A study is carried out into fracture behavior of steel/steel laminates both experimentally and through finite element analysis (FEM). The laminates produced by hot pressing consisted of low carbon and medium carbon steels with two volume fractions / 0.41 and 0.81. Fracture toughness, JIC has been measured using partial unloading technique assuming a critical value of crack extension. The technique is initially applied to monolithic material and then to the laminates in crack divider orientation. Evaluation of fracture toughness of laminates indicates that there is a substantial improvement of JIC with increase in the volume fraction. The systems under study were also evaluated by FEM modeling with the use MARC package program. To evaluate JIC, the problem has been evaluated in several steps / first two-dimensional plane strain problem is considered. This is followed by three-dimensional case and then by an artificially layered system, all for monolithic materials. Values of JIC derived were close to one another in all cases. Following this verification, the method, as implemented in layered monolithic system, was applied to laminates. This has shown that JIC of laminates can be predicted using FEM analysis, including the delamination. Values of JIC varied in the same manner as the experiment verifying that fracture toughness in the current system increases with increase in volume fraction. It has been concluded that modeling as implemented in this work can be used for useful composite systems incorporating hard/brittle reinforcements both in crack divider and crack arrester orientation.

abstract: With the increasing focus on developing environmentally benign electronic packages, lead-free solder alloys have received a great deal of attention. Mishandling of packages, during manufacture, assembly, or by the user may cause failure of solder joint. A fundamental understanding of the behavior of lead-free solders under mechanical shock conditions is lacking. Reliable experimental and numerical analysis of lead-free solder joints in the intermediate strain rate regime need to be investigated. This dissertation mainly focuses on exploring the mechanical shock behavior of lead-free tin-rich solder alloys via multiscale modeling and numerical simulations. First, the macroscopic stress/strain behaviors of three bulk lead-free tin-rich solders were tested over a range of strain rates from 0.001/s to 30/s. Finite element analysis was conducted to determine appropriate specimen geometry that could reach a homogeneous stress/strain field and a relatively high strain rate. A novel self-consistent true stress correction method is developed to compensate the inaccuracy caused by the triaxial stress state at the post-necking stage. Then the material property of micron-scale intermetallic was examined by micro-compression test. The accuracy of this measure is systematically validated by finite element analysis, and empirical adjustments are provided. Moreover, the interfacial property of the solder/intermetallic interface is investigated, and a continuum traction-separation law of this interface is developed from an atomistic-based cohesive element method. The macroscopic stress/strain relation and microstructural properties are combined together to form a multiscale material behavior via a stochastic approach for both solder and intermetallic. As a result, solder is modeled by porous plasticity with random voids, and intermetallic is characterized as brittle material with random vulnerable region. Thereafter, the porous plasticity fracture of the solders and the brittle fracture of the intermetallics are coupled together in one finite element model. Finally, this study yields a multiscale model to understand and predict the mechanical shock behavior of lead-free tin-rich solder joints. Different fracture patterns are observed for various strain rates and/or intermetallic thicknesses. The predictions have a good agreement with the theory and experiments. / Dissertation/Thesis / Ph.D. Mechanical Engineering 2011

Suite à la demande constante de réduire la taille des transistors et celle des dispositifs électroniques, guidée par la loi de Moore, l'intégration 2D n'est plus adaptée à cette demande croissante. Cela a conduit à l'intégration 3D des dispositifs actifs à l'aide de piliers Cu/Ni recouverts d'alliages de brasage à base de Sn. Dans les années à venir, les applications qui demandent des interconnexions à haute densité (optoélectroniques, microdisplays, les détecteurs IR, MEMS) nécessiteront l’utilisation de pas d'interconnexions inférieurs à 10 µm. Cependant, les piliers Cu/Ni/alliage de brasure base Sn n'ont jamais été étudiés en profondeur pour un si petit pas d'interconnexion. Avec la réduction de la dimension d'interconnexion, le diamètre des piliers Cu/Ni/alliage de brasure est réduit également. De ce fait, la formation des intermétalliques, qui joue un rôle primordial dans la bonne tenue de la jonction, peut poser des problèmes majeurs en raison de la réduction des dimensions du pilier de Cu et de l’alliage de brasure.Le travail de cette thèse est consacré à l'étude métallurgique et à la caractérisation d’interconnections de très petites dimensions (diamètre de 5 µm et pas de 10 µm) avec comme objectif principal l’étude des mécanismes physicochimiques des interactions entre les alliages de soudure Sn-Ag et les couches de Ni ou Ni/Au. Les mécanismes des interactions à l'état solide entre Sn et Ni ainsi que l’évolution du joint vers la transformation totale en intermétallique Ni3Sn4 (Solid-Liquid-Intercondiffusion - SLID processus), ont été étudiés pour la première fois dans de tels systèmes de dimensions micrométriques. De plus, les propriétés mécaniques et électriques ainsi que la stabilité thermique de ces interconnexions ont été étudiées. L’observation pour la première fois de la formation de la phase Ni3Sn2 à l’interface Ni/Sn à 200°C lors des vieillissements thermiques présente un intérêt pratique de grande importance. / With the constant demand for reducing the feature size of transistors and that of the devices, which is guided by Moore’s law, 2D integration is no longer fit to adapt the growing demand. This has led to 3D integration of active devices with the help of Cu/Ni pillars capped with Sn based solder alloys. In the coming years, applications which demand high density interconnects (optoelectronic, microdisplays, IR-detectors, MEMS) will require an interconnect pitch of 10 µm and below. However, Cu/Ni/solder pillars have never been investigated in depth for such a small interconnection pitch. With reduction of interconnect dimension, the diameter of Cu/Ni pillar and solder alloy also reduces. Thus, it is feared that the intermetallic formation, which is the key phenomenon responsible for the bonding, may be problematic due to the reduction in size of Cu pillar capped with solder alloy.The thesis is dedicated to the metallurgical study and its characterization for very small interconnects (5 µm) at 10 µm pitch, where the main focus is given on the physio-chemical mechanisms of soldering between Sn-Ag solder alloy and Ni or Ni/Au layers. For the first time, the mechanism of solid-state interactions between Sn and Ni is studied in depth and also for the first time the Ni3Sn4 SLID (Solid-Liquid-lnterdiffusion) system as an interconnect has been investigated at these dimensions. Moreover, the mechanical and electrical properties as well as the thermal stability of these interconnects are studied. Interestingly, during the latter part of this study, Ni3Sn2 layer is observed during aging of the Ni/Ni3Sn4 system for low temperature (200°C).

Inspection of optical components is essential to assure the quality and performance of optical systems. Evaluation of optical components includes metrology measurements of surface topography. It also requires optical measurements including refractive index, thin film thickness, reflectivity and transmission. The dispersion characteristics of optical constants including refractive index are also required. Hence, various instruments are used to make these measurements in research laboratories and for quality assurance. Clearly, it would be a significant advantage and cost saving if a technique was developed that could combine surface metrology with optical measurements. {Coherence Scanning Interferometry} (CSI) (also referred to as {Scanning White Light Interferometry} (SWLI)) has been used widely to measure surface topography with sub-nanometre vertical resolution. One of the benefits of the CSI is that the technique is non-contacting and hence non-destructive. Thus the test surfaces are not affected by the measurement using a CSI instrument whereas damage to the surfaces can occur when using traditional contact methods such as stylus profilometry. However use of CSI is geometrically limited to small areas ($\lesssim 10 \times 10$ mm) with gentle slopes ($\lesssim \ang{40}$) because of the numerical aperture of objective lens whereas stylus profilometry works well with larger areas and higher slopes due to the range of motion of the gauge and the traverse unit. Since the CSI technique is optical and involves light reflection and interference it is possible to extend the technique for the measurement of the thickness of transparent films, the roughness of surfaces buried beneath thin films or interfacial surfaces. It may also be used to determine spectral complex refractive index. This thesis provides an analytical framework of new methods to obtain complex refractive index in a visible light domain and interfacial surface roughness (ISR). It also provides experimental verification of these new capabilities using actual thin film model systems. The original Helical Complex Field (HCF) function theory is presented followed by its existing extensions that enable determination of complex refractive index and interfacial surface roughness. Further theoretical extensions of the HCF theory are also provided: A novel theory to determine the refractive index of a (semi-)transparent film is developed to address the constraint of the current HCF theory that restricted its use to opaque materials; Another novel theory is provided to measure ISR with noise compensation, which avoids erroneous surface roughness caused by the numerical optimisation affected by the existence of noise. The effectiveness of the ISR measurement with noise compensation has been verified using a number of computer simulations. Stylus profilometry is a well established method to provide a profile and has been used extensively as a 'reference' for other techniques. It normally provides a profile on which the roughness and the waviness are computed. Extension of the stylus profilometry technique to areal measurement of asymmetrical surfaces, namely raster scan measurement, requires a system to include error compensation between each traverse. The system errors and the random errors need to be separately understood particular when the measurement of a surface with nanometre-order accuracy is required. In this thesis a mathematical model to locate a stylus tip considering five mechanical errors occurring in a common raster scan profilometer is provided. Based on the model, the simulator which provides an areal measurement of a sphere was developed. The simulator clarified the relationship between the Zernike coefficients obtained from the form residual and the size of the errors in the form of partial derivatives of Zernike coefficients with respect to the errors. This provides theoretical support to the empirical knowledge of the relationship between the coefficients and the errors. Furthermore, a method to determine the size of errors directly from Zernike coefficients is proposed supported by simulations. Some of the error parameters were accurately determined avoiding iterative computation with this method whereas the errors are currently being determined by iterative computation.

Dans de nombreuses applications aérospatiales, on peut trouver des films liquides cisaillés, c'est-à-dire une fine couche liquide qui ruisselle sur une paroi entrainée par le gaz. Par exemple, une couche de liquide peut se développer sur la voilure des avions, givrer et dégrader les performances. Des vagues peuvent se développer à l'interface liquide-gaz, et l'analyse correcte de ces instabilités devient très importante pour modéliser ce phénomène physique. En effet, la présence d'instabilités modifie les échanges liquide-gaz, notamment les transferts de masse et chaleur. Le but de cette thèse est de développer une technique permettant de coupler la phase gazeuse afin de reproduire les interactions à l'interface. La couche de liquide étant beaucoup plus mince que celle du gaz, une approche intégrale sur l'épaisseur est utilisée pour la modélisation. Enfin, deux cas d'un écoulement diphasique se développant dans une conduite confinée et dans une conduite plus large sont étudiés. les résultats sont ensuite comparés à des autres méthodes de référence, plus coûteuses en temps de calcul. / In many aerospace applications one can find liquid films sheared by a gas flow. In example, these liquid sheets can develop on aircraft wings, freeze and then destroy the aerodynamics performances. Waves can develop at the liquid-gas interface, and the correct analysis of such instabilities becomes very important to model this physical phenomenon. Indeed, instabilities mdify liquid-gas exchanges, such as mass and heat transfers. The aim of the present work consists in developing a technique to couple the liquid phase to the gas phase in order to reproduce the interactions at the interface. Since the liquid layer is much thinner then the gas, anintegral approach is used for modeling. Finally, two cases of a two-phase flow developing in a strictly confined channel and in a large channel are studied. Results are then compared to other reference methods which are more expensive in terms of computational cost.

Original analytical theories are developed for partitioning mixed-mode fractures on rigid interfaces in laminated orthotropic double cantilever beams (DCBs) based on 2D elasticity by using some novel methods. Note that although the DCB represents a simplified case, it provides a deep understanding and predictive capability for real applications and does not restrict the analysis to a simple class of fracture problems. The developed theories are generally applicable to so-called 1D fracture consisting of opening (mode I) and shearing (mode II) action only with no tearing (mode III) action, for example, straight edge cracks, circular blisters in plates and shells, etc. A salient point of the methods is to first derive one loading condition that causes one pure fracture mode. It is conveniently called the first pure mode. Then, all other pure fracture modes can be determined by using this pure mode and the property of orthogonality between pure mode I modes and pure mode II modes. Finally, these 2D-elasticity-based pure modes are used to partition mixed-mode fractures into contributions from the mode I and mode II fracture modes by considering a mixed-mode fracture as the superposition of pure mode I and mode II fractures. The partition is made in terms of the energy release rate (ERR) or the stress intensity factor (SIF). An analytical partition theory is developed first for a DCB composed of two identical linear elastic layers. The first pure mode is obtained by introducing correction factors into the beam-theory-based mechanical conditions. The property of orthogonality is then used to determine all other pure modes in the absence of through-thickness-shear forces. To accommodate through-thickness shear forces, first two pure through-thickness-shear-force pure modes (one pure mode I and one pure mode II) are discovered by extending a Timoshenko beam partition theory. Partition of mixed-mode fractures under pure through-thickness shear forces is then achieved by using these two pure modes in conjunction with two thickness-ratio-dependent correction factors: (1) a shear correction factor, and (2) a pure-mode-II ERR correction factor. Both correction factors closely follow a normal distribution around a symmetric DCB geometry. The property of orthogonality between all pure mode I and all pure mode II fracture modes is then used to complete the mixed-mode fracture partition theory for a DCB with bending moments, axial forces and through-thickness shear forces. Fracture on bimaterial interfaces is an important consideration in the design and application of composite materials and structures. It has, however, proved an extremely challenging problem for many decades to obtain an analytical solution for the complex SIFs and the crack extension size-dependent ERRs, based on 2D elasticity. Such an analytical solution for a brittle interfacial crack between two dissimilar elastic layers is obtained in two stages. In the first stage the bimaterial DCB is under tip bending moments and axial forces and has a mismatch in Young s modulus; however, the Poisson s ratios of the top and bottom layers are the same. The solution is achieved by developing two types of pure fracture modes and two powerful mathematical techniques. The two types of pure fracture modes are a SIF-type and a load-type. The two mathematical techniques are a shifting technique and an orthogonal pure mode technique. In the second stage, the theory is extended to accommodate a Poisson s ratio mismatch. Equivalent material properties are derived for each layer, namely, an equivalent elastic modulus and an equivalent Poisson s ratio, such that both the total ERR and the bimaterial mismatch coefficient are maintained in an alternative equivalent case. Cases for which no analytical solution for the SIFs and ERRs currently exist can therefore be transformed into cases for which the analytical solution does exist. It is now possible to use a completely analytical 2D-elasticity-based theory to calculate the complex SIFs and crack extension size-dependent ERRs. The original partition theories presented have been validated by comparison with numerical simulations. Excellent agreement has been observed. Moreover, one partition theory is further extended to consider the blister test and the adhesion energy of mono- and multi-layered graphene membranes on a silicon oxide substrate. Use of the partition theory presented in this work allows the correct critical mode I and mode II adhesion energy to be obtained and all the experimentally observed behaviour is explained.

Made available in DSpace on 2016-06-02T19:12:08Z (GMT). No. of bitstreams: 1 3389.pdf: 4509591 bytes, checksum: 1b73995d4885804e38b608030ab546cd (MD5) Previous issue date: 2009-09-25 / Universidade Federal de Sao Carlos / Poly(ethylene terephthalate) (PET) is a semi-crystalline thermoplastic widely used for packaging of aereted soft drinks, which makes the recycling of post-consumer PET material necessary to prevent the negative environmental impact of its disposal. The recycling of PET as an engineering thermoplastic can be accomplished by the incorporation of glass fiber (GF) and elastomeric impact modifier to the PET matrix, forming a ternary hybrid composite. To assure an appropriate balance of mechanical properties of stiffness, strength and toughness in this composite, it is important that the GF and rubber particles are dispersed separately in the matrix, avoiding the encapsulation of the fibers by the rubber phase and promoting, simultaneously GF reinforcement and rubber toughening mechanisms. In this work, the influence of selective interfacial compatibilization on the mechanical properties of hybrid composites of recycled PET was studied, as the matrix polymer was modified with reactive olefin elastomers of E-MA-GMA and E-EA-MAH, as well as with short GF treated with either epoxy (FV952) or aminesilanes (FV983). Ternary systems of PET/E-MA-GMA/FV952, PET/E-MA-GMA/FV983 and PET/E-EA-MAH/FV983 were compounded in a twin-screw corotating ZSK-30 extruder and, depending on the relative reactivities of PET s chain-end groups with the functionalities present on the GF surfaces and in the E-MA-GMA and E-EA-MAH terpolymers, the GF is encapsulated or not by the elastomer phase and, consequently, the mechanical properties of the hybrid composites are affected differently. Mechanical tests and torque rheometry data indicated high reactivity between PET and E-MA-GMA terpolymer, and low reactivity with the E-EA-MAH. Analysis of tensile and Izod impact tests results, as well as from fiber-polymer interfaces observations by SEM, indicated good fiber-polymer adhesion in PET/E-MA-GMA/FV952 and PET/E-MA-GMA/FV983 systems, and fiber encapsulation by rubber particles in the case of the PET/E-EA-MAH/FV983 system. / O poli(tereftalato de etileno) (PET) é um termoplástico semi-cristalino largamente utilizado na fabricação de embalagens de refrigerantes, a ponto de necessitar a sua reciclagem pós-consumo para evitar impacto ambiental negativo do seu descarte. A reciclagem do PET como um termoplástico de engenharia pode ser realizada mediante a incorporação de reforço de fibra de vidro (FV) e modificador de impacto elastomérico à matriz de PET, formando um compósito híbrido ternário. Para assegurar um adequado balanço de propriedades mecânicas de rigidez, resistência e tenacidade neste compósito é importante que as fibras de vidro e as partículas de borracha estejam dispersas separadamente na matriz, evitando o encapsulamento da FV pela borracha e promovendo, simultaneamente, mecanismos de reforço mecânico com FV e tenacificação com partículas de borracha. Neste trabalho é analisada a influência da compatibilização interfacial seletiva nas propriedades mecânicas de compósitos híbridos de PET reciclado modificados com elastômeros olefínicos reativos E-MA-GMA (polietileno-co-acrilato de metila-co-metacrilato de glicidila) e E-EA-MAH (polietileno-co-acrilato de etila-co-anidrido maléico), assim como com FV s curtas contendo tratamentos superficiais de silanos epóxi (FV952) ou amino-funcionais (FV983). Sistemas ternários de PET/E-MAGMA/ FV952, PET/E-MA-GMA/FV983 e PET/E-EA-MAH/FV983 foram preparados numa extrusora dupla rosca corrotacional ZSK-30 e, dependendo da reatividade relativa entre as funcionalidades presentes na superfície das FV s, nos terpolímeros E-MA-GMA e E-EA-MAH, e dos grupos co-reativos finais de cadeia do PET, a FV é encapsulada ou não pelo elastômero e, consequentemente, as propriedades mecânicas dos compósitos híbridos são afetadas de maneira distinta. Ensaios mecânicos e de reometria de torque indicaram alta reatividade entre o PET e o terpolímero E-MA-GMA, e baixa reatividade com o E-EA-MAH. A análise de resultados dos ensaios mecânicos de tração e impacto Izod, assim como das interfaces fibra-polímero observadas em MEV, indicou a ocorrência de boa adesão das fibras nos sistemas de PET/E-MA-GMA/FV952 e PET/E-MA-GMA/FV983, e encapsulamento da FV pela fase elastomérica no sistema de PET/E-EA-MAH/FV983.

Orientador: Paulo Sollero / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecanica / Made available in DSpace on 2018-08-10T03:16:07Z (GMT). No. of bitstreams: 1 Paiva_SeilaVastiFariade_M.pdf: 1387945 bytes, checksum: 04ad3c76f01698f24ef5fd7ebfb49264 (MD5) Previous issue date: 2006 / Resumo: Nesta dissertação é apresentada uma análise de problemas da mecânica da fratura elástica linear em estruturas bimateriais anisotrópicas. Utilizando o método dos elementos de contorno é possível calcular os fatores de intensidade de tensão em problemas planos (2D) devido à presença de trincas interfaciais entre as lâminas que compõem o material. A estrutura pode estar submetida à carregamento em modo I ou modo misto. O problema é modelado usando-se a técnica de sub-regiões para descrever cada um dos diferentes subdomínios, representado por cada material. Na interface das sub-regiões, em que o domínio é dividido, são impostas condições de equilíbrio de forças e continuidade de deslocamentos, exceto na região que corresponde à trinca. O comportamento singular apresentado pelo campo de tensões próximo à ponta da trinca é modelado com elementos de ponto a um quarto com singularidade de forças de superfície. São apresentados exemplos numéricos de problemas com carregamentos no plano. Foi também apresentada a análise de convergência de malhas, mostrando uma pequena dependência da discretização mesmo quando malhas pouco refinadas foram usadas. Alguns dos exemplos têm correspondentes na literatura, os quais foram utilizados para comparação com os resultados obtidos. Observou-se uma boa concordância na comparação dos resultados / Abstract: This thesis presents an analysis of problems of linear elastic fracture mechanics in anisotropic bimaterial structures. Using the boundary element method, it is possible to evaluate stress intensity factors in plane problems (2D) due to the presence of interfacial cracks between the laminae that constitute the material, when the structure is submitted to a mode I or in mixed mode loading. The problem is modeled using the subregion technique to describe each one of the different subdomains, represented by each material. On the interface of subregions, which the domain is divided, conditions of tractions equilibrium and displacements continuity are imposed, except in the corresponding crack region. The singular behavior presented by the stress field near the crack tip is modeled by traction singular quarter point element. Numerical examples of problems with in-plane loading are presented. Mesh convergence analyses are also presented, showing little dependence on the discretization even when coarse meshes were used. Some of these examples have correspondents in literature, that were used for comparisons with the obtained results. A good agreement in the comparisons of results was observed. / Mestrado / Mecanica dos Sólidos e Projeto Mecanico / Mestre em Engenharia Mecânica

L’embolisation vasculaire est un traitement peu invasif utilisé pour éliminer ou interrompre de façon sélective les apports vasculaires à des régions spécifiques du corps. Une technique consiste en l’introduction d’un microcathéter dans le vaisseau sanguin cible et à administrer un agent embolique qui réagit au contact du sang. Les colles emboliques à base de cyanoacrylate sont les principaux agents liquides utilisés pour l’embolisation à cause de leur faible viscosité, leur bonne capacité de pénétration et leur faible toxicité tissulaire. Pour permettre sa détection après injection, la colle est mélangée à un agent de contraste radio-opaque telle que l’huile iodée Lipiodol®. Bien que la technique soit couramment utilisée, il existe peu de données sur la dynamique du processus d’injection au sein de flux sanguins complexes ou sur la cinétique de polymérisation du mélange colle-Lipiodol. Par conséquent, une occlusion sans danger est difficile à réaliser, même entre les mains de radiologues expérimentés. Le principal objectif de la thèse est d’étudier de façon quantitative les propriétés physiques et la cinétique de polymérisation des colles cyanoacrylates mélangées au Lipiodol dans différentes proportions. Nous avons conçu un nouveau dispositif expérimental pour caractériser le processus de polymérisation d’un mélange colle/Lipiodol en contact avec une solution ionique ou protéinée. Les résultats montrent un processus de polymérisation rapide à l’interface entre la colle et le substrat, suivi par la proagation d’un front de polymérisation dans le volume de préparation de colle. Les constantes de temps des processus dépendent des compositions de la solution et du mélange de colle. Un autre objectif est d’analyser le processus d’embolisation dynamique. Un modèle in vitro du processus d’injection est utilisé pour étudier en premier lieu la formation de goutte entre deux flux immiscibles et qui ne réagissent pas entre eux. L’injection d’une préparation de colle dans une solution ionique en écoulement est ensuite réalisée pour montrer l’influence conjointe de la polymérisation et de l’hydrodynamique. C’est la première fois qu’une telle caractérisation exhaustive de colles emboliques à base de cyanoacrylate est obtenue. Les résultats peuvent apporter des informations cruciales aux radiologues interventionnels, ce qui les aidera à comprendre et contrôler le comportement de la colle après injection afin d’accomplir une oblitération permanente des vaisseaux en toute sécurité. / Vascular embolization is a minimally invasive treatment used to selectively eliminate or stop the vascular supply to specific body areas. One technique consists of navigating a microcatheter into the targeted blood vessel and injecting an embolic agent which reacts in contact with blood. Cyanoacrylate-based embolic glues are the main liquid adhesives used for vascular embolization owing to their low viscosity, good penetration ability and low tissue toxicity. To enable its detection once injected, the glue is mixed with a radio-opaque contrast agent such as the Lipiodol iodized oil. Although the technique is commonly used, there is very little information on the dynamics of the injection process in complex blood flows or on the polymerization kinetics of the glue-Lipiodol mixture. Consequently, safe occlusion is difficult to achieve, even in the hands of experienced radiologists. The main objective of the thesis is to quantitatively investigate the physical properties and polymerization kinetics of cyanoacrylate glues mixed with Lipiodol in different proportions. We have designed a new experimental setup to characterize the polymerization process of a glue/Lipiodol mixture on contact with an ionic or proteinaceous solution. We find that there is a fast polymerization process at the interface between the glue and the substrate, followed by the propagation of a polymerization front in the glue mixture volume. The time constants of the processes depend on the solution and glue mixture compositions. Another objective is to analyze the dynamic embolization process. An in vitro model of the injection process is used to first investigate the drop formation between two non-reacting immiscible flows. The injection of a glue mixture into a flowing ionic solution is then performed to show the joint influence of polymerization and hydrodynamics. It is the first time that such comprehensive characterization of cyanoacrylate-based embolic glues is acquired. The results can provide crucial information to interventional radiologists, that will help them understand and control the glue behavior after injection to achieve a safe and permanent obliteration of the vessels.

La coextrusion multinanocouche est un procédé innovant qui permet de combiner deux polymères afin de produire des films composés de couches alternées dont le nombre peut être contrôlé et atteindre plusieurs milliers. Ainsi, les épaisseurs des couches individuelles dans le film peuvent en théorie atteindre quelques nanomètres. Les effets de confinement des chaînes macromoléculaires ainsi que la multiplication des interfaces peuvent alors conduire à des propriétés macroscopiques améliorées, pertinentes dans un contexte industriel (optiques, mécaniques, barrière aux gaz, …). Néanmoins, à ces échelles, des défauts dans la continuité des couches peuvent apparaître pendant la mise en forme et affecter ces propriétés. L’objectif de cette thèse est d’identifier les paramètres clés, procédés et matériaux, et de mieux comprendre les mécanismes à l’origine des instabilités conduisant à ces inhomogénéités de la nanostructure. Dans ce cadre, deux polymères amorphes ont été principalement étudiés, le polyméthacrylate de méthyle (PMMA) et le polystyrène (PS). Des films composés de 65 à plus de 8000 couches alternées, à différents taux d’étirage et compositions massiques, ont été fabriqués dans le but d’étudier la stabilité du procédé à différentes échelles et principalement à l’échelle nanométrique. Les films obtenus ont été caractérisés par microscopie, en particulier la microscopie à force atomique (AFM). Un premier travail a consisté à mettre en place une démarche statistique et quantitative pour caractériser l’épaisseur moyenne des couches obtenues, mais aussi la distribution d’épaisseur et la stabilité des couches. Puis, nous avons cherché à sonder l’effet de différents paramètres procédés et matériaux sur l’homogénéité des structures à l’échelle micronique. En se plaçant ensuite dans des conditions stables à ces échelles, nous avons cherché à faire varier de manière systématique les paramètres procédés pour étudier la stabilité des couches à l’échelle nanométrique. Nous avons mis en évidence l’existence d’une épaisseur critique en dessous de laquelle les couches rompaient, située autour de 10 nm pour le couple PS/PMMA. Lorsque l’épaisseur visée est de l’ordre de la dizaine de nanomètres ou inférieures, le taux de rupture de couches augmente également fortement. Des hypothèses sont faites quant aux causes de ces ruptures et de l’existence de cette épaisseur critique. Nous suggérons que ces ruptures peuvent être provoquées par des perturbations interfaciales (liées à des impuretés et/ou aux fluctuations thermiques) amplifiées par les forces de van der Waals qui deviennent non négligeables pour de faibles épaisseurs de couches (typiquement inférieures à 40 nm) et sont attractives entre deux couches de même nature. Des expériences modèles sont proposées dans la perspective d'une approche quantitative des conditions critiques d'apparition de ces défauts. / Nanolayer coextrusion enables the production of polymeric films composed of up to thousands of alternating layers. The thickness of each layer can in theory be controlled, by monitoring the number of layers, the mass ratio of the polymers, and the draw ratio of the film at the exit die, and can decrease down to several nanometers. It has been shown that such films can display drastically improved macroscopic properties, such as optical, gas barrier, or mechanical, due to confinement and interfacial effects. However, layer beak-up phenomenon occurring at such thicknesses, impacting the resulting properties, has also been reported for many polymer pairs. The goal of this thesis is to investigate the causes for these break-ups and for the instabilities leading to them. Most of this work deals with multilayer films of polymethyl methacrylate (PMMA) and polystyrene (PS), two amorphous polymers which blends were widely studied in the literature. Films with 65 to more than 8000 layers were fabricated by modifying processing and molecular parameters, to determine their impact on the homogeneity of the samples. These films were characterized mainly by using microscopy techniques, and especially atomic force microscopy (AFM), to extract not only the mean layer thickness, but distribution of thicknesses and the ratio of broken layers within the sample. A first necessary step was to develop a reliable statistical and quantitative analysis to obtain such information. Then, a first study focused on the effects of some process and material parameters on the homogeneity of multilayer films with micronic thicknesses. Choosing favourable experimental conditions at these scales, nanolayered films were then fabricated. We showed the existence of a critical layer thickness, below which layer breakup, estimated at around 10 nm for PS/PMMA films. When the targeted thickness is around or below 10 nm, the amount of broken layers increases significantly. We make the hypothesis that the layer breakup phenomenon is due to interfacial instabilities driven by van der Waals forces. The thicknesses of the layers we can reach with this process are so small that dispersive forces between two layers composed of the same polymer cannot be neglected (typically below 100 nm). Model experiments are proposed to quantitatively study the critical conditions of appearance of these layer breakups.