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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
21

Silicon nanowires, nanopillars and quantum dots : Fabrication and characterization

Juhasz, Robert January 2005 (has links)
Semiconductor nanotechnology is today a very well studied subject, and demonstrations of possible applications and concepts are abundant. However, well-controlled mass-fabrication on the nanoscale is still a great challenge, and the lack of nanofabrication methods that provide the combination of required fabrication precision and high throughput, limits the large-scale use of nanodevices. This work aims in resolving some of the issues related to nanostructure fabrication, and deals with development of nanofabrication processes, the use of size-reduction for reaching true nanoscale dimensions (20 nm or below), and finally the optical and electrical characterization to understand the physics of the more successful structures and devices in this work. Due to its widespread use in microelectronics, silicon was the material of choice throughout this work. Initially, a fabrication process based on electron beam lithography (EBL) was designed, allowing controlled fabrication of devices of dimensions down to 30 nm, although, generally, initial device dimensions were above 70 nm, allowing the flexible but low-throughput EBL, to be replaced by state-of-the-art optical lithography in the case of industrialization of the process. A few main processes were developed throughout the course of this work, which were capable of defining silicon nanopillar and nano-wall arrays from bulk silicon, and silicon nanowire devices from silicon-on-insulator (SOI) material. Secondly, size-reduction, as a means of providing access to few-nanometer dimensions not available by current lithography techniques was investigated. An additional goal of the size-reduction studies was to find self-limiting mechanisms in the process, that would limit the impact of variations in the size and other imperfections of the initial structures. Thermal oxidation was investigated mainly for self-limited size-reduction of silicon nanopillars, resulting in well-defined quantum dot arrays of few-nm dimensions. Electrochemical etching was employed to size-reduce both silicon nanopillars and silicon nanowires down into the 10-nm regime. This being a novel application, a more thorough study of electrochemical etching of low-dimensional and thin-layer structures was performed as well as development of a micro-electrochemical cell, enabling electrochemical etching of fabricated nanowire devices with improved control. Finally, the combination of nanofabrication and size-reduction resulted in two successful device structures: Sparse and spatially well-controlled single silicon quantum dot arrays, and electrically connected size-reduced silicon nanowires. The quantum dot arrays were investigated through photoluminescence spectroscopy demonstrating for the first time atomic-like photoemission from single silicon quantum dots. The silicon nanowire devices were electrically characterized. The current transport through the device was determined to be through inversion layer electrons with surface states of the nanowire surfaces greatly affecting the conductance of the nanowire. A model was also proposed, capable of relating physical and electrical properties of the nanowires, as well as demonstrating the considerable influence of charged surface states on the nanowire conductance. / QC 20101101
22

Surface treated cp-titanium for biomedical applications : a combined corrosion, tribocorrosion and biological approach / Fonctionnalisations d’une surface de titane commercialement pur en vue d’applications biomédicales : une triple approche combinant corrosion, tribocorrosion et biologie

Yang, Yaqin 16 October 2014 (has links)
La tribocorrosion peut être définie comme l’ étude de l’influence des facteurs environnementaux (chimiques et/ou électrochimiques) et mécanique (frottement) sur le comportement tribologique de surfaces en mouvement relatifs. En raison de leurs caractéristiques particulières: performances mécaniques, associées à une faible densité, bonne tenue à la corrosion, biocompatibilité, le titane et ses alliages sont souvent utilisés dans le domaine médical comme implants dentaires et orthopédiques. Cependant, leur faible résistance vis-À-Vis du frottement en milieu agressif et plus spécifiquement biologique reste un frein à leur usage courant dans le domaine prothétique. Pour améliorer la résistance à la corrosion et à l'usure du titane et de ses alliages, différentes méthodes de modification de la surface ont été proposées durant ces dernières décennies. Dans ce cadre, le but de ce travail est de comparer les comportements en corrosion et tribocorrosion du titane commercialement pur (cp Ti), avec ce même matériau ayant subi au préalable les traitements suivants :- soit une étape d'oxydation thermique à 650 °C à l’air durant 48 h (formation d’un film d'oxyde de titane (TiO2) en surface),- soit un dépôt électrochimique de calcium phosphate (CaP) en surface,- soit un dépôt électrochimique de calcium phosphate (CaP) suivi d’une tape d’oxydation thermique à 650 °C à l’air durant 6 h (formation d’un dépôt de type CaP/TiO2 en surface). Les phases cristallines des films modifiés ont été identifiées par diffraction des rayons X (XRD). La microscopie électronique à balayage (MEB) en combinaison avec la spectroscopie à dispersion d'énergie (EDS) a été utilisée pour caractériser la morphologie et la composition de ces films.Le comportement en corrosion pure des échantillons cp Ti avec ou sans modifications de surface à été étudié in situ à partir des mesures électrochimiques de suivi du potentiel en circuit ouvert (OCP), de la spectroscopie d'impédance électrochimique (EIS) et du tracé de courbes de polarisation potentio-Dynamiques.Le comportement en tribocorrosion à été étudié quant à lui à l'aide d'un tribomètre de type pion-Disque apte à travailler en milieu aqueux et permettant outre l’enregistrement des paramètres tribologiques classiques, la mise en œuvre in situ des techniques électrochimiques utilisées lors de l’étude en corrosion pure. Caractérisation et analyses de la surface(composition, morphologie, rugosité …) sont effectuées avant et après chaque étude de comportement (corrosion et tribocorrosion). Un protocole pour la culture des cellules sur la surface de titane a été validé, en se basant sur les résultats expérimentaux préliminaires. / Tribocorrosion is defined as the study of the interplay between chemical, electrochemical and mechanical processes that leads to a degradation of passivating materials in a corrosive environment. Due to the low density, excellent mechanical properties, high corrosion resistance and good biocompatibility, titanium and its alloys are widely used as dental and orthopedic implants. However, the poor wear resistant and bio-Inert properties limit their further development as more efficient and economic biomedical implants. To improve the corrosion-Wear resistance and even bioactivity of metallic implants, different surface modification methods are imposed in the past decades.The aim of this work is to provide a deep insight in the area of corrosion and tribocorrosion behavior of commercially pure titanium (cp Ti) under the guidance of a tribocorrosion protocol for passivating materials. And then three different surface modification treatments, as:- one-Step thermal oxidation at 650 °C for 48 h in air atmosphere to form a titania (TiO2) film on the surface of cp Ti.- one-Step electrochemical deposition of calcium phosphate (CaP) bioactive film on the surface of cp Ti.- electrochemical deposition of CaP bioactive film followed by thermal oxidation at 650 °C for 6 h in air atmosphere to form a CaP/TiO2 bioceramic film on cp Ti surface.The crystalline phases of the modified films were identified by X-Ray diffraction (XRD). Scanning electron microscopy (SEM) combined with energy dispersive spectroscopy (EDS) was used to characterize the morphology and composition of these films on cp Ti surface. In situ electrochemical measurements, like open circuit potential (OCP), electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization are used to characterize the corrosion behavior of cp Ti samples without or with surface modification. The tribocorrosion behavior was investigated in an aqueous environment by combining a pin-On-Disc tribometer with the in situ electrochemical equipment. The classical tribological parameters could be also recorded under mechanical loaded condition. Surface characterization and analysis (like chemical composition, morphology, roughness...) are carried out before and after each corrosion and tribocorrosion test. A protocol for the culture of cells on the surface of titanium was validated, basing on the preliminary experimental results.
23

Degradação do colesterol submetido ao aquecimento na presença de ácidos graxos e antioxidantes = estudo em sistemas-modelo / Cholesterol thermal degradation in the presence of oxidants and fatty acids : model-system study

Nogueira, Gislaine Chrystina 03 March 2011 (has links)
Orientador: Neura Bragagnolo / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-17T18:17:21Z (GMT). No. of bitstreams: 1 Nogueira_GislaineChrystina_D.pdf: 842615 bytes, checksum: dfc01b70cfa919dc9a7f7698e623e3ea (MD5) Previous issue date: 2011 / Resumo: Uma das rotas de degradação do colesterol, quando submetido ao aquecimento em presença de oxigênio, é a formação de óxidos de colesterol (COP). Estes compostos têm sido associados a uma série de efeitos biológicos e doenças degenerativas e sua formação pode ser influenciada pela presença de outras substâncias, como antioxidantes e ácidos graxos. A influência dos antioxidantes está associada ao seu mecanismo de ação, que podem atuar nas fases de iniciação ou de propagação da oxidação lipídica. Já a influência dos ácidos graxos está associada com o grau de insaturação na molécula, em função da formação de radicais livres. Com o objetivo de verificar o comportamento do colesterol durante o aquecimento frente a influencia dessas substâncias, sistemas modelo contendo colesterol e ß-caroteno, TBHQ, vitamina E, ácido esteárico (saturado) ou ácido linolênico (com 3 insaturações), foram estudados. Os sistemas foram submetidos a 140, 180 e 220 °C, na presença de oxigênio, até que pelo menos 75% do colesterol fossem degradados. Os teores de colesterol, 7- hidroperoxicolesterol e COP foram avaliados ao longo do período de aquecimento. A degradação do colesterol foi observada em todas as temperaturas investigadas, ocorrendo em velocidade diretamente proporcional ao aumento da temperatura, totalizando aproximadamente 8 minutos a 220 °C, 20 minutos a 180 °C e 1 hora a 140 °C. De acordo com os resultados obtidos, a formação de COP atinge um máximo e a seguir sofre degradação, exceto na temperatura de 140 °C, em que o máximo da formação de COP só foi observado nos sistemas adicionados de ácidos graxos. A presença de ácidos graxos acelerou a formação de COP, entretanto, os sistemas contendo ácido linolênico apresentaram menores teores totais em todas as temperaturas estudadas e os sistemas contendo ácido esteárico apresentaram menores teores apenas a 220 °C, em comparação ao colesterol puro. Com exceção do TBHQ, a 140 °C, todos os antioxidantes estudados reduziram e/ou retardaram a formação de COP durante o aquecimento / Abstract: One of the pathways of cholesterol degradation, when it is submitted to heat, is the production of cholesterol oxidation products (COP). Those compounds have been associated to several biological effects and degenerative diseases and their formation can be influenced by other substances, such as antioxidants and fatty acids. The influence of the antioxidants is related to their mechanisms, which can act in the initiation and or propagation phases of the lipid oxidation. The influence of the fatty acids is associated to their degree of unsaturation, because of the free radical formation. In order to verify the cholesterol behavior during heating with the influence of those substances, model systems containing cholesterol and ß-carotene, TBHQ, vitamin E, stearic acid or linolenic acid, were studied. The model systems were heated at 140, 180 and 220 °C until at least 75% of cholesterol was degraded. The amount of cholesterol, COP and 7-hydroperoxycholesterol ¿ an intermediate compound of COP formation ¿ was evaluated during heating process. Cholesterol degradation was observed at all studied temperatures, occurring at a velocity directly proportional to the temperature increase, totalizing approximately 8 min at 220 °C, 20 min at 180 °C and 1 h at 140 °C. According to the obtained results, COP are formed reaching a maximum content and after that are degraded, but at 140 °C, the maximum was reached only at the systems containing fatty acids. The presence of fatty acids accelerated COP formation; however, the systems containing linolenic acid showed lower total content at all studied temperatures, on the other hand, the systems containing stearic acid showed lower content only at 220 °C, when compared to the pure cholesterol system. Except TBHQ, at 140 °C, all antioxidants were able to reduce and/or delay the maximum amount of total COP during heating / Doutorado / Doutor em Ciência de Alimentos
24

Thermo-oxydation des polyamides / Thermal oxidative degradation of polyamides

Okamba Diogo, Octavie 12 March 2015 (has links)
Les polyamides sont des thermoplastiques techniques qui entrent dans la conception de pièces destinées à remplacer certains composants métalliques des moteurs automobiles. En dépit de propriétés mécaniques initiales satisfaisantes, leur tenue à long terme est limitée par leur sensibilité à l'oxygène conduisant à des réactions de thermo-oxydation. Ces réactions ont été largement étudiées dans le cas des polyoléfines mais peu dans le cas des polyamides, rendant nécessaire l'élaboration d'un modèle cinétique susceptible de prédire la fragilisation donc la durée de vie des polyamides. Cette thèse est une contribution à la compréhension du processus d'oxydation dans le cas des polyamides aliphatiques et à la construction d'un modèle cinétique. La démarche cinétique réside tout d'abord dans la caractérisation physico-chimique multi-échelle de films de PA11 oxydés dans différentes conditions de températures (90 à 165 °C sous air) et sous différentes pressions partielles d'oxygène. Un modèle cinétique couplant oxydation et post-polycondensation est proposé ici : il permet de simuler les données expérimentales (hydroperoxydes, carbonyles et masse molaires) quelles que soient les conditions d'exposition. Parallèlement, un critère intrinsèque gouvernant la fragilisation du PA11 est identifié afin de prédire cette dernière à partir du modèle cinétique. Enfin, l'influence de l'ajout d'antioxydants phénoliques et des sels de cuivre sur la cinétique d'oxydation est caractérisée. Un premier modèle cinétique prenant en compte la stabilisation du PA11 décrit les tendances spécifiques de la stabilisation du PA11 comme l'apparition de la pseudo-période d'induction contribuant à une augmentation significative de la durée de vie du PA11. / Some metal components of automotive engine are bound to be replaced by polyamide parts. However, despite their thermal resistance polyamides are sensitive to oxygen leading to thermal oxidation chain reactions responsible for their long-term properties. While durability is critical for polyamide users, only a few studies deal with the elaboration of a kinetic model capable of predicting polyamide lifetime (time to embrittlement) in contrary to polyolefins (especially polyethylene). This PhD thesis is a contribution to the understanding of aliphatic polyamide thermal degradation by considering chemical and physical aspects of oxidation process in order to build a kinetic model. Our approach is based on a multi-scale physicochemical characterization of oxidized PA11 film samples under air between 90 and 165 °C but also under oxygen pressure. The proposed kinetic model coupling oxidation and solid state polymerization is able to simulate the whole experimental data (hydroperoxides, carbonyls and molar mass changes). In a same time, an intrinsic criterion for embrittlement is assessed to predict lifetime whatever the exposure conditions. Finally, the influence of phenols and copper salts on the oxidation kinetic is investigated. A first kinetic model including the phenol stabilizing effect is capable of simulating the main observed trends for stabilized PA11 such as the appearance of the pseudo induction period which contributes to the significant improvement of PA11 durability.
25

Uniformity of VO<sub>2</sub> Phase Change Material (PCM) Thin Films Produced by Thermal Oxidation of Vanadium

Zhang, Haixin 09 August 2021 (has links)
No description available.
26

Fyzikálně-chemické základy biokompatibility slitin přechodových kovů / Biocompatibility of transition metal alloys: physical-chemical background

Rafaj, Zdeněk January 2017 (has links)
Titanium alloys are widely used for manufacturing of bone implants. Recent studies proved superior mechanical and chemical properties of TiNb alloys. The performance of TiNb is analyzed on Ti39Nb alloy and on evaporated layers of Ti, Nb and TiNb. Performance is compared to Ti6Al4V and pure Ti. This work is focused on the early stage of a bone growth process (studied in vitro). An investigation of this early stage has not been found in any available literature. At this early stage, CaHPO4 compound is formed. This compound is accompa- nied by Mg oxide formation. It is a difference to later stage of this process (as observed in many studies) where the layer is created solely by hydroxylapatite, Ca10(PO4)6(OH)2. The thermal oxidation of surface leads to a grain structure and to a rougher surface. The surface with different roughness effects growth rate depending on material. Generally, the best performance is achieved with TiNb (only polished as well as subsequently thermally oxidized), followed by Ti. 1
27

Avaliacao da qualidade de oleos vegetais sob estresse fotoxidativo e termoxidativo por espectroscopia de UV e RMN e H

Tolentino, Marina Caldeira 14 April 2008 (has links)
Made available in DSpace on 2017-07-21T18:53:10Z (GMT). No. of bitstreams: 1 Resultados.pdf: 1211314 bytes, checksum: 38baa9c0e58df7dddd94d9184303e7b7 (MD5) Previous issue date: 2008-04-14 / Photo and thermal oxidation effects on the stability of refined soybean, corn, canola and sunflower oils was evaluated by spectroscopy and titration methods in this work. Oils samples were submitted to oven test (63°C – 45 days) and photoxidation (room temperature – 4000 lux – 60 days). The antioxidants addition effects was evaluated on the oil protection during photoxidation. The results showed that the canola oil is more resistant to thermal and photoxidation while the sunflower oil shows less resistance. Good correlations between peroxide values and ultraviolet and 1H NMR data were found (correlation coefficients 0.962 to 0.996). The ultraviolet data indicated that the antioxidants effectiveness on the photoxidation oil protection was: propyl gallate (PG) > tert-butyl hydroquinone (TBHQ) > butilated hydroxytoluene (BHT) > butilated hydroxyanisole (BHA) > citric acid. The results showed that UV and NMR are efficient techniques to monitoring antioxidants effects, oxidative changes and vegetable oil quality control under thermal or photochemical stress. / Neste trabalho foram avaliados os efeitos da fotoxidação e termoxidação na estabilidade dos óleos de soja, milho, canola e girassol, por técnicas titulométricas e espectroscópicas. As amostras foram submetidas ao oven test (63°C – 45 dias) e à fotoxidação (temperatura ambiente – 4000 lux – 60 dias). Foram avaliados também os efeitos da adição de antioxidantes na proteção dos óleos durante a fotoxidação. Os resultados indicaram que o óleo de canola é o mais resistente à oxidação térmica e fotoxidativa enquanto o óleo de girassol é o menos resistente. Foram obtidas excelentes correlações entre o índice de peróxidos e os dados de ultravioleta e RMN de 1H, cujos coeficientes de regressão variaram de 0,962 a 0,996. Os dados de ultravioleta indicaram que a eficiência dos antioxidantes na proteção de óleos vegetais sob estresse fotoxidativo foi: propil galato (PG) > terc-butil-hidroquinona (TBHQ) > butil-hidroxitolueno (BHT) > butilhidroxianisol (BHA) > ácido cítrico. Os resultados mostraram que a espectroscopia de ultravioleta e RMN de 1H são técnicas eficientes para monitorar os efeitos de antioxidantes, alterações oxidativas e controle de qualidade de óleos vegetais sob estresse térmico ou fotoquímico.
28

Réalisation de cellules solaires intégrées par oxydation localisée d'un substrat de silicium fritté poreux / Realization of integrated solar cell by localized oxidation of a porous sintered silicon substrate

Boye, Youssouf 12 February 2016 (has links)
Les travaux de recherche menés dans cette thèse s’inscrivent dans le cadre de la réalisation de la technologie cellule solaire intégrée (i-Cell), qui est une technologie innovante de fabrication de cellules solaires à hauts rendements de conversion et à bas coût de production. L’i-Cell consiste en la réalisation de plusieurs cellules élémentaires ou sous-cellules, en feuilles minces de silicium cristallin purifié, qui sont connectées en série sur un substrat de Si fritté bas coût. La technologie i-Cell permet en effet la réduction du coût de la plaquette grâce à la faible épaisseur des feuilles de silicium et grâce à l’utilisation de substrats issus du frittage de poudres de silicium. Dans une telle structure la fonction photovoltaïque est assurée par la feuille mince de surface alors que le transport du courant et la fonction mécanique sont gérés par le substrat fritté ce quipermet de réduire les coûts de fabrication de la cellule. En effet, à l’instar des couches minces, on peut décomposer la couche active en cellules de faibles surfaces et ainsi produire sur une surface standard (156 x 156 mm²), une cellule dans laquelle circule un faible courant qui permet de réduire fortement la consommation des métaux précieux au sein de la cellule (Argent) et entre les cellules du module (Cuivre). En outre, la configuration des cellules à i-Cell permet de s’affranchir des busbars en Ag traditionnellement utilisés dans les technologies silicium. Ceci présente l’avantage d’éviter le masquage de la lumière et donc d'augmenter la puissance de la cellule. Ce travail de thèse s’articule sur deux axes de recherche principaux. Le premier est orienté sur l’étude de la cinétique d’oxydation thermique de substrats de silicium frittés poreux. Le deuxième axe concerne la réalisation du substrat fritté intégré et la réalisation des premiers prototypes d’i-Cells sur ces derniers. Ce travail a permis de démontrer la faisabilité de l’i-Cell et de réaliser des prototypes d’i-Cell sur le substrat fritté intégré. Des rendements de conversion PV supérieurs à 18% ont été ainsi obtenus. / The research work conducted in this thesis are within the framework of the realization of the integrated solar cell technology (i-Cell), which is an innovative solar cell technology with a high conversion efficiency and a low cost production. The i-Cell consists of the realization of several elementary cells or sub-cells, in purified crystalline silicon thin foils, which are connected in series on a low cost sintered silicon substrate. In fact, the i-Cell technology allows the reduction of the cost of the wafer thanks to the low thickness of the silicon foils and through the use of substrates obtained from the sintering silicon powders. In such a structure, the photovoltaic function is provided by the thin purified Si foil on the surface. Whereas both the current transport and the mechanical function are provided by the sintered silicon substrate – thin allows to reduce the cell manufacturing costs. In fact, just like thin films, we can decompose the active layer in small cell surfaces and thus produce, on a standard surface (156 x 156 mm²), a low current cell that greatly reduces the consumption of precious metals within the cell (Silver) and between the cells within the module (Copper). Furthermore, the configuration of cells in the i-Cell technology permits to eliminate the use of Silver busbars traditionally used in the Si solar cell technologies. This offers the advantage of avoiding the masking light and thus increases the power of the i-Cell. This thesis work focuses on two main axes of research: The first axis relates to the study of the kinetics of thermal oxidation of porous sintered silicon substrates. The second axis of research focuses on the realization of the “integrated sintered substrates”, which consists of the realization of local conductive zones on the insulating porous sintered substrate, and the fabrication of the first i-Cells prototypes on them. This work demonstrated the feasibility of i-Cell and produced prototypes of i-Cell on the integrated sintered substrate. High photovoltaic conversion efficiencies, greater than 18%, were obtained.
29

Etude de l'oxydation thermique du titane et du zirconium sous irradiation aux ions d'argon dans le domaine du MeV (E ≤ 15 MeV)

Do, Ngoc-Long 21 November 2012 (has links) (PDF)
Nous avons montré que l'irradiation aux ions d'argon d'énergie comprise entre 1 et 15 MeV cause des dommages en surface du titane et du zirconium, qui prennent la forme d'une oxydation accélérée et/ou d'une cratérisation dont les effets évoluent en fonction de l'énergie du projectile et de l'atmosphère de recuit (température et pression), simulant les conditions environnementales représentatives de l'interface gaine/combustible d'un réacteur REP. Par AFM, nous avons montré que la surface du titane et du zirconium était attaquée par bombardement aux ions d'argon, à haute température (jusqu'à 500°C) en milieu faiblement oxydant (sous pression d'air sec raréfié comprise entre 5,7 10-5 Pa et 5 10-3 Pa) et à une dose moyenne fixée à environ 5 1014 ions.cm-2. On observe ainsi la formation de cratères nanométriques sur toute la surface du titane irradié entre 2 et 9 MeV et celle du zirconium irradié à 4 MeV, dont les caractéristiques varient en fonction de la température et de la pression. Dans le cas du couple Ar/Ti, l'efficacité d'endommagement superficiel augmente lorsque l'énergie du projectile diminue de 9 à 2 MeV. Par ailleurs, alors que la surface du titane apparaît transparente au faisceau d'ions à 15 MeV, celle du zirconium révèle de nombreux cratères micrométriques entourés d'un large halo sombre. Les caractéristiques des cratères (taille et densité superficielle) diffèrent de façon significative de celles observées à la fois dans le domaine des basses énergies (keV) où le dépôt d'énergie est contrôlé par les collisions balistiques (Sn) et dans le domaine des hautes énergies (MeV - GeV) où le dépôt d'énergie est contrôlé par les excitations électroniques (Se), ce qui n'était pas complètement inattendu dans le domaine d'énergie intermédiaire étudié, dans lequel des effets de pouvoir d'arrêt combiné Sn - Se sont envisageables. Par XPS couplé au décapage ionique, nous avons montré qu'il existe un effet d'irradiation sur l'oxydation thermique du titane, exacerbée sous faisceau d'ions d'argon entre 2 et 9 MeV, et qu'il existe aussi un effet d'énergie sur l'épaisseur et la stœchiométrie de l'oxyde. L'étude menée par Ellipsométrie Spectroscopique sur les films d'oxyde formés entre 1 et 9 MeV a corroboré ces résultats et montré précisément qu'il existe un pic d'oxydation en fonction de l'énergie d'ions d'argon, qui présente un maximum à 3 MeV, dans les conditions de l'expérience. Les mesures de gain d'oxygène effectuées par NBS confirment l'existence de ce pic d'oxydation. Les résultats acquis à ce jour par NBS concernant l'oxydation thermique du zirconium sous irradiation à l'argon de 4 et 9 MeV confirment les travaux antérieurs du groupe Aval du Cycle Electronucléaire de l'Institut de Physique Nucléaire de Lyon, et suggèrent fortement l'existence d'un pic d'oxydation dans la même plage d'énergie de projectile que pour le titane.
30

Mediation of Osteoblast Responses to Titanium Roughness by Adsorbed Proteins

Wilson, Cameron January 2005 (has links)
Stable fixation of implants such as artificial teeth depends on the direct apposition of bone to the implanted material. While endosseous implants were traditionally allowed to "osseointegrate" over several months without carrying load, clinical and experimental data show that prostheses with roughened surfaces allow successful integration when subject to earlier loading and more challenging implant sites. However, to design implant surfaces for an optimal biological response requires an understanding of the mechanism by which roughened surfaces promote osseointegration. Research into this mechanism has, to date, focussed primarily on the response of osteoblastic cells to surface topography in vitro. While these have demonstrated some consistent trends in cell behaviour, the fundamental means by which cells sense and respond to roughness remain unclear. It has been suggested that cell responses to changes in topography may relate to differences in the proteins adsorbed from serum (in vitro). While experimental evidence indirectly suggests that physical features can affect protein adsorption, few studies have examined this with respect to surface roughness, particularly as a mediator of cell responses. To address this issue, cell culture and protein adsorption experiments were conducted on a limited range of surface textures. Titanium samples were ground to produce morphologically similar surfaces with three grades of roughness. A duplicate set of specimens were heated at 600°C for one hour, with the aim of masking potential variations in physicochemical properties with differing degrees of grinding. Osteoblast attachment and proliferation studies were conducted over a short time-frame of 48 hours or less, to highlight the effects of proteins adsorbed from serum rather than secreted by adherent cells. Gel electrophoresis provided a profile of the proteins adsorbed to each surface after 15 minutes, corresponding to the time by which the cells had settled onto the surface. Finally, confocal microscopy was used to examine cell morphology on each surface, and to visualize specific interactions between cellular structures and adsorbed adhesion-mediating proteins. Although the effects were inconsistent, attachment assays showed some indications that fewer cells attached in the first 90 minutes as roughness increased. This inverse cell number-roughness trend was significant at 48 hours; however, the variability in attachment assays prevented reliable separation of attachment and proliferation rate effects. While the reduction in cell number with increasing roughness is consistent with previous reports, it is typically observed at later time points, and thus may be increasingly confounded by contact inhibition and differentiation. Thermal oxidation of the titanium did not impact on osteoblast responses to roughness, although it significantly slowed cell proliferation. The latter result was unexpected on the basis of previous reports. One-dimensional gel electrophoresis revealed no significant differences in the composition of adsorbed layers with variations in roughness. However, as expected on account of wettability changes, the heat-treatment did correspond to significant changes in the adsorption profile. While this was not a highly sensitive analysis, it suggests that the cell responses to roughness changes were not governed by broadscale differences in the proteins initially available to adhering cells. In addition to the composition of the adsorbed layer, the distribution of proteins may also vary with topography. The immunofluorescence methods were not sufficiently sensitive to reveal the distribution of adsorbed adhesion proteins (vitronectin and fibronectin). However, the lack of clear labelling does suggest an absence of large accumulations due to specific topographic features. Further work is required to address this issue conclusively. Observations of cell morphology were consistent with widely-reported contact guidance phenomena on grooved surfaces, with elongation and alignment (with topography) increasing with groove depth. Cell elongation was also enhanced on the more hydrophilic, heat-treated titanium, but this effect diminished over time. Although increased elongation at 90 minutes corresponded to lower cell numbers at 48 hours, no causal relationship has yet been established.

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