L'imbibition d’eau pour les matériaux granulaires induit des changements dans la morphologie des ponts capillaires qui passent d'une forme isolée (entre deux grains voisins), à une forme fusionnée (entre plusieurs grains voisins). Ces changements de morphologie des ponts liquides influencent le comportement mécanique de ces matériaux, et peuvent être à l’origine d’instabilités telles que l’effondrement capillaire. La thèse présente une approche expérimentale multi-échelle au laboratoire de l'effondrement capillaire de matériaux granulaires lors d'une imbibition d'eau. L’approche concerne les trois échelles: macroscopique d'un Volume Élémentaire Représentatif, mésoscopique de quelques grains et locale de trois ou quatre grains. À l'échelle macroscopique, des essais d’imbibition, dans une cellule triaxiale, ont permis l'identification et l'analyse du phénomène d'effondrement capillaire en mettant l'accent sur l'évolution des déformations dans le temps. Les essais sont réalisés sur deux types de matériaux granulaires, le premier est un matériau constitué de billes de verre et le deuxième est un sable concassé. Une fraction argileuse est parfois incorporée au matériau. Plusieurs paramètres ont été étudiés en vue de comprendre leurs contributions dans le déclenchement du phénomène d'effondrement comme : la granularité, la teneur en eau initiale, la compacité initiale et le pourcentage des particules argileuses. Aux échelles mésoscopique et locale, on propose une étude expérimentale de caractérisation du comportement mécanique des matériaux granulaires dans le régime pendulaire et funiculaire. On s’intéresse en particulier à l’effet de l’imbibition et de la coalescence sur la force capillaire entre les grains solides à l’échelle considérée. Les essais d'imbibition sont réalisés par ajout d’incréments de volume d’eau aux ponts capillaires. Les résultats relatifs au comportement et à l’effondrement à l’échelle macroscopique lors de l'imbibition d'eau sont discutés en s’aidant des résultats obtenus aux échelles inférieures. / Wetting in granular materials induces changes in the morphology of capillary bridges which pass from an isolated form (between two neighboring grains) to a merged form (between several neighboring grains). These changes in the morphology of the liquid bridges impact the mechanical behavior of these materials, and can lead to instabilities such as capillary collapse. The thesis presents a multi-scale experimental approach in the laboratory of the capillary collapse of granular materials during wetting. The approach concerns the three scales: macroscopic of a Representative Elementary Volume, mesoscopic of several grains and local of three or four grains. At the macroscopic scale, the wetting tests, carried out in a triaxial cell, allowed the identification and the analysis of capillary collapse phenomenon, focusing on the evolution of deformations over time. The tests are carried out on two granular materials, the first is a material made of glass beads and the second is a crushed sand. A clay fraction is sometimes incorporated into the material. Several parameters have been studied in order to understand their contributions to the triggering of the collapse phenomenon, such as: grain size, initial water content, initial compactness and percentage of clay particles. At the mesoscopic and local scales, an experimental study is proposed to characterize the mechanical behavior of a granular materials, in the pendular and funicular regimes. In particular, this study focus on the effect of the wetting and the coalescence of bridges, on the capillary force between grains at the considered scale. Wetting tests were performed by adding water volume increments to the capillary bridges. The results on behavior and collapse at the macroscopic scale during wetting are discussed using the results obtained on the lower scales.

O presente trabalho tem como proposição investigar a hipótese de que a diminuição da tensão superficial do líquido favorece o comportamento reológico de suspensões concentradas, uma vez que as partículas estão mais próximas e a contribuição da força de capilaridade possivelmente aumenta. Como suspensões concentradas tendem ao comportamento viscoelástico, investigou-se métodos reológicos propícios para analisar possíveis consequências devido à alteração da tensão superficial da água. Foram utilizados dois carbonatos de cálcio equivalentes (P1 e P5) que se diferenciam pela distribuição granulométrica. Utilizou-se dois dispersantes de mercado e etilenoglicol como modificadores de tensão superficial. A análise de superfície pelo ensaio de potencial zeta, revelou carga superficial positiva. Embora os pós sejam equivalentes, a mobilidade eletroforética do P5 é menor. Verificou-se que o íon cálcio é determinante do potencial. Verificou-se contribuição eletrostática apenas dos dispersantes. O ensaio de gota pendente constatou diminuição da tensão superficial da água com os três aditivos. Ensaios de ascensão capilar pelo método de Washburn revelaram maiores ângulos de contato para ensaios com aditivos, sendo menor para P5. Avaliou-se geometrias e métodos reológicos a fim de selecionar bom conjunto para medidas de viscoelasticidade, sendo oscilatório de tensão e geometria vane escolhidos. O acréscimo dos dispersantes resultou em menores valores de G\' e tensões de escoamento, enquanto o etilenoglicol resultou em maiores. Não há relação clara entre valores calculados de ângulo de contato e mobilidade eletroforética. Os ensaio reológicos e de mobilidade relacionaram-se apenas para os dispersantes. A hipótese foi verificada pelos valores de tensão de escoamento e IPS. Para os dispersantes, foi possível observar comportamento próximo à hipótese, quanto menor foi a tensão superficial do líquido, menores valores de tensão para menores IPS. Explorou-se também a hipótese pelos ensaios de ângulo de contato, observou-se novamente curva próxima a hipótese. Embora necessidade de mais ensaios, o presente trabalho contribuiu para metodologia de exploração de características de superfície, dispersão e reológicas de suspensões concentradas. / The proposition of the present work is to investigate the hypothesis that the reduction of the surface tension of the liquid favors the rheological behavior of concentrated suspensions, since the particles are closer and the contribution of capillarity forces possibly increases. As concentrated suspensions tend to viscoelastic behavior, rheological methods were examined to analyze possible consequences due to changes of surface tension of the water. Two equivalent calcium carbonates (P1 and P5) were used and differ by particle-size distribution. Two market dispersants and ethylene glycol were used as surfactant. Surface analysis by the zeta potential test revealed positive surface charge and, although the powders are equivalent, the electrophoretic mobility of P5 is lower. The reults show that calcium is potential determining ion. Electrostatic contribution was found only for the dispersants. Pendant drop test showed a decrease in the surface tension of the water with the three additives. Washburn capillary rise technique estimated greater contact angles for tests with additives and lower ones for P5. Rheological geometries and methods were evaluated in order to select good set for viscoelasticity measurements, choosing oscillatory stress sweep and vane geometry. The addition of the dispersants resulted in lower values G \'and yield stress, while ethylene glycol resulted in higher values. There is no clear relation between contact angle and electrophoretic mobility. The rheological and eletrophoretic mobility showed relation only for dispersants. The hypothesis was verified by the values yield stress and IPS. For the dispersants, it was possible to observe behavior close to the hypothesis, the lower the surface tension of the liquid, the lower the yield stress for lower IPS. The hypothesis was also explored by the contact angle tests, a curve next to the hypothesis was observed again. Although the need for more tests, the present work contributed to the methodology of exploration of surface characteristics, dispersion and rheological characteristics of concentrated suspensions.

Capillarity is often exploited in self-cleaning, drag reducing and fluid absorption/storage (sanitary products) purposes just to name a few. Formulating the underlying physics of capillarity helps future design and development of optimized structures. This work reports on developing computational models to quantify the capillary pressure and capillary forces on the fibrous surfaces. To this end, the current study utilizes a novel mass-spring-damper approach to incorporate the mechanical properties of the fibers in generating virtual fibrous structures that can best represent fibrous membranes. Such virtual fibrous structures are then subjected to a pressure estimation model, developed for the first time in this work, to estimate the liquid entry pressure (LEP) for a hydrophobic fibrous membrane. As for accurate prediction (and not just estimation) of the capillary pressure, this work also presents an energy minimization method, implemented in the Surface Evolver code, for tracking the air–water interface intrusion in a hydrophobic fibrous membrane comprised of orthogonally oriented fibers. This novel interface tracking algorithm is used to investigate the effects of the membrane’s microstructure and wetting properties on its resistance to water intrusion (i.e., LEP). The simulation method developed in this work is computationally affordable and it is accurate in its predictions of the air–water interface shape and position inside the membrane as a function of pressure. Application of the simulation method in studying effects of fiber diameter or contact angle heterogeneity on water intrusion pressure is reported for demonstration purposes. Capillary forces between fibrous surfaces are also studied experimentally and numerically via the liquid bridge between two parallel plates coated with electrospun fibers. In the experiment, a droplet was placed on one of the polystyrene- or polyurethane-coated plates and then compressed, stretched, or sheared using the other plate and the force was measured using a sensitive scale. In the simulation, the liquid bridge was mathematically defined for the Surface Evolver finite element code to predict its 3-D shape and resistance to normal and shearing forces, respectively, in presence of the contact angle hysteresis effect. Despite the inherent non-uniformity of the fibrous surfaces used in the experiments and the simplifying assumptions considered for the simulations, reasonable agreement was observed between the experiments and simulations. Results reveal that both normal and shear force on the plates increase by increasing the liquid volume, or decreasing the spacing between the plates.

This thesis highlights generic aspects of contact angle hysteresis and stick-slip motion,encountered in most practical wetting situations.First, we study the scaling relation between the heterogeneity strength and the amplitudeof the contact angle hysteresis it induces in the model configuration of a chemicallyheterogeneous microchannel. A key parameter which determines the qualitativefeatures is the heterogeneity wavelength. In particular, we identify a near-thresholdbehavior where the quadratic scaling between the heterogeneity amplitude and the resultinghysteresis, already known for a dilute system of wetting defects, is explainedby the closeness to the threshold, and a macroscopic limit without observable stick-slipwhere this scaling is linear.In the second part, we adapt the description to the configuration of a meniscusaround a wavy fibre. This adaptation brings the generic results of the first part in thereach of experiments. A comparison with experiments is achieved at the level of theindividual topography-induced jumps.In the third part, we expand the formulation to treat the quasi-steady interface shapecontact line dynamics and study how the the presence of stick-slip motion at the observableor unobservable scale modifies the scaling relation between the contact linevelocity and contact angle. We recover the known result that the scaling exponent dependson the nature of the externally controlled parameter, identify the causes of thisdependency in the corresponding static limits, and predict the disappearance of this dependencyabove a critical velocity which decreases with the heterogeneity wavelength.Finally, we show trough examples how the modelling framework which permitscapturing contact angle hysteresis and stick-slip motion in a minimalistic way can beadopted to treat configurations with a finite amount of contact points, or the 3D problemof a drop with a deformed contact line. We discuss the arising configuration-specificeffects, also in configurations of biomimetic interest. / Doctorat en Sciences de l'ingénieur et technologie / info:eu-repo/semantics/nonPublished

In several types of coating processes a solid substrate is removed at a controlled velocity U from a liquid bath. The shape of the liquid meniscus and the thickness of the coating layer depend on U. These dependencies have to be understood in detail for non-volatile liquids to control the deposition of such a liquid and to lay the basis for the control in more complicated cases (volatile pure liquid, solution with volatile solvent). We study the case of non-volatile liquids employing a precursor film model that describes partial wettability with a Derjaguin (or disjoining) pressure. In particular, we focus on the relation of the deposition of (i) an ultrathin precursor film at small velocities and (ii) a macroscopic film of thickness h ∝ U^(2/3) (corresponding to the classical Landau Levich film). Depending on the plate inclination, four regimes are found for the change from case (i) to (ii). The different regimes and the transitions between them are analysed employing numerical continuation of steady states and saddle-node bifurcations and simulations in time. We discuss the relation of our results to results obtained with a slip model. In connection with evaporative processes, we will study the pinning of a droplet due to a sharp corner. The approach employs an evolution equation for the height profile of an evaporating thin film (small contact angle droplet) on a substrate with a rounded edge, and enables one to predict the dependence of the apparent contact angle on the position of the contact line. The calculations confirm experimental observations, namely that there exists a dynamically produced critical angle for depinning that increases with the evaporation rate. This suggests that one may introduce a simple modification of the Gibbs criterion for pinning that accounts for the non-equilibrium effect of evaporation.

O fenômeno de molhamento, estudo de como um líquido se deposita em um sólido, apresenta problemas ainda em aberto, dos pontos de vista da modelagem física e da simulação numérica. O maior interesse acadêmico neste tipo de escoamento é a linha tríplice (ou linha de contato) formada da interação sólido-líquido-gás. A condição de contorno clássica de não escorregamento na interface líquido-sólido leva a uma singularidade no tensor de tensões nesta linha. Além disso, ainda não está estabelecido qual o melhor modelo para descrever o ângulo de contato formado entre a superfície livre e o substrato (o sólido). Neste trabalho, são discutidos métodos numéricos para a simulação de linhas de contato dinâmicas. Os efeitos da tensão superficial são estudados com a abordagem do princípio do trabalho virtual, o qual leva o problema à equações na formulação variacional, linguagem natural para o tratamento numérico com o método dos elementos finitos (FEM). O domínio é discretizado por uma malha não-estruturada de forma que as interfaces separadoras são explicitamente representadas pela malha. As derivadas temporais são tratadas em uma abordagem Lagrangeana-Euleriana arbitrária (ALE). Finalmente, são apresentados os resultados numéricos obtidos com o método ALE-FEM, discutindo alguns aspectos da sua convergência temporal e espacial. / Wetting phenomena, study of how of a liquid spreads out on a solid substrate, presents challenges both in physical modeling and in numerical simulation. The triple line (or contact line) formed by the solid-liquid-gas interaction has increasingly attracted the attention of the fluid dynamic community. The classical no-slip boundary condition on the liquid-solid interface leads to a singularity in the stress tensor at contact lines. Furthermore, there is no consensus on what the best model to describe the dynamics of the contact angle formed by the solid substrate and free surface. In this work, numerical methods for simulating dynamic contact lines are considered. The capillarity effects are studied in the approach of the virtual-work principle, which describes the problem in the variational formulation, natural language for numerical treatment with the finite element method (FEM). The domain is discretized by a dynamic unstructured mesh, where the separating interfaces are explicit represented by the mesh. Time derivatives present in the governing equations are treated with the arbitrary Lagrangian-Eulerian (ALE) framework. Finally, we discuss some temporal and spatial convergence issues ofthe ALE-FEM method.

Swedish hardwood is today used in the energy, pulp and mechanical hardwood industries. Only very small volumes of Swedish hardwood are, however, consumed by the mechanical industry that normally pays the highest timber price. The smallness of the volumes used for mechanical refinement is a result both of forestry not focusing on the production of hardwood for these uses, and of the fact that the mechanical hardwood industry, particularly the sawing industry, is not designed to process the existing raw material in an optimal manner. This thesis discusses the possibilities of improving the conditions for the mechanical refinement of hardwood. The aim of the work has been to investigate the possibilities of developing products and methods for processing of Swedish hardwood. The thesis proposes a new manufacturing system for Swedish hardwood to better utilize the inherent properties of the wood material. The system is based on the so-called PrimWood Method and the star-sawing concept. Compared to normally sawn wood, the sawing concept utilizes the raw material more efficiently with regard to volume yield, and increases the distance between knots in the sawn wood. The material produced has vertical annual rings which give the wood smaller movements as a result of moisture variations and a different textural appearance. Using the PrimWood Method for hardwood would make it possible to more closely match customer requirements regarding hardwood products. Since Swedish hardwood is nowadays mainly used indoors, a possible way of expanding the market would be to increase the outdoor use of the material. Here the durability is of great importance, and one important factor is then the capillary characteristics of the material. The thesis therefore focuses on the characterisation of the capillarity in wood for the future improvement of its durability. It is shown that with the material produced by the proposed manufacturing system, i.e. wood with vertical annual rings, the possibility of using hardwood outdoors increases, because the susceptibility to cracking decreases.

Parmi les différentes techniques permettant d'assembler à la fois mécaniquement et électriquement les puces empilées, le collage direct de surfaces mixtes Cu-SiO2 représente l'option la plus prometteuse à ce jour. En effet, cette méthode permet d'atteindre la densité d'interconnexions de 10^6/cm² visée par l'industrie, tout en offrant une faible résistivité de contact et une excellente fiabilité. Les méthodes d’assemblages actuelles reposent sur l’utilisation d’outils de Pick&place par l’intermédiaire desquels les puces sont positionnées mécaniquement. Cette technique rencontre néanmoins de plus en plus de difficultés à concilier précision d’alignement et cadence d’assemblage. Cette thèse propose d’adresser cette problématique au travers de la mise au point d’un procédé d’auto-assemblage assisté par capillarité et collage direct. Grâce à l’utilisation des forces de capillarités, il est possible de réaliser l’alignement des puces de façon spontanée : on parle alors d’auto-assemblage. La première partie de ce manuscrit présente une analyse synthétique des méthodes d’assemblages et d’interconnexions existantes et statue sur l’état de maturité de chaque procédé. Cette partie permet par la même occasion d’introduire les mécanismes de collages SiO2-SiO2 sur lesquels repose la méthode d’assemblage développée dans ce manuscrit. Un design de puce permettant la mise en œuvre du procédé d’auto-assemblage est ensuite établit dans la seconde partie. La capacité de la puce à confiner le film de liquide apparait comme l’élément moteur du processus d’auto-alignement. Des auto-assemblages présentant des valeurs d’alignement inférieur au micromètre sont ainsi obtenus, tout en conservant un procédé répétable. La mise en place de simulations numériques permettant de modéliser l’effet d’auto-alignement est présenté dans la troisième partie. Ce modèle a ensuite été généralisé a des puces de formes polygonales. Enfin la dernière partie présente le transfert du procédé d’auto-assemblage a des puces présentant des surfaces de cuivre et d’oxyde de silicium. L’utilisation de ce type de puce a notamment permis de valider la viabilité électrique du processus d’auto-assemblage. / Among the various techniques allowing to assemble both mechanically and electrically stacked chips, the direct bonding of Cu-SiO2 mixed surfaces is the most promising option to date. Thanks to this method, the interconnection density of 106/cm² aimed by the industry is achievable, while providing a low contact resistivity and excellent reliability.Current assemblies’ processes are based on Pick&place tools thanks to which the dies are mechanically placed.Nevertheless, these tools have difficulties to council high throughput and high alignment accuracy. This thesis proposes to address this issue through the development of a process of self-assembly assisted by capillary forces and direct bonding.Through the use of capillaries forces, it is possible to achieve spontaneously chips alignment: it is called self-assembly. The first part of this manuscript presents a synthetic analysis of the different assemblies and interconnections technics and decides on the maturity of each process.As the same time, this section allows to introduce the SiO2 -SiO2 bonding mechanisms underlying the assembly method developed in this manuscript.A specific chip design is then established in a second part allowing deploying self-assemblies with SiO2 full sheet chips.The ability of the chip to confine the liquid film appears as the driving element of the self- alignment process. Self- assemblies with alignment values lower than one micrometer are obtained while maintaining a repeatable process. The introduction of numerical simulations to model the self-alignment effect is presented in the third part. This model was then generalized has polygonal shaped chips. Finally the last part presents the transfer of the self- assembly process on SiO2-Cu patterned chips.The use of this kind of chip has enabled to validate the electrical viability of the self-assembly process.

Nowadays, the assembly of small (<1mm) components has become an industrial reality. Many domains like MEMS, surgery, telecommunications, car industry, etc. now have large use of micro-parts. At this scale, predominant forces are different than in macroworld. The pieces often undergo adhesion problems. The adhesion forces can be splitted in different components :van der Waals, electrostatics and capillary condensation. This work focuses on capillary condensation as it often can be the major component of the adhesion force. <p><p>The first part of this work details a review of literature of different fields involved in capillary condensation. A simulation tool is then implemented and theoretically validated in the second part of the work. Finally, a test bed is presented; this bed is then used to experimentally validate the simulation results.<p><p>Experiments and simulation results are shown to concord. Therefore, the simulation tool can be used to model the force due to capillary condensation. / Doctorat en Sciences de l'ingénieur / info:eu-repo/semantics/nonPublished

Les effets capillaires sont très courant dans la Nature. Dans le contexte du séchage de milieux poreux dont la taille de pore est dans la gamme micromètre-millimètre, ils jouent un effet dominant en contrôlant la répartition des phases (liquide-vapeur) dans l’espace poral, au fur et a` mesure que le séchage se produit. L’idée du présent travail est d’étudier le séchage d’un fluide pur et mouillant dans des micromodèles, c’est-à-dire des milieux poreux modèles quasi-2D et micro-fabriqués. Nous présentons des résultats obtenus pour différentes géométries. Typiquement, les micromodèles utilisés sont constitués de réseaux de cylindres pris en sandwich entre deux plaques. La distribution des phases et le taux d’évaporation dans de tels micromodèles peuvent être aisément mesurés par visualisation directe puis traitement d’images.En jouant sur l’arrangement spatial des cylindres, on obtient dans un premier temps des micromodèles pour lesquels le taux de séchage est quasi-constant, depuis le début de l’expérience de séchage jusqu’à l’évaporation totale du liquide saturant initialement le système. Typiquement, cette situation est obtenue quand la taille des pores décroît en allant du centre du micromodèle vers sa périphérie (les micromodèles sont axisymmétriques). Au contraire, quand la taille des pores croît du centre vers la périphérie, l’invasion d’un front de séchage stable est observée, d’ou` un temps de séchage total bien supérieur.Nous avons aussi réalisé un autre type de microsystèmes, au sein duquel les cylindres sont arrangés en spirale de Fibonacci, en nous inspirant de motifs observés en phillotaxie. Dans de tels systèmes, des films liquides épais se développent le long des spirales, au cours du séchage, et jouent un rôle crucial dans la cinétique d’évaporation. Cette situation rappelle celle déjà étudiée par Chauvet dans des tubes capillaires de section carrée. Cependant, elle est plus complexe, de par la nature poreuse du micromodèle (alors qu’un tube capillaire, tel qu’étudié par Chauvet, peut être vu comme un pore unique) et parce que les films liquides y ont une forme plus complexe. Pour de tels systèmes, nous présentons des résultats expérimentaux quantifiant l’effet des films liquides sur la cinétique de séchage, en lien avec des prédictions théoriques issues d’un modèle de séchage visco-capillaire. Un tel modèle nécessite l’utilisation du logiciel Surface Evolver pour modéliser la forme des films liquides, couplée avec des simulations directes de l’écoulement de Stokes dans les films liquides, pour y calculer la résistance visqueuse a` l’écoulement induit par l’évaporation.Enfin, dans un dernier chapitre, plusieurs expériences d’évaporation sont conduites sur des micromodèles déformables. Des effets élasto-capillaires peuvent en effet induire des changements de géométrie de l’espace poral en cours d’évaporation, ce qui, comme vu précédemment, peut affecter la distribution des phases et la cinétique de séchage. / Capillarity is a common phenomenon encountered in Nature. In the context of the drying of porous media with pore size in the micrometer-millimeter size range, capillary effects play a dominant role in controlling the phases (liquid or vapor) distribution in the pore space as drying occurs. The basic idea of the present work is to study the drying of pure, wetting fluids in micro-fabricated, quasi-2D, model porous media (hereafter called micromodels). We present results obtained for different micromodel geometries. Typically, the micromodels used consist of arrangements of cylinders sandwiched between a top and bottom plate. Phases distribution and evaporation rates in such micromodels can easily be measured by direct visualizations and subsequent image processing.By tuning the cylinders pattern, one can first obtain micromodels for which the drying rate is almost constant, from the beginning of the drying experiment to the total evaporation of the liquid initially filling the system. Typically, this situation is obtained when the pores size decreases from the micromodel center to the periphery (the micromodels are axisymmetric). On the contrary, when the pores size increases from the center to the periphery, invasion of a stable drying front is observed, resulting in a much longer total drying time.We also designed another type of micromodel where the cylinders are arranged in a Fibonacci spiral pattern, a design inspired by phyllotaxic structure. In such systems, thick liquid films develop along the spirals during drying and play a key role in the drying kinetics. This situation is reminiscent of that already studied by Chauvet in capillary tubes with square cross-sections. However, it is more complex because of the porous nature of the micromodel (whereas a single capillary tube, as studied by Chauvet, can be viewed as a unique pore), and because of the much more complex liquid films shapes. For such systems, we present some experimental results on the liquid films effects on the drying kinetics, together with theoretical prediction, based on a visco-capillary drying model. Such a modelling requires the use of the Surface Evolver software to model the film shape, coupled with DNS simulations of the Stokes flow within the liquid films to compute the viscous resistance to the evaporation-induced flow.Finally, as a last part of this thesis, several evaporation experiments performed on deformable micromodels are presented. This preliminary work aims at reaching a situation where elasto-capillary effects modify the pore space geometry during evaporation. This, as seen above, should in turn alter the phase distribution during evaporation and the drying kinetics.