFA) binary system. In chapter 4, we examine advanced bisphenol A (BPA) lateral flow assays (LFAs) that use multiple nanosystems. The assays include three nanosystems, namely, gold nanostars, gold nanocubes, and gold nanorods, which are rarely applied in LFAs, compared with general gold nanoparticles. The developed LFAs show different performances in the detection of BPA. In chapter 5, a stable electrical sensing platform is developed for MMP-9 detection.
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