Rozprawy doktorskie na temat „Cold-bonding”

Introduction 100Mo target design is key to commercially viable large scale cyclotron production of 99mTc. The target back plate supporting the 100Mo must be chemically inert to the target dissolution conditions but ideally it should also be able to dissipate the high thermal loads of irradiation, not contaminate target substrate with radionuclidic by-products, and be adequately inexpensive to allow for single use. Aluminum was selected as our target support as it satisfies these requirements. Our process entails rolling 100Mo powder into a foil of desired thickness, and then diffusion bonding [1] the foil onto an aluminum back plate. The 100Mo targets were designed to be 20×80×0.1 mm to match our TR24 cyclotron’s proton beam profile and energy. Efforts are currently underway to scale up the process to allow for simultaneous production of multiple targets at once. Material and Methods The crude enriched 100Mo foil (99.815% enrichment) was made from 100Mo powder using a horizontally mounted rolling mill and an aluminum hopper. The crude foil was rolled repeated-ly, and the space between the rollers gradually reduced until the thickness of the foil was changed from an initial thickness of 0.3 mm to a thickness of 0.1 mm. The rolled 100Mo foil was annealed under reducing atmosphere and then bonded to the aluminum target plate support under inert atmosphere in a heated press at 500 °C. Results and Conclusion By rolling 100Mo foils from powder we were able to produce uniform foils with an average density of > 98 % compared to the maximum theoretical density of 100Mo (n = 5) and thicknesses of roughly 0.1 mm. All foils produced were the desired 20 mm width (i.e. limited by the width of the opening of the hopper) and trimmed to the desired 80 mm length. The annealing process was necessary due to the brittleness of the un-annealed rolled foil and the difference in the thermal expansion coefficients of molybdenum and aluminum which caused un-annealed foils in previous experiments to crack and break off during pressing (n = 10). Surface preparation of the aluminum support plate was also found to play a critical step in the efficiency of the bond, and continuing effort to scale the above de-scribed procedure to mass produce 100Mo tar-gets is ongoing. Targets have undergone preliminary testing to 250 μA.

Cold gas dynamic spraying (CDGS) is a material deposition technique, in which powder particles are accelerated to speeds of between 300-1200 m/s and upon impact deform plastically and adhere. The overall aims of this research project were to understand the bonding behaviour in cold spraying of copper, aluminium and titanium, and to produce corrosion resistance barrier layer of titanium coatings using cold spraying. The mechanism of bonding in cold spraying is still a matter of some debate. In this thesis, copper has been cold sprayed onto aluminium alloy substrates, the surfaces of which had been prepared in a variety of ways. The coating - substrate bonding was assessed via a novel intermetallic growth method along with adhesive pull-off testing. The bond strength has been rationalised in terms of a modified composite strength model, with two operative bonding mechanisms, namely (i) metallurgical bonding and (ii) mechanical interlocking of substrate material into the coating. In most cases, mechanical interlocking is able to account for a large proportion of the total bond strength, with metallurgical bonding only contributing significantly when the substrate had been polished and annealed prior to spraying. In addition, grit-blasting has been shown to significantly reduce the bond strength compared to other substrate preparation methods. Aluminium has also been cold sprayed onto copper substrates, the mechanical interlocking of substrate material was not observed and the bond strength was relatively low. Titanium particles have been deposited onto three different steel substrates, namely low carbon steel, an Armco iron, and an austenitic stainless steel. Using the novel intermetallic growth method it was found that a barrier does exist at the interface of the titanium deposited onto the low carbon steel and Armco iron substrates which is not removed in either of the stages of impact or during the heat treatment process. On the other hand, in the case of titanium deposited onto the austenitic stainless steel, the barrier is removed. Cold spraying is believed to have the potential for the deposition of corrosion resistant barrier coatings. However, to be effective, a barrier coating must not have interconnected porosity. Titanium coatings were sprayed using nitrogen as an accelerant gas at two process gas temperatures of 600 and 800˚C to reduce porosity. A modified in-situ grit blasting was used to improve the coating-substrate adhesion. The mean bond strength of the titanium deposits was ~70 MPa and tensile strength was 250 MPa. Mercury intrusion porosimetry (MIP) was used to characterize the interconnected porosity over a size range of micrometers to nanometers. The MIP results showed that in cold sprayed deposits a significant proportion of the porosity was sub-micron and so could not be reliably measured by optical microscope based image analysis. A set of free standing deposits was also vacuum heat treated to further decrease porosity levels. The effect of porosity on the corrosion behaviour of titanium coatings onto carbon steels was investigated in 3.5 wt.% NaCl. The electrochemical measurements of the coatings showed significant substrate influence when the interconnected porosity of the coating was 11.3 vol.% but a decreased substrate influence with a porosity level of 5.9 vol.%. Salt spray (fog) tests confirmed these electrochemical findings and showed the formation of corrosion products following 24-h exposure. Laser surface melting (LSM) was used to seal the top ~140 μm of the coating to eliminate any interconnected porosity. The LSM titanium coatings showed no sign of corrosion after 100-h of salt spray tests, and the open circuit potential and passive current density values were similar to those of the bulk titanium.

The objective of the thesis is to understand the particle/substrate interaction of micron-sized High Purity (HP) aluminum (Al) powder particles with varying surface oxide/hydroxide layers, during single particle impact and determine the critical impact velocity (CIV). Advancements in analytical techniques enable in-situ supersonic impact of individual metallic micro-particles on substrates with micro-scale and nanosecond-level resolution. This novel capability allowed direct observation and measurement of a material-dependent threshold velocity, above which the particle underwent impact-induced material ejection and adhered to the substrate, (critical impact velocity). The data was then compared to empirical, as well as predicted values of the CIV from published data that were based upon theoretical iso-entropic fluid dynamics models. A major emphasis of this research was to perform, in-depth characterization of the Al powder in the as-received, gas atomized state and subsequent to controlled temperature and humidity exposure (designed to form a prescribed oxide and/or hydroxide surface layer) and finally after single particle impact. Analytical techniques including XPS, ICP, IGF, TEM and SEM were performed to determine the species of oxide and/or hydroxide, bulk chemical composition, oxygen content and thickness of the surface oxide/hydroxide layer. Finally, bulk samples of material were produced by the cold spray process, from powder representing select test groups and subsequently characterized to determine tensile and hardness properties, chemistry, microstructure and conductivity. A fundamental understanding of the role of surface oxidization in relationship to particle deformation during impact and the bonding mechanism will be applicable toward the development of optimized parameters for the cold spray (CS) process. Results from this study will aid in the development of industrial practices for producing, packaging and storing Al powders.

Adhesive bonding for structural applications has many advantages such as reducing the weight of vehicles and providing efficient stress transfer across joined materials. The largest asset of adhesive bonding is that they can join dissimilar materials. To achieve the highest joint strength possible when using metals, however, the metal surfaces have to be pre-treated. This can be done in a variety of ways, such as grit blasting or chemical etching. Chemically etching the surface produces the highest strength joints, but has many drawbacks. The first of which is that each metal used requires a different treatment chemistry. This reduces the materials available for selection as a result of increased pre-treatment complexity. The current work focusses on stainless steel and titanium alloy. The lap shear bond strength for both metals increased significantly after a cold atmospheric plasma (CAP) treatment and was in line with the chemical etching processes. The durability of both metals demonstrated that the plasma treatment increases the performance. For stainless steel the durability is similar to the chemical etch process. For titanium the durability performance is increased, but does not reach the level of the chemical treatment process. A combination of surface science techniques has revealed that there are three mechanisms which lead to an increased bond strength. These are: a reduction in hydrocarbon contamination, shown using X-ray photoelectron spectroscopy (XPS) and time of flight\,-\,secondary ion mass spectrometry (ToF-SIMS). The growth of the surface oxide layer, analysed using an XPS sputter depth profile, and functionalisation of the oxide layer, which has been probed using ToF-SIMS, both lead to an increase in lap shear bond strength. The feasibility of the process rests on two factors. The first is achieving equivalent mechanical properties, the second factor is the energy, resources and time required for a given treatment. The first has been satisfied in this work, the second has been investigated using a life cycle analysis approach which found that plasma treatment had a higher impact on the environment when compared to oxalic acid etching. but this assumed that the acid is 100\% efficient, which is far from the case. When simulated in a `real world' scenario, there is nearly parity between the two treatments Based on the data presented in this work, including analysis of the process life cycle, CAP has the potential as a first multi material pre-treatment for structural adhesive bonding.

The impact phenomena of high velocity micron-size particles, although commonly considered and described as detrimental in numerous engineering applications, can be used in a beneficial way if properly understood and controlled. The Cold Gas Dynamic Spray (CGDS) process, known as a surface modification, repair and additive manufacturing process, relies on such high velocity impacts. In the process, solid particles are accelerated by a supersonic gas flow to velocities up to 1200 m/s and are simultaneously heated to temperatures lower than their melting point. When propelled under proper velocity and temperature, the particles can bond onto a target surface. This bonding is caused by the resulting interfacial deformation processes occurring at the contact interface. Hence, the process relies heavily on the gas/particle and particle/substrate interactions. Although numerous experimental and/or numerical studies have been performed to describe the phenomena occurring during particle flight and impact in the CGDS process, numerous phenomena remain poorly understood. First, the effect of substrate surface topographical condition on the particle deformation and ability to successfully adhere, i.e. atomically and/or mechanically, has not been thoroughly investigated such that its influence is not well understood. Another aspect of the process that is generating the largest gap between experimental and numerical studies in the field is the lack of particle in-flight temperature measurements. Obtaining such data has proven to be technically difficult. The challenges stem from the short particle flight time, low particle temperature and small particle size preventing the use of established thermal spray pyrometry equipment. Relatedly, lack of such measurements precludes a proper experimental study of the impact related phenomena at the particle/substrate interface. As a result, the effect of particle size dependent temperature on overall coating properties and atomic bonding relies currently on estimates. Finally, the effect of particle impact characteristics on interfacial phenomena, i.e. grain size and geometry, velocity/temperature, and oxide scale thickness, on adhesion and deformation upon single particle collision has also been scarcely studied for soft particle depositions on hard substrate. Hence, the current research work aims at studying fundamental aspects of particle/gas heat transfer and particle/substrate impact features in goals to improve the understanding of the CGDS process. Different surface preparation methods will be used to create various surface roughness and topographical features, to provide a clear understanding of the target surface state influence on coating formation and adhesion. Additionally, new equipment relying on novel technology, i.e. high-speed IR camera, will be utilized to obtain particle in-flight temperature readings with sequence recordings. Subsequently, the experimental particle in-flight temperature readings will be used to develop a computational fluid dynamics model in goals to validate currently used Nusselt number correlations and heat transfer equations. The particle size-dependent temperature effect on the particle’s elastic and plastic response to its impact with a targeted surface and its ability to successfully bond and form a coating will be studied experimentally. A thorough CFD numerical work, based on experimental findings, will be included to provide full impact characteristics (velocity, temperature, size and trajectory) of successfully deposited particles. Finally, the numerical results will be utilized in the ensuing study to correlate single particle deformation, adhesion and interfacial features to impact characteristics. A finite element model will be included to investigate the effect of particle size dependent temperature on single particle interfacial pressure, temperature and bonding ability.

Le principe du procédé cold spray réside dans la projection de poudres à haute vitesse sur un matériau, le substrat. La formation d'un revêtement plus ou moins dense à sa surface passe par l'adhérence et l'empilement des particules projetées. Un des domaines d'application d'un tel procédé est la réparation de composants métalliques ou composites utilisés dans le secteur aéronautique. Les particules et le substrat adhèrent par différents mécanismes, notamment mécaniques. Les duretés respectives des matériaux et la topographie de surface du substrat influent sur l'intensité de cet ancrage mécanique. Cette étude permet de statuer sur ces deux contributions. Pour cela, des systèmes purement métalliques et composites aux propriétés mécaniques différentes sont choisis. Le dépôt de particules sur des surfaces rugueuses est étudié à travers l'élaboration de revêtements d'aluminium pur sur substrats d'alliage d'aluminium plus durs. Des mécanismes de déformation plastique et d'empilement sont analysés par construction de revêtements d'Al-SiC sur aluminium. L'élaboration de ces revêtements passe par l'optimisation de nombreux paramètres liés au procédé et à la nature des matériaux (température, pression, granulométrie). Les conditions d'impact des particules sont également déterminées par l'emploi de techniques mesurant la vitesse des poudres projetées (DPV 2000), la température du substrat par thermocouples et la température des particules par simulation numérique. L'ancrage mécanique des particules est analysé par observation en coupe de l'interface revêtement-substrat. Le gradient de dureté est également quantifié. Une analyse de la morphologie des surfaces sablées est réalisée afin de corréler la granulométrie des particules aux dimensions de rugosité mesurées. Un modèle d'impact par simulation numérique est mis en place pour étudier les déformations plastiques des interfaces en fonction de la topographie de surface. Enfin, des essais d'adhérence par choc laser (LASAT®) sont entrepris afin d'identifier le rôle de la rugosité d'interface sur les seuils de rupture déterminés numériquement
The cold spray process is based on high-speed spraying of a powder onto a substrate. The formation of a more or less dense coating depends on sprayed particle adhesion and coating build-up. The repair of metallic or composite aircraft / aerospace components is a recent application of cold spraying. The particle-substrate bond strength is due to various mechanisms, including mechanical anchoring. Substrate material hardness and surface topography governs the degree of mechanical anchoring. This thesis study is centered on the influence of these two contributions. Pure metallic and composite systems with different mechanical properties are selected. Particle deposition onto rough surfaces is investigated through the development of pure aluminium coating of harder aluminum alloy substrates. Plastic deformation and build-up mechanisms are studied for Al-SiC coatings onto ductile substrate. All the coatings resulted from an optimization stage where process parameters and materials properties are considered (gas temperature, gas pressure, particle size). Particle impact conditions are also determined by particle speed experimental measurements (using a DPV 2000 system). Substrate temperatures are determined using thermocouple and particle temperatures are studied by numerical simulation. Mechanical anchoring of particles is investigated by cross-section observation of the coating-substrate interface. Hardness gradient is also quantified. An analysis of sand-blasted surfaces morphology is performed to correlate particle size and roughness parameters. A model of particle impact is established from a finite element analysis of interface plastic deformation as a function of surface topography. Lastly, dynamic adhesion testing using a laser shock (LASAT®) are undertaken to study the potential role of interface roughness on the fracture thresholds in the light of a numerical analysis

The objective of this study is to successfully deposit Titanium Ti-6Al-4V layers onto Ti-6Al-4V substrate using two new commercially available Cold Spray processes such as Low Pressure Cold Spray (LPCS) and Pulsed Gas Dynamic Spray (PGDS). The second objective of this work is to develop a technique to repair Titanium parts since there is currently no repair technique commercially available. It is envisioned that commercial cold spray systems could be used to repair gashes on Titanium components. The examination of both feedstock powders and coatings were performed by different techniques such as optical microscopy and Scanning Electron Microscopy (SEM). Porosity, hardness, adhesion strength, flattening ratio, wipe test, fracture surface, wear test, XRD and chemical composition of the coatings using EDS have been evaluated. Cold spray has shown to be a promising technique for the deposition of heat sensitive particles such as titanium. LPCS and PGDS both produced high quality coatings. Low porosity, high hardness, adhesion strength over 40 MPa, metallurgical bonding, similar to bulk material wear rate, no oxide and nitride phases inside coating were measured.

La projection à froid, aussi appelée cold spray, est considérée comme un nouveau membre de la famille de laprojection thermique depuis une trentaine d'années maintenant. Cette thèse propose d'étudier le comportement endéformation des particules et du substrat et de mettre en avant les liaisons formées dans le revêtement par deuxapproches complémentaires, expérimentale et de simulation.Une méthode innovante pour observer directement la surface fracturée des particules déposées après décollementdu substrat a été testée avec succès. Par ce moyen, la surface de contact entre particule et substrat sousdifférentes conditions a été analysée.Concernant les résultats expérimentaux, une nouvelle théorie a été proposée pour expliquer le mécanisme deliaison interfaciale d'un revêtement dur de Ni sur substrat mou d'Al reposant sur l'effet de martelage répété desparticules, sur l'effet de pression du gaz principal et sur l'effet de préchauffage du substrat. La transformation dumécanisme de liaison revêtement/substrat au cours de la construction du dépôt a été mise en évidence en passantdu verrouillage mécanique à une combinaison d'une liaison mécanique et d'une liaison métallurgique, puis à laformation d'instabilités sous forme d'un mélange tourbillonnaire à l'interface. Plus de zones de liaisonsmétallurgiques sont générées sous forte pression, une plus grande déformation plastique apparaît grâce latempérature de préchauffage, et une adhérence plus forte au sein des dépôts est capable de se produire en dépitde la présence d'un film d'oxyde épais sur la surface du substrat
Cold spraying, also called cold gas dynamic spraying, is a new coating technology which has been developed duringthe past three decade. In this study, a comprehensive investigation on particle deformation behavior and bondingbehavior between particle and substrate was conducted by experiment and numerical method.This thesis aims at presenting an innovative method to directly observe the fractured contact surface between thecold sprayed particle and substrate. By this means, the particle/substrate fractured contact surfaces were analyzedfor different conditions.Based on the experimental results, a new theory was proposed to explain the interfacial bonding mechanism of hardNi coating onto soft Al substrate. It is assumed that the particle peening effect is essential for the formation ofdiscontinuous metallurgical bonding. The dominant coating/substrate bonding mechanism is responsible of thetransformation during the coating build-up process of the initial mechanical interlocking to a combination ofmechanical interlocking and metallurgical bonding therefore of the formation of interfacial instabilities. The highcontact pressure is the relevant factor determining the particle/substrate metallurgical bonding. More metallurgicalbonding areas were generated due to strengthen peening effect of the subsequently deposited particles with higherpropelling gas pressure. Finally, stronger adhesion is able to occur despite the presence of a thick oxide film on thesubstrate surface by the preheating of the substrate. Higher temperatures help the materials to undergoes astronger plastic deformation that disrupts the oxide films. That leads to initiate an intimate contact between particleand substrate

L’électronisation de l’industrie a mené à l’augmentation de la pollution électromagnétique pouvant être néfaste pour les systèmes électroniques sensibles et les êtres vivants. L’un des moyens pour limiter la propagation des champs électromagnétiques est l’utilisation d’un blindage. L’étude s’est ainsi focalisée sur l’élaboration à froid d’un composite bimétallique pour le blindage magnétique. Le composite étudié allie les propriétés physiques de l’aluminium et de l’acier via le trilame Al8011/AcierDC01/Al8011. Le trilame est élaboré par colaminage à température ambiante. Il s’est avéré que la qualité de l’adhérence des interfaces Al/Acier et l’architecture du trilame dépendent fortement des paramètres du colaminage. Une préparation minutieuse des tôles et de leurs surfaces concomitantes se révèle être tout aussi importante que le colaminage en lui-même. De plus, au cours du colaminage, la tôle d’acier s’est montrée sensible à des instabilités plastiques qui amènent par la suite à sa striction et à sa fragmentation. Ces instabilités plastiques favorisent l’adhérence grâce à des soudages Al/Al mais n’en sont pas un prérequis. Au niveau de l’efficacité de blindage, le trilame s’est révélé être particulièrement intéressant puisque, grâce à sa composition et à sa structuration, il est capable d’atténuer aussi bien les champs magnétiques basses fréquences (< 1 kHz) que les champs magnétiques de plus hautes fréquences (> 1 kHz). Dans une étude à iso-masse, le trilame a présenté une meilleure efficacité de blindage que les tôles d’Al, de Cu et d’acier. Cependant, la fragmentation de l’acier dans le trilame s’est révélée être néfaste pour le blindage magnétique, nécessitant de faire alors un compromis entre tenue mécanique et efficacité de blindage
The growth of electronic devices has led to an increase in electromagnetic pollution that can be harmful to sensitive electronic systems and living beings. One of the means of limiting the propagation of electromagnetic fields is the use of shielding. Then, the study focused on the elaboration of a bimetallic composite for magnetic shielding. The studied composite combines the physical properties of aluminum and steel via the Al8011/SteelDC01/Al8011 trilayer. The trilayer is produced by cold roll bonding (CRB). It has been found that the adherence quality of the Al/Steel interfaces and the architecture of the composite heavily depend on the CRB parameters. Careful preparation of the sheet and their concomitant surfaces is just as important as CRB itself. Furthermore, during CRB, the steel sheet was sensitive to plastic instabilities which subsequently led to its necking and fragmentation. These plastic instabilities promote adherence through Al/Al welds but are not a prerequisite. In terms of shielding effectiveness, the bimetallic composite has proved to be particularly interesting. Thanks to its composition and its structuring, it can attenuate both low (< 1 kHz) and high frequency (> 1 kHz) magnetic fields. In an iso-mass study, the composite showed a higher shielding effectiveness than Al, Cu and steel sheets. However, the steel fragmentation in the composite proved to be detrimental to magnetic shielding, then requiring a compromise between mechanical strength and shielding effectiveness

This thesis presents methods for fabricating MicroElectroMechanical System (MEMS) actuators and high-flow gas microvalves using wafer-level integration of Shape Memory Alloys (SMAs) in the form of wires and sheets. The work output per volume of SMA actuators exceeds that of other microactuation mechanisms, such as electrostatic, magnetic and piezoelectric actuation, by more than an order of magnitude, making SMA actuators highly promising for applications requiring high forces and large displacements. The use of SMAs in MEMS has so far been limited, partially due to a lack of cost efficient and reliable wafer-level integration approaches. This thesis presents new methods for wafer-level integration of nickel-titanium SMA sheets and wires. For SMA sheets, a technique for the integration of patterned SMA sheets to silicon wafers using gold-silicon eutectic bonding is demonstrated. A method for selective release of gold-silicon eutectically bonded microstructures by localized electrochemical etching, is also presented. For SMA wires, alignment and placement of NiTi wires is demonstrated forboth a manual approach, using specially built wire frame tools, and a semiautomatic approach, using a commercially available wire bonder. Methods for fixing wires to wafers using either polymers, nickel electroplating or mechanical silicon clamps are also shown. Nickel electroplating offers the most promising permanent fixing technique, since both a strong mechanical and good electrical connection to the wire is achieved during the same process step. Resistively heated microactuators are also fabricated by integrating prestrained SMA wires onto silicon cantilevers. These microactuators exhibit displacements that are among the highest yet reported. The actuators also feature a relatively low power consumption and high reliability during longterm cycling. New designs for gas microvalves are presented and valves using both SMA sheets and SMA wires for actuation are fabricated. The SMA-sheet microvalve exhibits a pneumatic performance per footprint area, three times higher than that of previous microvalves. The SMA-wire-actuated microvalve also allows control of high gas flows and in addition, offers benefits of lowvoltage actuation and low overall power consumption.
QC 20120514

Исследовано влияние состояния поверхностей оптических сборок склеенных из стекол ЛК7 и ТФ7 на технические характеристики сборок, склеенных клеем «Бальзамин М», при воздействии различных климатических условий, их деформации, а также на прочность клеевого соединения при равномерном отрыве сборок, изготовленных из стекла К8, склеенных клеем «Бальзамин М».
The influence of the state of the surfaces of optical assemblies glued from LK7 and TF7 glasses on the technical characteristics of assemblies glued with "Balzamin M" glue, under the influence of various climatic conditions, their deformation, as well as on the strength of the adhesive bond with uniform tearing of assemblies made of K8 glass glued with "Balzamin M" glue.

Diploma thesis gives an overview of artificial lightweight aggregates based on fly ash. Fly ash such as the residues of coal burning is currently one of the most used secondary raw materials for new building materials for research papers. The results shows that the secondary energy products are not just fully substitute the primary component, but in many cases improves the final properties of building products. Wide complex of fly ashes not only from domestic sources was tested and it`s main properties important for it`s further application was determined. Laboratory production of artificial aggregates based on fly ash made by sintering and also by cold bonding and following manufacture of artificial fly ash aggregates in technological conditions are also solved. The thesis is simultaneously concentrate on review of the suitability of fly ash aggregates in lightweight concrete.It was found that the highest quality fly ash for the production of sintered fly ash aggregate is fly ash and FBC ash is the best for the production of cold bonded aggregates. It was also verified that both types of aggregates are applicable to lightweight concrete class LC 20/22. The vast majority of manufactured aggregates is suitable for the production of lightweight concrete class LC 30/33. It was demonstrated that the sintered fly ash aggregates can be also used for high strength lightweight concrete class LC 50/55. Tests have also verified that all tested fly ashes and products produced from them meet the requirements of legislation on environment.

Thesis (M.S.)--West Virginia University, 2004.
Title from document title page. Document formatted into pages; contains xi, 56 p. : ill. Vita. Includes abstract. Includes bibliographical references (p. 41-44).

Thesis (M.S.)--West Virginia University, 2006.
Title from document title page. Document formatted into pages; contains vii, 47 p. : ill. (some col.). Vita. Includes abstract. Includes bibliographical references (p. 35-38).

Le procédé de projection à froid a démontré ses avantages uniques dans la préparation de revêtements métalliques, composites et céramiques. Parmi ces revêtements, ceux constitués de magnésium pur ou de composites à matrice métallique à base de magnésium font partie des matériaux les plus prometteurs en raison de leur excellente résistance spécifique. Pourtant, les mécanismes de fabrication, par ce procédé de projection, des revêtements magnésium et composites à base de magnésium n'ont pas été étudiés. C'est le sujet de cette thèse. Les recherches menées dans cette étude s'articulent autour de plusieurs domaines, à savoir: La science des matériaux avec des études sur l'effet de la granulométrie des particules de magnésium, l'effet de la taille et de la teneur (15% vol. - 60 % vol.) des particules de renforcement (SiC) ; La mécanique des fluides avec des modélisations de géométrie de buse, d'écoulement de gaz et des vitesses des particules de magnésium et alliage de magnésium (AZ91D) ; Les caractérisations des dépôts avec des analyses de microstructure et des mesures de microdureté, d'adhérence et de comportement au frottement des revêtements;Les résultats montrent que la projection à froid peut être utilisée pour fabriquer des revêtements de magnésium purs ou composites sans aucune oxydation ou transformation de phase. La taille de ces particules doit rester dans une fourchette acceptable pour égaler la vitesse critique (entre 653 m*s-1 et 677 m*s-1) permettant la déposition. Concernant plus spécifiquement les résultats sur les revêtements de magnésium pur, le maximum de rendement de dépôt est obtenu par projection d'une poudre de granulométrie comprise entre 22 μm et 64 μm. L'adhérence atteint 11.6 ± 0.5 MPa lorsque le substrat est préchauffé à 200 oC. Pour le cas des revêtements AZ91D, la construction du dépôt s'effectue par effet de verrouillage mécanique. Le type de frottement observé sur ces revêtements est une usure adhésive. Dans les revêtements composites d'AZ91D - SiC, la teneur en particules de renforcement SiC présentes dans le dépôt diminue avec leur taille dû à l'effet "onde de choc". Le rendement de dépôt augmente avec la teneur en SiC de 15 vol.% à 30 vol.%, puis diminue au-delà de 30 vol%. Le type de frottement correspond à une usure par abrasion.

Notre thèse s’insère dans le cadre du projet ANR Micro « Matériaux Innovants Composites pour la Réparation d'Ouvrages : Approche fiabiliste du dimensionnement pour leur requalification et la prédiction de leur durabilité » L'objectif principal de la thèse est d’appréhender le problème de la durabilité par une approche expérimentale phénoménologique multi-échelle et de proposer des modèles de durée de vie au sens probabiliste. Le matériel d’étude est un carbone/époxy bidirectionnel non équilibré en masse (70% /30%) réticulé à l’ambiante et mis en œuvre par moulage au contact. Six vieillissements hygrothermiques obtenus par croisement entre les températures (20°C, 40°C et 60°C) et les humidités (50%, 75% et immersion) à diverses échéances ont été réalisés au cours de l’étude. Après identification des divers indicateurs, nous avons réalisé des analyses physico-chimiques (absorption-désorption, DSC, TMA, Infrarouge, DMA et Tomographie) ainsi qu’un suivi des caractéristiques mécaniques (traction, cisaillement interlaminaire, pull-out et double cisaillement) afin de définir les différents mécanismes de dégradation des propriétés mécaniques et physicochimiques des matrices polymères, des interfaces fibres–matrice, des joints de colle à l’interface composite-structure renforcée au cours du vieillissement pour le système classique Carbone/Epoxy. Ces indicateurs ont été analysés statistiquement afin de valider plus rigoureusement les tendances qui ont été observées. Le suivi des indicateurs mécaniques de performance par le vieillissement accéléré a été réalisé puis comparé à 1 an de vieillissement naturel. L’antagonisme des différents mécanismes de dégradations a été mis en évidence dans le cas de traction simple et du cisaillement interlaminaire. Il ressort que la plastification est le mécanisme qui affecte le plus les performances des composites carbone/époxy. Pour les températures élevées, il semble que la post-réticulation en densifiant le réseau a amélioré les cohésions interfaciales, ce qui a inhibé l’impact de la dégradation thermique sur les performances mécaniques. En comparant avec le vieillissement naturel, on a pu remarquer que le vieillissement en milieu aqueux était plus dégradant de façon générale et accélérait convenablement la dégradation en milieu naturel. En particulier, les tendances observées ne suivent pas des évolutions qui permettent d’apprécier trivialement la chute de performance par des modèles de prédiction. La qualité de l’adhérence composite/béton a été évaluée par des tests d’arrachement. Les fortes disparités entre les résultats rendent les interprétations délicates. Mais il a été mis en évidence que la post-réticulation semblent améliorer la cohésion tandis que la plastification est très néfaste pour la stabilité du joint de colle accélérant de façon excessive la dégradation en comparaison avec le vieillissement naturel. Cette instabilité a également été prouvée par les tests de double cisaillement où le délaminage était observé dès les premières échéances de vieillissement. La dernière partie du travail a consisté à proposer un traitement statistique des données pour valider tout d’abord les tendances observées expérimentalement, apporter plus d’informations et discuter sur le choix des modèles de prédiction. Bien que très apprécié par la communauté, l’utilisation des modèles physiques n’est pas systématique car elle suppose des performances dégénératives, ce qui en pratique n’est pas le cas. Une approche physique a été proposée sur la base de données épurée afin de respecter les conditions d’écriture du modèle. Le modèle choisi pour prédire la résistance ultime en traction est conservateur mais a le mérite d’être utilisable pour des études de fiabilité. L’enrichissement bayésien pourra être utilisé pour démontrer l’avantage qu’il peut conférer dans les études de fiabilité
Our thesis is part of this MICRO project "Innovative Composite Materials for the Repair of Structures: Reliability approach of the dimensioning for their requalification and the prediction of their durability". Final objective of the thesis is to understand the problem of sustainability through a multi-scale phenomenological experimental approach and to propose probabilistic life-time models. So, we defined the methodology of our study, as well as the methods, materials and analysis techniques. The study material is a non-equilibrium (70% / 30%) unbalanced bidirectional carbon / epoxy that is crosslinked at room temperature and made by hand layup process. Six hygrothermal aging obtained by crossing between temperatures (20°C, 40°C and 60°C) and humidities (50%, 75% and immersion) at various times were carried out during the study. After identifying the various indicators, we carried out physicochemical analyzes (absorption-desorption, DSC, TMA, Infrared, DMA and Tomography) as well as a follow-up of the mechanical characteristics (tensile, interlaminar shear, pull-out and double shear). These indicators were analyzed statistically to more rigorously validate the trends that were observed. The monitoring of mechanical performance indicators by accelerated aging was carried out and then compared to 1 year of natural aging. The antagonism of the various mechanisms of damage has been demonstrated in the case of simple traction and interlaminar shear. It appears that plasticization is the mechanism that most affects the performance of carbon / epoxy composites. For high temperatures, it appears that post-cure by densifying the network has improved interfacial cohesion, which has inhibited the impact of thermal degradation on mechanical performance. Comparing with natural aging, it was noted that aging in an aqueous condition was more generally degrading and aqueous conditions accelerated well the degradation in a natural environment. In particular, the trends observed do not follow evolutions that permit to write simplified prediction models. The quality of the composite / concrete adhesion was evaluated by pull-out tests. The strong disparities between the results make the analysis delicate. But it has been shown that the post-cure seems to improve the cohesion whereas the plasticization is very harmful for the stability of the bonded joints accelerating excessively the degradation in comparison to the natural aging. This instability has also been proven by the double shear tests where the delamination was observed from the first maturities of aging. The anchor length is reduced and a time-sensitive model has been proposed for the selected aging condition (60°C-immersion). On the other hand, this plasticization softens the failure due to the increased deformability of the joint. In this environmental condition, the monitoring of the elastic limit stress seems to be a relevant indicator for the monitoring of the durability because it simulates the natural aging with reasonable differences. The last part of our work consisted in the proposal of a statistical treatment of the data in order to validate firstly the trends observed experimentally, to bring more information and to discuss on the choice of the models of prediction. Although, physical model is very appreciated by the community, it is not systematically applicable. Indeed, it assumes degenerative performance, which in practice is not the case. A physical approach has been proposed on the refined database in order to respect the writing conditions of the model (degenerative trends). The model chosen to predict the ultimate tensile strength is conservative but applicable for reliability studies. Bayesian enrichment can be used to demonstrate the advantage it can confer in reliability studies

In der vorliegenden Arbeit wird ausgehend vom Stand der Wissenschaft und Technik für Ver-fahren und Werkstoffe des Titanlötens das Kaltgasspritzen in seiner Eignung als Vorbelo-tungsprozess beim löttechnischen Fügen von Titanlegierungen untersucht und qualifiziert. Die Parameter des Beschichtungsvorgangs werden dabei mit den resultierenden Schichtgefügen und späteren Lötergebnissen korreliert, wodurch eine Bewertung ermöglicht und ein Beitrag zum Verständnis der Mechanismen einer spritztechnischen Vorbelotung geliefert wird. Es werden dabei sowohl materialografische als auch mechanische Charakterisierungen durchge-führt. Ergänzt werden die Arbeitspunkte durch eine hochauflösende TEM-Untersuchung der Grenzfläche von kaltgasgespritzten Zink-Schichten und Aluminium-Substraten, die der Über-prüfung theoretischer Erkenntnisse zum Haftungsmechanismus kaltgasgespritzter metallischer Schichten auf Leichtmetallsubstraten dient. Die Arbeit schließt mit einer Diskussion und Fol-gerung und gibt Empfehlungen für weiterführende Forschungen auf diesem Gebiet
The present work qualifies the cold gas dynamic spray process (CGS) as a process for the application of braze filler coatings onto titanium alloy substrates. The work program results from needs and problems that were identified in the state-of-the-art of science and technology. The parameters of the coating process are correlated with the resulting coating microstruc-tures and the posterior brazing results. Materialographic and mechanic characterisations of the filler coatings and braze seams are carried out. Thereby, an evaluation of the braze filler ap-plication by cold gas spraying is permitted. In addition, high-resolution TEM investigations within the interfaces of a cold sprayed zinc coating and an aluminium base material proof the theory of the bonding mechanisms of CGS coatings on light weight metals. The work dis-cusses the achieved results and gives an outlook to continuative investigations in this field of science

Aluminiumschichten werden durch Kaltgasspritzen auf fünf verschiedene poly- und monokristalline keramische Werkstoffe (Al2O3 , AlN, SiC, Si3N4 , MgF2 ) appliziert. Dabei erfolgt eine Variation der Substrattemperatur und der Partikelgröße. Ausgewählte Proben werden einer nachfolgenden Wärmebehandlung unterzogen. Die im Fokus der Arbeit stehende Erforschung der an der Grenzfläche zwischen Aluminium und Keramik wirkenden Haftmechanismen erfolgt sowohl mithilfe einer mechanischen Charakterisierung (Stirnzugversuche) als auch durch verschiedene mikroskopische, spektroskopische und hochauflösende Methoden. Die Bewertung der Untersuchungsergebnisse zeigt, dass im Allgemeinen ein Anstieg der Haftzugfestigkeit mit steigender Substrat- und Wärmebehandlungstemperatur sowie mit zunehmender thermischer Effusivität des Substratwerkstoffs zu verzeichnen ist. Eine vergleichbare Auswirkung hat innerhalb bestimmter Grenzen die Zunahme der Partikelgröße. Mit der Heteroepitaxie wird neben der mechanischen Verklammerung ein weiterer wichtiger Haftmechanismus kaltgasgespritzter metallischer Schichten auf keramischen Substraten identifiziert. Die Ausbildung von quasiadiabatischen Scherbändern und statische Rekristallisationsprozesse wirken dabei als wichtige begleitende Mechanismen. Als Nachweis für heteroepitaktisches Wachstum ist die Existenz von (annähernd) parallelen, senkrecht oder geneigt zur Grenzfläche stehenden Ebenenpaaren, die eine geringe Gitterfehlanpassung aufweisen, zu werten. Der Vergleich mit PVD-Schichten zeigt, dass in Bezug auf die Orientierung von Gitterebenen verschiedene Mechanismen der Heteroepitaxie existieren, die von der atomaren Mobilität des Beschichtungswerkstoffs bestimmt werden.

碩士
國立臺灣科技大學
營建工程技術學系
81
To underatand the material behavior under theonditions similar to the real fire situation,this studyould adopt the standard time temperature curve for test.est results indicated that the residual strength of cold bonding fly ash lightweight aggregate would get to the lowest point after ignited at 600℃.At 1200℃, the residual strengh would achieve the highest point. The residual strength of fly-ash lightweight aggregate concrete after ignition would be the highest at 200℃,lose at 600℃,and lose completely at 800℃.Compared with nomal fly-ashlight weight aggregate concrete had better anti-separatingapability, and better fire resisting capability when the strengthas almost equal to that of nomal concrete.

博士
國立交通大學
機械工程學系
99
This study comprises three sections that include cold roll-bonding, forming limit diagrams (FLDs), and sheet hydroforming (SHF). First, the bonding performance of Al/Cu clad metal sheet with different initial thickness and reduction rate were discussed. The heat flux calculation with thermal conduction, plastic heat and friction consideration were adopted in finite element analysis (FEA). The temperatures of clad metal sheet at maximum reduction region were obtained by rigid-plastic FE code (DEFORM-2D), and then the temperature distribution of Al/Cu clad metal sheets with different combinations of process parameter were determined. The simulation results pointed out that higher rotation speed, higher reduction rate, and asymmetrical rotation are positive to improve the bonding performance for clad metal sheets. The possibility of applying FLDs to fracture prediction of clad metal sheets is examined. The forming limits of Al/Cu clad metal sheets with different thickness reduction are investigated via FLD test. Moreover, deep drawing tests are carried out to compare the numerical results. The results pointed out that the fractures of clad metal sheets are predicated by experimental FLDs. For clad metal sheet application, the SHF was adopted to improve the formability of Ti/Al clad metal sheet used in 3C product housings. Some significant process parameters were analyzed for improving formability of clad metal sheet by FEA. In numerical simulation, a virtual film technique was proposed to realistically approach the hydraulic loading for SHF. And pre-bulging and tool modification are proposed to reduce thinning ratio of Ti/Al clad metal sheet, operation stage, and tooling cost.