L'implantation d'hydrogène à forte dose est utilisée dans le procédé Smart Cut(tm) afin de transférer des couches de silicium assez épaisses (>200 nm) sur un autre substrat. En utilisant l'implantation à très basse énergie, la co-implantation d'H et d'He pour des doses totales bien plus faibles que celles requises lorsque l'hydrogène est implanté seul ouvre la voie à un transfert de couches beaucoup plus minces (< 50 nm). Cependant, les phénomènes mis en jeu ainsi que les mécanismes responsables de l'interaction, près de la surface libre du wafer, entre l'H et l'He, et les interstitiels et les lacunes qu'ils génèrent, restent à ce jour largement incompris. Dans ce travail, nous avons tout d'abord déterminé l'effet de la réduction des énergies d'implantation d'H et d'He sur la formation et le développement, lors d'un recuit, des cloques qui se forment à partir de micro-fissures en l'absence d'un raidisseur collé à la plaque implantée. Une approche basée sur la comparaison entre les caractéristiques dimensionnelles des cloques obtenues expérimentalement et la simulation par éléments finis, nous a permis de déterminer la pression et la quantité d'He et d'H2 hébergées dans ces cloques. En comparant ces résultats avec les doses d'ions implantées, nous avons pu mettre en évidence l'absence d'exo-diffusion d'He et d'H lors d'un recuit quelle que soit la distance entre la surface et les profils d'ions implantés, qui montre une forte efficacité des cloques à préserver les molécules. Nous avons pu identifier, puis expliquer, la différence en efficacité de coalescence des cloques en fonction de leurs positions en profondeur en la reliant à la variation de l'augmentation d'énergie élastique des cloques par rapport à leur surface. Nous avons ensuite étudié le rôle du dommage ionique, c'est-à-dire des défauts résultants de la co-implantation d'He et d'H, sur la formation et l'évolution thermique de la microstructure du silicium implanté. Cette étude a été menée soit en fonction de l'ordre d'implantation, soit en fonction de la position nominale en profondeur du profil d'He par rapport au profil d'H, soit en fonction du ratio entre les doses d'implantation d'He et d'H. Nous avons montré que la distribution en profondeur de l'H n'est jamais affectée par la co-implantation d'He. L'He est toujours piégé dans la zone où le dommage est maximal. Lorsque le dommage est maximal dans la zone du profil d'H, l'He y diffuse et y est piégé dans des nano-bulles et/ou des microfissures. Mais si le dommage généré dans la zone où est distribué l'He est supérieur à celui généré autour du profil d'H, l'He reste piégé en dehors du profil d'H dans des nano-bulles. L'He contenue dans des nano-bulles, quelle que soit leur distribution en profondeur, ne contribue pas à la pressurisation des cloques ce qui ralenti la coalescence des cloques. Finalement, nous avons pu proposer différents scénarii permettant de rendre compte des similarités et des différences mises en évidence tant avant recuit qu'après recuit, à basse ou plus haute température selon le type d'implantation réalisé. / The high dose hydrogen ion implantation is used in the Smart Cut (tm) process to transfer relatively thick (i.e. >200 nm) Si layers from a donor substrate onto a host material. Hydrogen and helium co-implantation at low energies for a much lower total fluence opens the way for transferring extremely thinner (i.e. <50 nm) layers. However, the phenomena and the mechanisms responsible for the interaction, close to a wafer surface, between H, He, silicon interstitials and vacancies they generate remain poorly understood. First, we studied the effect of reducing the ion energies during both H and He implantations onto the formation and the development of blisters during annealing. Blisters were formed from the micro-cracks since a stiffener was not bonded to the implanted wafer. An approach, based on the comparison between experimentally obtained size characteristics of blisters with the finite element method simulations, allowed us to deduce the pressure inside blister cavities and the fraction of the implanted fluences used to pressurize them. We showed that even when implanted at very low energy, H and He atoms do not exo-diffuse out of the implanted region during annealing. We were able to identify, and then relate the efficiency of blister coalescence to a variation in the elastic energy of blisters as a function of their depth position. In a second part, we studied the role of the damage, produced by He and H coimplantation, on the formation and the thermal evolution of the microstructure of the implanted silicon. These investigations were realized as a function of either the order of co-implantation, or the nominal position of the He profile with respect to the H one, or the ratio between He and H fluences. We showed that the H depth distribution was never affected by He co-implantation. Helium was always trapped at the depth where the damage was maximum. When the damage was highest within the H profile, He diffused and was trapped there in the nano-bubbles and /or the blister cavities. However, when the damage was higher within the He profile than within the H one, He remained trapped in the nano-bubbles outside the H profile. Helium contained in the nano-bubbles, whatever their depth distribution, did not contribute to a pressurization of blister cavities that slowed down their coalescence. Finally, we have proposed various scenarios accounting for the similarities and the differences evidenced both before and after annealing at low or higher temperatures depending on the type of realized implantation.

Neu entstehende Prozessketten und Technologien mit hoher Komplexität gepaart mit geometrisch immer komplexeren Bauteilen und massiv steigenden Stückzahlenanforderungen führen zu neuen Forschungsfragen hinsichtlich Effizienzsteigerung und Technologieweiterentwicklung. Für die faktenbasierte Identifizierung, Validierung und Nutzung von Wirkketten in komplexen Prozessketten wird in dieser Dissertation ein neuer Ansatz vorgestellt, der in der Prozesskette Aluminium-Strukturbauteile am Fehlerbild Blister validiert wird. Voraussetzung für die Identifizierung von Wirkketten innerhalb komplexer Prozessketten sind definierte Fehlerbilder und eine objektive Erfassung. Im Rahmen dieser Arbeit wurden mit der Entwicklung einer Richtlinie für Blister sowie einer automatisierten Anlage zur Detektion von Blistern genau diese Grundvoraussetzungen für die Identifizierung und Validierung von Wirkketten sprich komplexen Prozesszusammenhängen geschaffen. Die daraus gewonnenen Erkenntnisse lassen sich direkt auf die laufende Serienproduktion, Serienplanung und Forschung anwenden. Dies führt zu einer Effizienz- und Stabilitätssteigerung laufender und zukünftiger Prozessketten, darüber hinaus lassen sich die Potenziale einer Technologie hinsichtlich Gewichtseinsparung, Funktionsintegration oder Einsatzmöglichkeiten noch weiter ausreizen. Für zukünftige Herausforderungen in immer komplexer werdenden Prozessketten kann diese Vorgehensweise als Leitfaden für die Identifizierung und Validierung von Wirkketten sowie die anschließende Nutzung der gewonnenen Erkenntnisse in den Bereichen Serienproduktion, Serienplanung und Forschung verwendet werden.

No description available.

[pt] As embalagens de medicamentos acondicionam e protegem os fármacos, sendo que alterações nos materiais de embalagem têm impacto crítico no desempenho do produto. Os blisters, que consistem de um tipo de embalagem primária de filmes poliméricos, entram em contato direto com o medicamento. A caracterização dos materiais de embalagens primárias é o principal meio de garantir a adequação dos mesmos ao uso pretendido. Reconhecendo essa necessidade, a nova farmacopeia dos Estados Unidos, que entrará em vigor em 2020, amplia suas considerações para caracterização de embalagens. Contudo, o novo documento ainda apresenta limitações de abrangência das recomendações técnicas e não considera filmes multicamadas, os quais são amplamente utilizados na indústria. No presente trabalho, cinco tipos de filmes para embalagem foram caracterizados por meio da Calorimetria Exploratória Diferencial e Espectroscopia no Infravermelho, ambas mencionadas nas farmacopeias; e também, para determinar os limites térmicos dos materiais avaliados, pela Análise Termogravimétrica. Com a inexistência de referências para filmes em multicamadas, os resultados foram comparados com divergentes valores publicados na literatura. Identificou-se, nos cinco materiais analisados, a existência de um plastificante não informado pelos fabricantes. O estudo realizado confirma a importância da caracterização dos blisters, apontando para a necessidade tanto da ampliação das recomendações da farmacopeia para inclusão de novos materiais e filmes multicamadas, quanto da produção de materiais de referência para os polímeros empregados nas embalagens. / [en] Pharmaceutical packaging wraps and protects drugs, and changes in packaging materials have a critical impact on product performance. Blisters, which consist of one type of primary packaging of polymer films, come into direct contact with the drug. The characterization of the primary packaging materials is an essential strategy for ensuring that they are suitable for the intended use. Recognizing this need, the new United States Pharmacopeia, which will come into effect in 2020, expands its considerations for characterization of packaging. However, the new document still contains limitations on the scope of the technical recommendations and does not consider multilayer films, which are widely used in industries. In the present work, five types of packaging films were characterized by Differential Scanning Calorimetry and Infrared Spectroscopy, both mentioned in the pharmacopeias; and also, to determine the thermal limits of the evaluated materials, by the Thermogravimetric Analysis. With the lack of references for multilayer films, the results were compared with divergent values published in the literature. It was identified, in the five materials analyzed, the existence of a plasticizer not identified by the manufacturers. This study confirms the importance of the characterization of the blisters, pointing to the need to not only expand the recommendations of the pharmacopeia, but also to include new materials and multilayer films, and the production of reference material for the polymers used in packages.

Environmental stresses arising from temperature and moisture changes, and/or other aggressive fluid ingressions can degrade the mechanical properties of the adhesive, as well as the integrity of an adhesive interface with a substrate. Therefore such disruptions can significantly reduce the lifetime and durability of an adhesive joint.1-4 In this research, the durability of certain epoxy adhesive joints and coatings were characterized using a fracture mechanics approach and also by constant frequency impedance spectroscopy. The shaft-loaded blister test (SLBT) was utilized to measure the strain energy release rate (G) or adhesive fracture energy of a pressure sensitive adhesive tape. In this study, support for the value of the SLBT fracture mechanics approach was obtained. The SLBT was then used to investigate the effects of relative humidity on a model epoxy bonded to silicon oxide. Lastly, the effects of water and temperature on the adhesion of a commercial filled epoxy bonded to silicon oxide was characterized and interpreted. A novel impedance sensor for investigating adhesion was developed in a collaborative effort between Virginia Tech and Hewlett-Packard. Utilizing the technique of constant frequency impedance spectroscopy, the distribution and transport of fluids at the interface of adhesive joints was measured. A broad spectrum of adhesives was tested. In addition, the effects of hygroscopic cycling on the durability of adhesive coatings were measured for the commercial filled epoxy using the device. Lastly, recommended modifications of the experimental set-up with the new sensor are proposed to improve the technique. / Ph. D.

Cette étude porte sur la détermination d’un critère de rupture des gaines de combustible de Zircaloy-4 détendu hydruré contenant un blister d’hydrures, en conditions accidentelles représentatives d’un accident d’injection de réactivité. Deux plages de comportement différentes en fonction de la température ont clairement été mises en évidence grâce à l’étude bibliographique, aux différentes campagnes d’essais mécaniques et aux analyses des faciès de rupture des éprouvettes rompues : une rupture de type fragile pour la gaine à 25°C et une rupture ductile à 350°C.A 25°C, la rupture fragile a été traitée par une analyse globale en mécanique élasto-plastique de la rupture. A partir des essais mécaniques effectués à 25°C sur les gaines contenant des blisters, des simulations numériques par éléments finis ont été réalisées avec le code CAST3M. Des calculs d’intégrales-J en pointe de fissure ont alors permis d’identifier un critère de rupture en ténacité moyenne de 13,8 +/- 3,1 MPa.m1/2.A 350°C, une campagne d’essais biaxés de type pression interne couplée à la traction axiale a été réalisée sur des tronçons de Zircaloy-4 contenant des blisters, à des biaxialités des contraintes représentatives du RIA. Il a été montré que la rupture de la gaine, avec et sans blister, avait lieu de façon ductile, que la déformation diamétrale à rupture de la gaine diminuait lorsque la profondeur de blister augmentait, et que la biaxialité des contraintes n’avait pas d’effet sur la rupture des gaines contenant un blister suffisamment profond.Un modèle d’endommagement ductile couplé à la plasticité, basé sur un formalisme de type GTN, a été utilisé. Afin d’améliorer la description de l’endommagement des gaines de Zircaloy-4, une nouvelle source de germination de porosités liée au paramètre de Lode a été intégrée dans le modèle. L’évaluation de la triaxialité des contraintes et du paramètre de Lode dans les simulations numériques de la rupture ductile des gaines à 350°C a notamment permis de comprendre certaines tendances expérimentales. / This study deals with the determination of a fracture criterion for hydrided, cold worked and stress relieved Zircaloy-4 fuel cladding tubes with hydride blister, during a reactivity initiated accident. Two types of fracture profiles were identified, depending on the temperature, thanks to a bibliographical study, mechanical tests and fracture profiles analysis : brittle fracture at 25°C, and ductile fracture at 350°C.At 25°C, brittle fracture was studied by a global analysis in elasto-plastic fracture mechanic. Numerical simulations were performed by a finite element method with the CAST3M code, based on mechanical tests on fuel cladding tubes with blisters. Crack tip J-integral calculations were carried out to identify a mean fracture toughness of 13,8 +/- 3,1 MPa.m1/2.At 350°C, internal pressure combined to axial tensile tests were performed on Zircaloy-4 fuel cladding tubes with hydride blisters, at stress biaxialities corresponding to those of a RIA. It was observed a ductile fracture for tubes with and without blister. It was shown that hoop strain at failure decreases when blister thickness increases, and that stress biaxiality has no effect on cladding tubes bearing a thick blister. A ductile fracture model based on the GTN model was employed and a nucleation of voids due to shear stress was introduced, based on the Lode parameter. Stress triaxiality and Lode parameter were assessed in numerical simulations to understand some experimental observations.

<p>Bonding techniques intended for assembling space microsystems are studied in this work. One of the largest problems in bonding pre-processed semiconductor wafers are the severe process restrictions imposed by material compatibility issues. Plasma processes have shown to be good for sensitive materials integration why the influence of different plasma parameters on the bondability of wafers is particularly studied. Conventional wet chemical and field-assisted methods are also examined. The resulting bond quality is assessed in terms of mechanical strength, homogeneity, and yield.</p><p>The effect of spaceflight environment on the reliability of wafer bonds is also investigated. Both high and low temperature annealed bonds are found to be very robust. Effects observed are that low temperature bonds are reinforced by thermal cycling in vacuum and that high temperature bonds degrade slightly by low dose γ irradiation.</p><p>Adhesion quantification is important for all bonding. Development of accurate quantification methods is considered necessary since most methods at hand are limited. This work includes the development of the blister test method. Former test structures are improved to be more practical to work with and to yield low experimental scatter. A physical stress model for the improved structure is suggested with which successful predictions of fracture for different test specimen configurations are made. The blister test method is used throughout this work to assess the strength of wafer bonds. The physics background and modelling of other common test methods are also thoroughly analysed. The methods’ practical capabilities and limitations are commented; origin and mitigation of measurement errors are discussed. It is shown that all methods can be significantly improved by small means.</p><p>Weibull statistics is introduced as a tool to characterise wafer bonds. This method is suitable to use in brittle materials design as the inherent variability in strength can be properly accounted for.</p>

Bonding techniques intended for assembling space microsystems are studied in this work. One of the largest problems in bonding pre-processed semiconductor wafers are the severe process restrictions imposed by material compatibility issues. Plasma processes have shown to be good for sensitive materials integration why the influence of different plasma parameters on the bondability of wafers is particularly studied. Conventional wet chemical and field-assisted methods are also examined. The resulting bond quality is assessed in terms of mechanical strength, homogeneity, and yield. The effect of spaceflight environment on the reliability of wafer bonds is also investigated. Both high and low temperature annealed bonds are found to be very robust. Effects observed are that low temperature bonds are reinforced by thermal cycling in vacuum and that high temperature bonds degrade slightly by low dose γ irradiation. Adhesion quantification is important for all bonding. Development of accurate quantification methods is considered necessary since most methods at hand are limited. This work includes the development of the blister test method. Former test structures are improved to be more practical to work with and to yield low experimental scatter. A physical stress model for the improved structure is suggested with which successful predictions of fracture for different test specimen configurations are made. The blister test method is used throughout this work to assess the strength of wafer bonds. The physics background and modelling of other common test methods are also thoroughly analysed. The methods’ practical capabilities and limitations are commented; origin and mitigation of measurement errors are discussed. It is shown that all methods can be significantly improved by small means. Weibull statistics is introduced as a tool to characterise wafer bonds. This method is suitable to use in brittle materials design as the inherent variability in strength can be properly accounted for.

No description available.

Three testing methods are proposed to characterize properties of fuel cell materials that affect the mechanical durability of proton exchange membranes (PEMs). The first two methods involved measuring the in-plane biaxial strength of PEMs and the biaxial hygrothermal stresses that occur in PEMs during hygrothermal cycles. The third method investigated the nonuniform thickness and compressibility of gas diffusion media which can lead to concentrated compressive stresses in the PEM in the through-plane direction. Fatigue and creep to leak tests using multi-cell pressure-loaded blister fixtures were conducted to obtain the lifetimes of PEMs before reaching a threshold value of gas leakage. These tests are believed to be more relevant than quasi-static uniaxial tensile to rupture tests because of the introduction of biaxial cyclic and sustained loading and the use of gas leakage as the failure criterion. They also have advantages over relative humidity cycling test because of the controllable mechanical loading. Nafion® NRE-211 membrane was tested at three different temperatures and the time-temperature superposition principle was used to construct a stress-lifetime master curve. Tested at 90°C, extruded Ion Power® N111-IP membrane was found to have longer lifetime than Gore™-Select® 57 and Nafion NRE-211 membranes under the same blister pressure profiles. Bimaterial specimens fabricated by bonding a piece of PEM to a substrate material were used to measure the hygral stresses, compressive and tensile, in the PEM during relative humidity cycles. The substrate material and its thickness were carefully chosen so that stresses in the PEM could be obtained directly from the curvature of the bimaterial specimen without knowing the constitutive properties of the PEM. Three commercial PEMs were tested at 80°C by cycling the relative humidity between 90% and 0% and by drying the membrane to 0%RH after submersion in liquid water. Stress histories for all three membranes show strong time-dependencies and Nafion® NRE-211 exhibited the largest tensile stress upon drying. Besides in-plane stresses, hard spots in gas diffusion media (GDM) can locally overcompress PEMs in the out-of-plane direction and cause electrical shorting. In this study, GDM samples sealed with an impermeable Kapton® film on the surface were compressed with uniform air pressure and the nonuniform displacement field was measured with a three-dimensional digital image correlation technique. Hard spots as a result of the nonuniform thickness and compressibility of the GDM were found and their severities as stress risers are evident. Locally, a nominal platen compression (similar to bipolar plate land compression) of 0.68 MPa can lead to compressive stress as large as 2.30 MPa in various hard spots that are in the order of 100s µm to 1 mm in size. / Ph. D.