One of the many promising applications of metal/ceramic joining is in biomedical implantable devices. This work is focused on vacuum brazing of C.P titanium to 96% alumina ceramic using pure gold as the filler metal. A novel method of brazing is developed where resistance heating of C.P titanium is done inside a thermal evaporator using a Ta heating electrode. The design of electrode is optimized using Ansys resistive heating simulations. The materials chosen in this study are biocompatible and have prior history in implantable devices approved by FDA. This research is part of Boston Retinal implant project to make a biocompatible implantable device (www.bostonretina.org). Pure gold braze has been used in the construction of single terminal feedthrough in low density hermetic packages utilizing a single platinum pin brazed to an alumina or sapphire ceramic donut ( brazed to a titanium case or ferrule for many years in implantable pacemakers. Pure gold (99.99%) brazing of 96% alumina ceramic with CP titanium has been performed and evaluated in this dissertation. Brazing has been done by using electrical resistance heating. The 96% alumina ceramic disk was manufactured by high temperature cofired ceramic (HTCC) processing while the Ti ferrule and gold performs were purchased from outside. Hermetic joints having leak rate of the order of 1.6 X 10-8 atm-cc/ sec on a helium leak detector were measured. Alumina ceramics made by HTCC processing were centreless grounded utilizing 800 grit diamond wheel to provide a smooth surface for sputtering of a thin film of Nb. Since pure alumina demonstrates no adhesion or wetting to gold, an adhesion layer must be used on the alumina surface. Niobium (Nb), Tantalum (Ta) and Tungsten (W) were chosen for evaluation since all are refractory (less dissolution into molten gold), all form stable oxides (necessary for adhesion to alumina) and all are readily thin film deposited as metals. Wetting studies are also performed to determine the wetting angle of pure gold to Ti, Ta, Nb and W substrates. Nano tribological scratch testing of thin film of Nb (which demonstrated the best wetting properties towards gold) on polished 96% alumina ceramic is performed to determine the adhesion strength of thin film to the substrate. The wetting studies also determined the thickness of the intermetallic compounds layers formed between Ti and gold, reaction microstructure and the dissolution of the metal into the molten gold.

O objetivo do estudo foi avaliar o efeito da utilização de película de metilcelulose e das atmosferas de acondicionamento com ar atmosférico, vácuo e argônio sobre a conservação de batatas minimamente processadas (MP) e também sobre sua qualidade após fritura. Tubérculos foram selecionados, lavados, sanificados, cortados na forma de palitos e tratados com ácido cítrico. As batatas foram imersas em solução filmogênica contendo metilcelulose (1%) e sorbitol (0,75%) como plastificante, com posterior secagem, acondicionadas sob ar atmosférico, e modificada com argônio (20seg. e 230mmHg), além de vácuo (15seg. e 54mmHg). O produto MP armazenado a 8°C durante 12 dias foi avaliado em intervalos de 3 dias mediante análises microbiológicas, fisiológicas, físicoquímicas e físicas. A cada 3 dias as batatas MP foram também fritas e avaliadas quanto à perda de umidade, absorção de óleo, textura instrumental e avaliação sensorial. O acondicionamento sob ar atmosférico foi efetivo em reduzir a perda de massa das batatas MP. As embalagens sob vácuo foram mais efetivas para o produto MP sem película, pois mantiveram o pH, acidez titulável, teor de amido e de açúcares mais próximos do dia do início do experimento, como também mantiveram baixo o índice de escurecimento. O acondicionamento sob vácuo, entretanto, não seria indicado quando a finalidade fosse a fritura, pois foi o tratamento que apresentou maiores perdas de umidade e maior absorção de óleo. O acondicionamento sob atmosfera de argônio também foi mais efetivo nas batatas MP sem película, sendo fator determinante em reduzir os teores de CO2 no interior da embalagem, apresentou menor taxa respiratória, menor índice de escurecimento tanto antes como após a fritura, reduziu a perda de umidade durante a fritura, manteve mais a firmeza do produto frito e também minimizou a absorção de óleo a partir do 3° dia de armazename nto. A utilização de película foi efetiva em reduzir a respiração do produto MP até o 6° dia. Já no produto frito, foi fator determinante na retenção de umidade das batatas, como também na redução, ao longo do armazenamento, da absorção de óleo / The aim of this study was to evaluate the effect of methylcellulose as edible coating and packaging atmospheres with atmospheric air, vacuum and argon on the conservation of minimally processed (MP) potatoes as well as on their quality after frying. Tubers were selected, washed, sanitized, cut in the shape of sticks and treated with citric acid. Potatoes were immersed in a filmogenic solution of methylcellulose (1%) with sorbitol (0,75%) as a plasticizer, dehydrated, and then packaged under atmospheric air, and modified with argon (20seg. e 230mmHg), and vacuum (15seg. e 54mmHg). Stored MP product at 8°C for 12 days was assessed at intervals of 3 days by microbiological, physiological, physicochemical and physical analyses. Every 3 days the MP potatoes were fried and evaluated for moisture loss, oil absorption, instrumental texture and sensory evaluation. Packaging under atmospheric air was effective in reducing the mass loss of MP potatoes. The vacuum packaging was more effective for the MP product without edible coating, because they kept the pH, acidity, starch and sugar level more similar to the first day experiment, as well as low browning rate. The vacuum packaging, however, would not be appropriate when the purpose is frying, because this treatment showed the greatest loss of moisture and increased oil absorption. Packaging under argon atmosphere was also more effective for the MP product without edible coating, and it was an important factor to reduce CO2 levels inside the package, showed lower respiratory rate, lower browning index both before and after frying, reduced moisture loss during frying, kept fried product firmness better and also minimized oil absorption from the 3rd day of storage. The use of edible coating was effective in reducing the respiration of MP product until the 6rd day. For the fried product, the use of coating was a determining factor for moisture retention during frying of potatoes, and also to decrease oil absorption along the potato storage.

Glass fiber core Vacuum Insulation Panels (VIPs) have thermal performance per unit thickness of about 5-10 times higher than the traditionally used building insulation materials such as mineral wool, XPS, EPS, foam, etc. This advantage of VIP has made it very attractive new option for innovative building designs. Especially in Canada, where some of the areas have long and very cold winters. Confidence in the service life of a building material is necessary before putting a product to market. Extensive research has been conducted on the product development, quality improvement, and field application of VIPs around the world. However, there is lack of consistent and simple prediction method for the long-term thermal performance of VIPs. This paper discussed the process and performance of a field project using glass fiber VIPs to retrofit a commercial building in Yukon, Canada. The thermal performance of the VIPs used in this project was continuously monitored and critically analyzed since the start in 2011. The results have shown satisfactory thermal performance of VIPs for the past 8 years. The findings were also used to validate glass fiber core VIP accelerated aging tests conducted by the National Research Council Canada (Ottawa), and the aging rate of VIPs in a cold and dry climate was determined. The second part of this study investigated the monitored performance results from two sets of simplified accelerated laboratory aging tests, the results were analyzed with the aim to separate the impact of air diffusion from water vapour on the long-term thermal performance of glass fiber VIPs. In addition, this study also investigated the potential application of VIPs in balcony constructions to reduce heat transfer through thermal bridges. Computer modeling exercises, using a benchmarked (EN ISO 10211) three-dimensional transient and steady-state heat transfer simulation tool HEAT3, were carried out on the most optimal (thermal performance) balcony assemblies of wood framed buildings using VIP as insulation. This niche application of VIPs can significantly increase the energy efficiency of building envelopes/skins in extreme climates of Canada and elsewhere in the world. / Graduate / 2021-11-06

Que ce soit dans l‟étude du claquage sous vide ou dans les sources d‟électrons par effet de champ, l‟émission électronique est un phénomène physique essentiel qui a lieu et devient dominante à la cathode sous haute tension. Dans le cas du claquage sous vide, la première étape de ce mécanisme est l‟émission d‟électrons au sommet de rugosités présentes sur la surface. Celles-ci peuvent être représentées sous la forme de pointes. Dans le cas des sources d‟électrons, l‟émission des électrons peut se faire au niveau d‟émetteurs qui eux aussi peuvent être décrits sous la forme de « pointes » distribués de manière ordonnée sur la surface. Un modèle numérique décrivant l‟émission thermo-ionique assistée par effet de champ a été développé dans le cas d‟une pointe axisymétrique et dont le traitement peut être réduit en 2D.Il s‟agit là d‟un problème multi-physique couplé nécessitant la résolution de problèmes de différentes natures : quantiques, électrostatique, électrocinétique et thermique. A partir de ce modèle, l‟étude de l‟émission et du claquage au sommet d‟une pointe soumise à une pulse électrique de l‟ordre de la nanoseconde a été étudiée. L‟étude de l‟émission électronique sur une cathode soumise à la haute tension et illuminé par un laser picoseconde a ensuite été faite en développant un modèle qui décrit notamment le chauffage du métal en régime hors équilibre. Enfin, dans le cas du claquage sous vide, la modélisation de l‟interaction entre des microparticules, présente dans l‟espace inter-électrodes,et de l‟émission électronique provenant du sommet d‟une rugosité a été realisée. Différents régimes de trajectoires de la microparticules ont été observée suivant le courant appliqué au sommet de la rugosité. / Electron emission in vacuum from a cathode at high voltage is an important physical phenomenon for the study of vacuum breakdown or electron sources. In the vacuum breakdown, the first step of this mechanism is electron emission at the top of the microprotrusions on the surface. Microprotrusions or emitters in electron sources have the shape of a tip. A numerical model describing the thermo-field emission has been developed for a 2D axisymmetric tip. The problem is multi-physical and it is necessary to solve problems of different natures: quantum mechanics, electrostatic, electric current and thermal heating. With this model, it is possibleto study electron emission and vacuumbreakdown when nanosecond high voltage pulses are applied. Furthermore, the study of electron emission when a picosecond pulsed laser illuminates a high voltage cathode has been performed. A new model has been developped to describe the photo-electric effect and a two-temperature model has been implemented to describe the heating of the cathode in a non-equilibrium regime. Finally, the modeling of the interaction between microparticles and electron emission from microprotusions has been realised, in order to study the breakdown voltage. Different trajectories of microparticles have been identified based on the results, depending on the electron emission current.

Les pérovskites hybrides célèbrent cette année leurs 10e anniversaire dans le domaine du photovoltaïque. En plus de la progression inégalée des rendements des cellules solaires, les pérovskites ont des propriétés optoélectroniques ajustables et peuvent être fabriquées par des procédés bas coûts, ce qui en fait de sérieuses candidates pour les cellules solaires multijunctions. Le réseau cristallin caractéristique des pérovskites hybrides offre une certaine liberté, supportant l’introduction partielle de cations et d’ions halogénures multiples. L’ajustement de la composition d’un matériau pérovskite se traduit par un ajustement de ces propriétés électroniques dont notamment sa structure de bandes. En adaptant la composition il est possible d’obtenir un matériau pérovskite avec une bande interdite de 1,7 eV qui serait parfaitement adapté pour une cellule tandem à base de Silicium cristallin. Les films minces de pérovskites peuvent être fabriqués par une grande diversité de techniques de dépôt, à partir de précurseurs ‘bon marché’ (CH3NH3I et PbI2 par exemple), par des procédés à basse température. Même si la grande majorité des films de pérovskites sont obtenus par la méthode d’enduction centrifuge, celle-ci ne permet pas l’obtention de films homogènes, sur grandes surfaces et de façon répétable. Etant donné l’enjeu industriel qui attend les pérovskites et l’intérêt croissant pour les structures tandems Silicium/Pérovskite, les méthodes sans solvant semblent plus adaptées. Déjà très largement utilisé dans l’industrie des OLEDs, le procédé de coévaporation thermique semble constituer une solution commercialement viable. Publiée pour la première fois en 2013, la synthèse par coévaporation des pérovskites est pour le moment encore étudiée par peu de groupes, car nécessitant des équipements plus coûteux. La présente thèse vise à mettre en place et développer la technique de coévaporation pour la fabrication de films de pérovskites hybrides pour des applications en cellules solaires.Afin d’évaluer la faisabilité du procédé, nous avons commencé notre travail sur un réacteur de démonstration, ce qui nous a permis d’appréhender la réponse à la sublimation des deux précurseurs. Nous avons très vite identifié le comportement du sel organique CH3NH3I comme étant problématique car difficilement contrôlable (s’évaporant sous forme de « nuage »), comme nous l’avions lu dans la littérature. En six mois d’utilisation de ce réacteur, nous avons fabriqué des films de pérovskites ayant permis d’atteindre des rendements de 9% sur des cellules solaires, malheureusement avec une faible reproductibilité (que nous expliquons en partie par le caractère aléatoire de l’évaporation du composé organique CH3NH3I). Nous nous sommes trouvés dans l’incapacité de comprendre plus en profondeur le procédé à cause d’un manque de fonctionnalités de l’équipement. Grâce à ces différents retours d’expérience nous avons pu concevoir, en étroite collaboration avec l’équipementier, un réacteur semi-industriel dédié à la fabrication de films de perovskites par coévaporation. Suite à sa mise en place, nous nous somme focalisé sur la problématique de la reproductibilité dans nos expériences en essayant de diminuer l’impact du nuage organique. Bien que les efficacités atteintes en cellules solaires pour des films coévaporés fussent moindres que pour des films déposés par la technique classique d’enduction centrifuge, nous soupçonnions néanmoins une meilleure homogénéité des films obtenus par voie sèche. Nous avons ainsi intégré à cette thèse une étude comparative voie liquide/voie sèche par le biais d’une technique de spectromicroscopie rayons X en Synchrotron. / Hybrid perovskites celebrate this year their 10-year anniversary in the photovoltaic field. Besides the unprecedented rise in solar cells efficiencies, perovskite materials have tunable optical properties and can be manufactured at low cost, making them very promising candidates for the high efficiency, multijunction solar cells strategy. Perovskite crystal structure offers a relative degree of freedom, allowing the partial integration of multiple cations and halide ions. This chemical composition tuning translates into a bandgap tuning. Through fine chemical engineering, the 1.7 eV requirement for a c-Si-based tandem device can be achieved. Perovskite thin films can be prepared by a large variety of deposition techniques, from low cost precursors (CH3NH3I and PbI2 for instance), through low-temperature processes. While most of the reported works on perovskite thin films are based on the basic wet-process spincoating technique, this latter hardly allows large scale, homogeneous and reproducible deposition. With the future challenge of industrialization and the increasing interest for the Silicon/Perovskite tandem approach, solvent-free methods appear more suitable. Already widely implemented in the OLED industry, coevaporation stands as a viable option for perovskites’ future. Reported for the first time in 2013, coevaporated perovskites are still scarcely studied compared to wet-based techniques, requiring more expensive set ups. In the present thesis, we implemented and developed the coevaporation process to fabricate perovskite thin films for solar cells applications.Starting off on a proof-of-concept reactor to assess the feasibility of the technique, we got accustomed to the perovskite precursors behaviour and identify very early on the organic precursor to be hardly manageable, as reported in the literature. In six months, we were nonetheless able to obtain nice perovskite films leading to 9% efficient photovoltaic devices, unfortunately with a poor reproducibility that we think to be partially due to the cloud vapour behaviour of CH3NH3I. We eventually found ourselves missing some features on the equipment, preventing us from accurately get a grasp on the process. From this feedback we then designed, hand in hand with the manufacturer, a dedicated semi-industrial equipment for perovskite coevaporation. Following its implementation, we then focused on establishing the reproducibility of the method, trying to mitigate the parasitic effect of the organic compound. Even though the efficiencies in solar cells were still slightly lower for coevaporated perovskites, with respect to classical spincoated ones, we expected the material homogeneity to be in favour of the vacuum-based process. We then eventually integrated to this thesis a comparative study between wet- and dry-processed perovskite films using a Synchrotron-based X-ray spectromicroscopy technique.

The space environment presents various challenges when designing systems and selecting materials for applications beyond Earth’s atmosphere. For mission success, these challenges must be considered. One of the detrimental aspects of the space en- vironment is Atomic Oxygen, AO. Only present in harmful quantities in Lower Earth Orbit, LEO, AO causes significant damage to materials by breaking molecular bonds. California Polytechnic State University’s, Cal Poly’s, space environments laboratory features an apparatus capable of simulating this environment. Very thin or short samples were tested to observe the mass loss due to erosion of the sample material. Recent modifications to the system allow it to expose surfaces of three dimensional objects to AO rather than only those two dimensional objects. Simulating this effect on taller samples makes available the opportunity to test coupons that are then used in additional testing to measure the effect of that erosion on other properties. Challenges in adapting the AO system are explored and addressed, as well as some possible use cases for future work. As a use case, bending moment specimens were exposed to AO prior to testing in four point bending. Multiple regression models were constructed to determine variables contributing to slope changes between specimen pairs’ linear-elastic regions of force-displacement graphs. Results show that AO exposed specimens had significantly gentler slopes in the linear elastic region of the force-displacement curve, meaning that AO exposure reduced structural rigidity of the coupons.

The thesis deals with the study of the behavior of advanced insulating materials on the basis of secondary raw materials and the possibilities of their use in the production of vacuum insulation using in the construction and industry. The work will be devoted to possible raw material resources, problems of long-term behavior of insulators on the basis of selected secondary raw materials under reduced pressures as well as economic evaluation of the competitiveness of alternative insulators on the building market in the field of vacuum insulation.

This diploma thesis deals with the design of an autonomous universal machine for removing a loose dirt on headlamp assembly lines according to customer requirements and standards for safety and ergonomics. The thesis also includes a draft flowchart for machine control logic, a pneumatic mechanism diagram and a drawing documentation of the assembly and selected subassemblies.

The project elaborated design of optimization venting of molds exhibiting bubbles or low quality weld lines. Based on a literature study of the injection mold venting, the use of vacuum venting, namely the VACUUMJET system of the Spanish CUMSA manufacturer, has been proposed. The experiments proved the elimination of bubbles in the part and the marked improvement of visual quality of the weld lines. The effect on the closing force was not confirmed. The use of the system is more economical for larger batches production, or when high quality parts are required that allow price increasing.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第22776号 / 工博第4775号 / 新制||工||1747(附属図書館) / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 杉村 博之, 教授 邑瀬 邦明, 教授 宇田 哲也 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM