Les émulsions fluorées de Pickering sont étudiées et mises au point dans la technologie demicrofluidique en gouttes pour des applications d’études sur des cellules adhérentes isolées.Les principaux résultats de ce projet sont : l’établissement d’un lien entre la couverture desurface des nanoparticules et la fluidité de l’émulsion de Pickering ; l’établissement deslignes directrices pour la stabilisation des gouttes avec un débit de production élevé et unminimum de déchets de particules ; et la mise en oeuvre d’une plateforme technologiquecomplète pour l’étude des cellules RPE, pour mesurer leur hétérogénéité phénotypique auniveau de la cellule individuelle. / Fluorinated Pickering emulsions are studied and engineered within droplet-based microfluidicstechnology for adherent-cell studies applications. The main findings of this projectinclude: linking the nanoparticles surface coverage to the bulk flowability of the Pickeringemulsion; deriving guidelines for droplet stabilization with high production throughput andminimal particle waste; and implementing the full technological platform for the study ofRPE cells, while unraveling their phenotypic heterogeneity at the single cell level.

A preparação de partículas pela técnica de granulação por solidificação de material fundido em leito fluidizado tem se destacado no âmbito da indústria farmacêutica. As vantagens do uso deste método têm atraído muitos pesquisadores para aprimorar e colocar em prática tal técnica de preparo. A principal vantagem deste processo é dispensar o uso de solventes e diminuir o tempo de preparo dos granulados para compressão. O objetivo do presente trabalho foi o desenvolvimento e estudo desta técnica de granulação, usando a lactose tipo spray-dried como substrato e como agente aglutinante uma dispersão do polímero polietilenoglicol 4000 contendo indometacina como fármaco modelo. Outra motivação para este trabalho foi realizar a caracterização físico-química dos granulados obtidos e avaliar um possível aumento da solubilidade deste fármaco de classe II. Resultados obtidos durante estudos preliminares mostram que a solubilidade da indometacina foi consideravelmente aumentada com o uso do PEG e análises físico-química indicaram que não há interação entre a indometacina e o PEG. O método utilizado na granulação consistiu na atomização da dispersão liquefeita de PEG 4000 contendo 25% de indometacina sobre o substrato a fim de obter grânulos contendo estes três componentes. Um estudo prévio da fluidodinâmica da lactose provou ser predominante o regime de leito fluidizado. Para viabilizar a obtenção destas dispersões sólidas, foram estudadas as variáveis do processo como vazão da dispersão carreador/fármaco, vazão do ar de atomização e quantidade total de dispersão adicionada, aplicando para tal um planejamento fatorial tipo Box-Behnken. O leito fluidizado se mostrou eficiente para a granulação e os granulados obtidos foram considerados de boa qualidade baseando-se na sua caracterização por densidades aparente e compactada, fluidez, distribuição granulométrica, doseamento do fármaco e perfil de dissolução in-vitro. Granulados de dois tamanhos médios diferentes e com ótima fluidez foram escolhidos para as análises seguintes. A integridade e ausência de interação do fármaco com os demais componentes destes granulados foram comprovadas por calorimetria exploratória diferencial, difração de raios-X, infravermelho, microscopia de plataforma quente e microscopia de varredura eletrônica. As micrografias mostraram visivelmente que as formas dos cristais de indometacina presentes no granulado apresentaram as características da forma y (II), que é a mesma da indometacina padrão. A dissolução de cápsulas gelatinosas duras contendo os lotes de grânulos escolhidos mostraram que no meio tampão fosfato (pH 7,2) foi liberado até 99% da indometacina. Porém, em meio HCl 0,1N; obteve-se liberação de até 28% da indometacina, o que corresponde a um aumento de 14,5 vezes a liberação obtida com a indometacina padrão. / Recently, there is a renewed interest in the fluidized bed hot melt granulation for the preparation of solid dosage forms in the pharmaceutical industry and academy. The several advantages of this technique have attracted may researchers, but the main advantage are undoubtedly the solvent free operation and the short processing times. The aim of this work was to develop and study this granulation technique using spray-dried lactose as substrate and a dispersion of indomethacin in hot melted polyethylene glycol 4000 and as the binder. Another goal in this work was to characterize the granules obtained and to evaluate any increase in indomethacin solubility in the solid dispersions. The results of preliminary evaluation of indomethacin/polyethylene glycol physical mixtures and solid dispersions showed a considerable increase in the drug solubility, while no chemical or physical interaction with the carrier could be observed. Before the granulation experiments the fluid dynamic behavior of the lactose was characterized as fluidization regime. The method of granulation consisted in the atomization of hot melted polyethylene glycol containing 25% of indomethacin onto the fluidized bed of lactose. In order to study the granulation process, a Box-Behnken design was applied to verify the effects of spray air flow rate, drug/carrier feed rate and total amount of drug/carrier added to granules. The fluidized bed showed to be an effective method for hot melt granulation and the granules quality can be considered adequate, based on their characteristics of apparent and compacted densities, flowability, particle size distribution, indomethacin content and in-vitro dissolution profile. From the whole set of experiments, two granule batches were chosen based on their mean particle sizes and excellent flow indexes, to verify any drug/PEG/lactose interaction during the granulation process. The non existence of interaction was proved by differential scanning calorimetry, X-ray powder diffraction, Fourier transform Infra-red, hot stage microscopy and scanning electron microscopy. The scanning electron microscopy showed that indomethacin crystals with the characteristic shape of the form y (II) could be observed in the granules, indicating that its crystalline form did not change during processing. The dissolution profiles of indomethacin from hard gelatin capsules containing the granules showed the release of 99% of the drug in phosphate buffer media (pH 7.2). However, in acidic media (HCl 0,1N) 28% of the total indomethacin was released, which corresponded to a 14.5 fold increase when compared to the pure indomethacin release under the same conditions.

The increasing volume of waste of all kinds is currently a phenomenon of economically developed society and one of the problems of environmental protection. It is therefore imperative, in the interest of sustainable development, to monitor impacts related to the impact on our ecology, to regulate waste production by legislation and universally promote their reuse and recycling. Construction and demolition waste occupy a significant share of the total waste volume. This category also includes excavated soils. Recycling of these materials could significantly reduce the amount of landfilled waste and at the same time, these materials could be used as an important source of secondary raw materials. The doctoral thesis describes the research and development of the new technology of reuse soils in the form of self-compacting grouts. The result of the solution will be a suspension of optimal rheological properties, providing a perfect leaking around the stored utility networks. Emphasis will be placed on the study of the interaction of different types of soils with the stabilizers, flowable or plasticizing additives and its typical dispersible substance, including verification of the developed technology in situ.

Concrete, the second most used material in the world, presents great performance and economic benefits. Yet, it is often characterized by a brittle behaviour, low tensile strength, and toughness. Fibers are usually added to concrete to counteract its brittle behaviour, increasing ductility and toughness, controlling crack propagation and delaying concrete failure. However, their addition significantly worsens the fresh state performance of the material. To improve fresh state of the so-called Fiber Reinforced Concrete (FRC), conventional mix-design methods recommend the use of high paste content, which results in a significant increase of Portland cement (PC) content and raises the carbon footprint of the material. The latter is responsible for 8% of the global annual carbon dioxide (CO2) anthropogenic emissions. Given the current worldwide concerns on global warming, the construction industry is in a need to lessen the demand, and thus production of PC. Recent studies have been focusing on the use of advanced mix-design techniques (i.e. particle packing models- PPMs) along with Inert Fillers (IF) as an alternative to reduce PC content in concrete. However, the latter was not applied to conventional FRC. In this work, advanced mix design techniques (i.e. PPMs) are used to overcome the aforementioned issues and mix-proportion eco-efficient FRC with low cement content (< 300 kg/m3). Fresh (i.e. VeBe time, slump, rheological behaviour) and hardened (i.e. compressive strength, and flexural behaviour) state tests were performed on the proposed mixtures and compared with control high PC content (375 kg/m3) FRC mixes. Results show that PPM designed mixes presented higher minimum torque (yield stress) but quite comparable apparent viscositiy when compared to conventionally designed mixtures. Moreover, the flowability (i.e. VeBe time, and slump) tends to decrease as fiber content, length, and/or as the amount of fillers increase in the mixtures. In addition, PPM mixes exhibited a shear thinning behaviour following the Herschel-Bulkley model, which enables the design of FRC PPM mix-proportioned mixtures for applications requiring high torque regimes such as vibrated and/or pumped concrete. Finally, results show that the use of PPMs to mix proportion eco-efficient low cement FRC mixtures produced improved hardened (i.e. compressive strength, and flexural performance) state behaviour with lower environmental impact than conventional ACI designed FRC mixtures.

Une technologie prometteuse pour répondre à la demande croissante en énergie renouvelable est la gazéification de biomasse lignocellulosique pour la production de biocarburants de deuxième génération. Ce procédé nécessite une alimentation en biomasse sous forme de poudre. Les problèmes de convoyage et de manipulation liés à la faible coulabilité de la biomasse broyée sont un verrou pour l’industrialisation des procédés BtL. La torréfaction comme procédé de prétraitement, en plus d'augmenter densité énergétique de la biomasse, peut influencer également les propriétés des particules obtenues après broyage, et en conséquence, l’écoulement des poudres. L'évaluation de l'écoulement des poudres de biomasse sous différentes conditions de consolidation est essentielle pour concevoir des technologies de manipulation et de convoyage efficaces.L'objectif de ce travail est d'évaluer l'effet des conditions de torréfaction et de broyage sur l’écoulement de poudres de biomasse. Une première partie consiste en une étude expérimentale dans laquelle la coulabilité d'échantillons torréfiés sous différentes intensités a été évaluée à l'aide d'un appareil de cisaillement annulaire. La coulabilité est corrélée à l'intensité de la torréfaction (mesurée par la perte de masse globale) pour deux essences différentes. La forme des particules semble être le paramètre qui influence de manière prédominante la coulabilité des poudres à l'état consolidé. La caractérisation de la coulabilité à l’état non consolidée a été effectuée à l'aide d'un tambour rotatif par l’analyse des avalanches des poudres. Des corrélations entre les caractéristiques des particules et la coulabilité sont ainsi établies. La modélisation de l'écoulement de la biomasse à l'aide de la Méthode des Éléments Discrets (DEM) constitue une deuxième partie de cette recherche. La taille submillimétrique des particules de biomasse, ainsi que leur faible densité, leur forme allongée et leur comportement cohésif sont des défis pour l’implémentation d’un modèle de réaliste d’écoulement particulaire en DEM. Un modèle DEM des particules de biomasse est mis en œuvre à l'aide d'une représentation simplifiée (assemblement de sphères) à gros grains de la forme des particules, ainsi que d'un modèle de force cohésif. Une procédure systématique de calibration des paramètres DEM permet d'obtenir un ensemble de paramètres ajustés. L'évolution expérimentale des contraintes de cisaillement d’une poudre dans un état consolidé peut alors être reproduite de façon réaliste. De même, le comportement d’avalanche des poudres dans un tambour tournant est également bien reproduit par les simulations, de façon qualitative et quantitative. Ces résultats mettent en évidence le potentiel des simulations DEM pour étudier l'effet des caractéristiques des particules, qui sont influencées par la torréfaction et les conditions de broyage, sur le comportement d'écoulement de la biomasse en poudre. / Gasification of lignocellulosic biomass for production of second-generation biofuels is a promising technology to meet renewable energy needs. However, feeding and handling problems related to the poor flowability of milled biomass considerably hinder the industrial implementation of Biomass-to-Liquid processes. Torrefaction as pretreatment step, in addition to improving energy density of biomass, also affects the properties of the milled particles (namely size and shape) that significantly influence flow behavior. The evaluation of biomass flow characteristics under different flow conditions is essential to design efficient and trouble-free handling solutions.The aim of this work is to assess the effect of the torrefaction and grinding conditions on the biomass flow behavior. A first part consists of an experimental study in which the flow properties of samples torrefied under different intensities were obtained using a ring shear tester. Flowability is correlated to the intensity of torrefaction, as measured by the global mass loss, for two different wood species. Particle shape seems to be the predominant parameter influencing flowability of powders in a consolidated state. Characterization of non-consolidated flowability through avalanching analysis using an in-house rotating drum was also conducted. Correlations between particle characteristics and flow behavior are thus established.The modelling of biomass flow using the Discrete Element Method (DEM) constitutes a second major part of this research. Challenging aspects of biomass particle modeling are their submillimetric size, low density, elongated shape and cohesive behavior. A material DEM model is implemented using a simplified (multisphere) upscaled representation of particle shape, along with a cohesive contact model. A systematic calibration procedure results in an optimal set of DEM parameters. The experimental shear stress evolution and yield locus can then be realistically reproduced. The avalanching behavior of the powders is also well captured by simulations, both qualitatively and quantitatively. These results highlight the potential of DEM simulations to investigate the effect of particle characteristics, which are driven by torrefaction and grinding conditions, on the flow behavior of powdered biomass.

The application of chemical additives, known as grinding aids (GA), dates back to 1930 in the cement industry. As opposed to the cement industry, where the use of GAs is on the final processing step, it could be one of the first process steps in ore beneficiation. A few investigations addressed the GA applications in ore dressing; therefore, further studies are required to better understand the GA effects on the product properties and downstream separation processes. This thesis undertakes a comparative study on the dry grinding of magnetite and the resulting product characteristics with and without GAs. The main aim is to reduce energy consumption and to address some of the challenges associated with dry processing.  The effects of GAs on the dry batch ball milling of magnetite were examined to analyze the energy consumption (Ec), particle size distribution, flow properties, bulk properties, surface morphology, particle fineness, and surface chemistry of products. Their effects on the ground product were systematically explored by sieve analysis, powder rheology, BET surface measurements, optical microscopy analysis, and zeta potential measurements. Compared with the absence of GAs, the dry grinding efficiency of magnetite increased after using GAs; however, an optimal dosage exists based on the GA type. Among GAs which considered in this investigation (Zalta™ GR20-587 (Commercial GA) and Zalta™ VM1122 (Commercial viscosity aid) as well as sodium hydroxide), Zalta™ VM1122, a polysaccharide-based additive, was the most effective GA where by using this GA; the Ec decreased by 31.1% from 18.0 to 12.4 kWh/t. The PSD became narrower and finer (P80 decreasing from 181 to 142 µm), and the proportion of the particles (38–150 µm) increased from 52.5 to 58.3%. In general, the results reveal that at sufficient GA dosages, they reduce the average particle size, increase the specific surface area, and narrow the particle size distribution. However, an excessive amount of GAs could be detrimental to the grinding performance.  Further studies on powder rheology indicated that the used GAs resulted in improved material flowability compared to grinding without additives (in the examined dosage range). The rheology measurements by the FT4 Powder Rheometer showed strong linear correlations between basic flow energy, specific energy, and the resulting work index when GAs was considered for grinding. There was a strong correlation between the grinding parameters and flow parameters (r &gt; 0.93). These results confirmed the effect of GA on ground particles' flowability. Zalta™ VM1122 showed the best performance with 38.8% reduction of basic flow energy, 20.4 % reduction of specific energy, 24.6% reduction of aerated basic flow energy, and 38.3% reduction of aerated energy. The present investigation showed that the predominant mechanism of GAs is based on the alteration of rheological properties. Further investigation on the surface properties showed that using GAs could increase the surface roughness, which is beneficial for downstream processes such as froth flotation. Zalta™ VM1122 resulted in increased surface roughness and minimum microstructural defects from the optical microscope images. Furthermore, Zalta™ VM1122 (non-ionic) resulted in similar zeta potentials and pH values for the product compared to experiments without GA. These comparable product properties are advantageous as they minimize any potential negative effects on all possible downstream processes. / Kolarctic CBC (KO1030 SEESIMA)

Dans cette étude, l’intérêt est porté sur l’effet des conditions opératoires sur l’enrobage en voie sèche de grosses particules « hôtes » par de fines particules « invitées » et aussi sur la modélisation de cet enrobage selon la méthode par éléments discrets (DEM) afin de mieux comprendre les phénomènes mis en jeu. Dans ce travail, les matériaux choisis comme particules hôtes sont les Suglets® et les particules invitées sont en stéarate de magnésium (StMg). Ces deux éléments sont introduits dans un mélangeur à fort taux de cisaillement, le Cyclomix. Les propriétés du produit final, comme la coulabilité, la mouillabilité et le degré d’avancement de l’enrobage, ont été caractérisés. La variation des propriétés est étudiée en fonction de la durée de traitement dans le Cyclomix pour diverses vitesses de rotation, taux de remplissage et rapport de taille de particules hôte et invitée. La coulabilité a été améliorée avec la durée du mélange ou la vitesse de rotationLe degré d’avancement présente une tendance semblable pour différentes conditions opératoires. Sa variation est représentée par une loi exponentielle empirique en fonction du temps de mélange, paramétrée par une constante ajustable. Cette constante permet d’estimer l’efficacité de l’enrobage. La simulation des mouvements de particules dans le mélangeur par DEM a permis d’obtenir des informations sur la position, la vitesse des particules, et d’autres paramètres énergétiques. Les champs de vitesse réelle ou numérique liés aux mouvements de particules, analysés par PIV (Particule Image Velocimetry), sont analogues. La constante d’enrobage dépend de la vitesse de rotation simulée et peut être ainsi prédite par DEM. / Investigations of the effect of the operating conditions on the dry coating and the motion of particles in a high shear mixer by the DEM simulation have been done. Big Suglets® and small Magnesium Stearate materials have been chosen for the dry coating process. The treatment has been carried out in a Cyclomix, a high shear mixer, at different mixing time, rotational speeds, filling ratio of the samples and particle size ratio to observe the effect of the operating conditions on the dry coating. A conversion ratio has been introduced to quantify the degree of coating and measured. The flowability has been improved when increasing the operation time in the mixer. Higher speeds of rotation can improve the flowability more rapidly. However, the flowability doesn’t seem to be sensitive to the filling ratio. The curves of conversion ratio versus time exhibit the same kind of variations for different operating conditions. It is possible to approximate this tendency by an exponential function in which a characteristic parameter “coating rate constant” is introduced, linked to the efficiency of the dry coating process, since the conversion ratio shows a linear relation with a flowability index and the wettability angle. Simulation of the particle motion in the mixer has been carried out by a Discrete Element Method: different parameters characterizing the location, the velocities, and the attachment of the particles have been derived. The velocity fields of the real and simulated particle motions, compared by Particle Image Velocity (PIV), are quite similar, validating the DEM method and allowing the prediction of the coating process.

Abstract : Recently, there is a great interest to study the flow characteristics of suspensions in different environmental and industrial applications, such as snow avalanches, debris flows, hydrotransport systems, and material casting processes. Regarding rheological aspects, the majority of these suspensions, such as fresh concrete, behave mostly as non-Newtonian fluids. Concrete is the most widely used construction material in the world. Due to the limitations that exist in terms of workability and formwork filling abilities of normal concrete, a new class of concrete that is able to flow under its own weight, especially through narrow gaps in the congested areas of the formwork was developed. Accordingly, self-consolidating concrete (SCC) is a novel construction material that is gaining market acceptance in various applications. Higher fluidity characteristics of SCC enable it to be used in a number of special applications, such as densely reinforced sections. However, higher flowability of SCC makes it more sensitive to segregation of coarse particles during flow (i.e., dynamic segregation) and thereafter at rest (i.e., static segregation). Dynamic segregation can increase when SCC flows over a long distance or in the presence of obstacles. Therefore, there is always a need to establish a trade-off between the flowability, passing ability, and stability properties of SCC suspensions. This should be taken into consideration to design the casting process and the mixture proportioning of SCC. This is called “workability design” of SCC. An efficient and non-expensive workability design approach consists of the prediction and optimization of the workability of the concrete mixtures for the selected construction processes, such as transportation, pumping, casting, compaction, and finishing. Indeed, the mixture proportioning of SCC should ensure the construction quality demands, such as demanded levels of flowability, passing ability, filling ability, and stability (dynamic and static). This is necessary to develop some theoretical tools to assess under what conditions the construction quality demands are satisfied. Accordingly, this thesis is dedicated to carry out analytical and numerical simulations to predict flow performance of SCC under different casting processes, such as pumping and tremie applications, or casting using buckets. The L-Box and T-Box set-ups can evaluate flow performance properties of SCC (e.g., flowability, passing ability, filling ability, shear-induced and gravitational dynamic segregation) in casting process of wall and beam elements. The specific objective of the study consists of relating numerical results of flow simulation of SCC in L-Box and T-Box test set-ups, reported in this thesis, to the flow performance properties of SCC during casting. Accordingly, the SCC is modeled as a heterogeneous material. Furthermore, an analytical model is proposed to predict flow performance of SCC in L-Box set-up using the Dam Break Theory. On the other hand, results of the numerical simulation of SCC casting in a reinforced beam are verified by experimental free surface profiles. The results of numerical simulations of SCC casting (modeled as a single homogeneous fluid), are used to determine the critical zones corresponding to the higher risks of segregation and blocking. The effects of rheological parameters, density, particle contents, distribution of reinforcing bars, and particle-bar interactions on flow performance of SCC are evaluated using CFD simulations of SCC flow in L-Box and T-box test set-ups (modeled as a heterogeneous material). Two new approaches are proposed to classify the SCC mixtures based on filling ability and performability properties, as a contribution of flowability, passing ability, and dynamic stability of SCC. / Résumé : Récemment, il y a un grand intérêt à étudier les caractéristiques d'écoulement des suspensions dans différentes applications environnementales et industrielles, telles que les avalanches des neiges, les coulées de débris, les systèmes de transport et les processus d’écoulement des matériaux. En ce qui concerne les aspects rhéologiques, la plupart des suspensions, comme le béton frais, se comportent comme un fluide non-Newtonien. Le béton est le matériau de construction le plus largement utilisé dans le monde. En raison de limites qui caractérisent le béton normal en termes de maniabilité et de capacité de remplissage de coffrage, il était nécessaire de développer une nouvelle classe de béton qui peut couler sous son propre poids, en particulier à travers les zones congestionnées du coffrage. Par conséquent, le béton autoplaçant (BAP) est un nouveau matériau de construction qui est de plus en plus utilisé dans les différentes applications. Étant donné sa fluidité élevée de BAP peut être utilisé dans certaines applications particulières, notamment dans la section densément renforcée. Cependant, la fluidité élevée rend le béton plus sensible à la ségrégation des gros granulats pendant l'écoulement (la ségrégation dynamique) et ensuite au repos (ségrégation statique). La ségrégation dynamique peut augmenter lorsque le BAP est coulé sur une longue distance ou en présence d'obstacles. Par conséquent, il est toujours nécessaire d'établir un compromis entre la fluidité, la capacité de passage, et la stabilité du BAP. Ceci doit être pris en considération afin de concevoir le processus de coulée et dosage des mélanges du BAP. Ceci est appelé la conception d'ouvrabilité du BAP. Une conception de maniabilité efficace et non coûteuse peut être achevée à travers la e prévision et l'optimisation de l'ouvrabilité des mélanges de béton pour les procédés de construction sélectionnés, notamment le transport, le pompage, la mise en place, le compactage, la finition, etc. En effet, les formulations de mélange doivent se confirmer à la qualité de la construction demandée, par exemple les niveaux exigés de fluidité, la capacité de passage, la capacité de remplissage, et la stabilité (statique et dynamique). Celui est nécessaire pour développer des outils théoriques afin d’évaluer dans quelles conditions les exigences de qualité de la construction sont satisfaites. Cette thèse est consacrée à la réaliser des simulations analytiques et numériques pour prédire la performance d'écoulement du BAP dans différents procédés de la mise en place du béton. L'objectif spécifique de cette étude consiste à simuler l'écoulement du BAP dans essais empiriques, notamment la boite en L et la boite en T pour évaluer la performance du BAP pendent la mise en place (la fluidité, la capacité de passage, la capacité de remplissage, et la ségrégation dynamique induite par cisaillement ou par gravité). Par conséquent, le BAP est modélisé comme matériau hétérogène. En outre, un modèle analytique est proposé pour prédire la performance à l'écoulement du BAP dans la boite en L en utilisant la théorie de Dam Break. D'autre part, les résultats des simulations numériques de l’écoulement du BAP dans une poutre renforcée sont comparés aux résultats expérimentaux par des profils de surface libres. Les résultats des simulations numériques de BAP coulée (modélisée comme un fluide homogène unique), sont utilisés pour déterminer les zones critiques correspondant à des risques plus élevés de ségrégation et de blocage. Les effets des paramètres rhéologiques, la masse volumique, le contenu des particules, la distribution de barres d'armature, et les interactions particule-barres sur les performances d'écoulement du BAP sont évaluées à l'aide de simulations MFN d’écoulement du BAP par les essais des L-Box et T-box (modélisée comme une matériau hétérogène). Deux nouvelles approches sont proposées pour classifier les mélanges du BAP sur la base de la capacité de remplissage, et les propriétés de performabilité, en fonction de la fluidité, la capacité de passage et de la stabilité dynamique du BAP.

L’enrobage à sec par action mécanique permet de formuler des particules composites dont les fonctionnalités et les propriétés physiques, comme l’écoulement, sont améliorées et cela sans l’ajout de solvant ou de liant. Actuellement la plupart des procédés d’enrobage à sec sont conduits en mode discontinu. L’objectif de ce travail est donc de développer et d’étudier une opération d’enrobage à sec par un procédé continu innovant, une extrudeuse bi-vis corotative sans filière, constituant une rupture technologique dans son domaine. Dans le cadre de ce travail, des sphères de cellulose microcristalline, appelées particules hôtes sont enrobées avec soit des talcs de différentes granulométries soit du stéarate de magnésium, nommées particules invitées. Dans un premier temps, le comportement des particules hôtes est étudié dans le procédé. Les particules sorties du procédé sont analysées par microscopie électronique à balayage, par granulométrie laser et par voluménométrie. Pour la configuration de vis présentant que des éléments de transport, la vitesse de rotation des vis (25 à 200 rpm) et le débit d’alimentation (0,5 à 2 kg/h) choisis influencent le taux de remplissage dans le fourreau, et pour un taux supérieur à environ 14 % : la quantité de particules endommagées est négligeable. Un taux de remplissage faible favorise les frictions particules-particules ou particules-métal au niveau de l’entrefer. L’ajout de zones de mélanges dans la configuration des vis accentue ce phénomène de brisure par l’augmentation des contraintes de cisaillement. Par ailleurs, des masses retenues de la poudre dans le fourreau évoluent linéairement en fonction de la masse de poudre transportée en un tour de vis pour différentes configurations de vis. Ces relations laissent penser à l’existence d’un volume mort. Les mesures de distribution de temps de séjour mettent en évidence par l’application d’un modèle d’association de réacteurs idéaux, la présence d’écoulement piston et d’un volume mort. Dans un second temps, la faisabilité d’une opération d’enrobage à sec par le procédé étudié est analysée. Une couche d’enrobage continu de talc modifiant le comportement hydrophile des particules hôtes, est obtenue pour une vitesse de rotation de vis de 50 rpm et une configuration de vis cisaillante. Le type de particules invitées influence la morphologie de la couche d’enrobage : de type film avec le stéarate de magnésium et de type discret avec le talc micronisé. Néanmoins les propriétés de taille, d’écoulement, de compressibilité des particules composites sont semblables à celle des particules hôtes, seule la propriété de mouillabilité est modifiée. La présence de stéarate de magnésium diminue le temps de séjour des particules dans le procédé grâce à son caractère lubrifiant. / Dry particle coating with mechanical action allows the production of composite particles whose functionalities and physical properties, such as flowability, are improved thanks to the absence of solvent or binder. Currently, most of dry particle coating processes are carried out in a discontinous mode. The objective of this work is thus to develop and study a dry particle coating operation with a continuous innovative process, twin screw co-rotating extruder without die, constituting a technological rupture in this application field. For this, spherical particles of microcristalline cellulose, as host particles, are coated with either talc particles of two sizes or magnesium stearate particles (MgSt), as guest particles. Firstly, the host particles behaviour is studied in the process. The exiting particles are analyzed by scanning electronic microscopy, laser granulometry and tapping test. Regarding the transport configuration, the chosen screw speed (between 25 an 200 rpm) and the feed rate (between 0.5 and 2 kg/h) have an important influence on the filling level in the barrel. For a filling level superior to approximatly 14 %, the quantity of broken particles is not significant. A low filling level facilitates the particle-particle or particle-metal friction in the barrel gap. When more mixing zones are added to the screw configuration, the shear stresses increase and, therefore, the breakage particle phenomenon becomes more prominent. Futhermore, the retained powder mass increases linearly when the transported mass in one screw turn increases for all the screw configurations. These evolutions suggest the existence of a dead volume. The residence time distribution mesurements highlight, thanks to the application of flowing model, the presence of plug-flow and a dead volume. Secondly, the feasibility of using the process for dry particle coating is analyzed. A continuous coating layer of talc modifiying the hydrophilic behaviour of the host particles is obtained for a low screw rotation speed (50 rpm) and a screw configuration with one mixing zone. The type of guest particles influence the morphology of the coating layer: film layer with the MgSt particles and discontinous layer with the micronized talc. However, size, flow and compressibility of the coated particles are similar to the ones of the initial host particles, only the wettability properties are modified. The presence of MgSt decreases the particle mean residence time in the process thanks to its lubricant action.

During the pressing of powder mixtures to make cemented carbide tools, the degree to which the powder spreads to fill the die and to which it compacts is uncertain. This leads to inconsistent dimensions and densities in the finished product. This performance changes with the composition of the powder, including the amount of pressing agent in the mixture, the particle size distribution and particle shape. One way to quantify the degree to which powder will spread to fill the mold evenly is using the property called 'flowability'. There are several techniques by which flowability can be measured, and each technique does not always give results that are consistent with other techniques. It is, therefore, important to know what technique(s) predict(s) the final behavior of the powder in this application before it is used in quality assurance or to design a process. Additionally, powder size distribution and shape metrics are measured using dynamic image analysis to investigate if there is any relationship between key values of these properties and compaction behavior. In this study, static Angle of repose, Tap Density, Hall flow time and Powder rheometry were benchmarked against each other and against the dimensions of presses and liquid phase sintered tool inserts to understand which technique had the strongest dependence on the compactability, which was defined as the ratio of the tallest dimension in the insert to the smallest. After the study, the results showed that a more extensive particle size distribution improves the compaction properties and that the powders with a higher resistance to a rotating blade tend to have better compaction properties. On the other hand, a clear pattern for the results of all measurement methods and the correlation between the compaction behavior of the carbide tools could not be discerned. In conclusion, the study showed that it is possible to determine a relationship between the results of measurement methods and the compaction behavior of powders. By using simple tests to predict the compactability properties, both money and time can be saved on the research of new, improved powder. Furthermore, the implementation of this study can lead to even better pressing and compactibility properties in the future for cemented carbide tools. / Vid pressning av pulverblandningar för tillverkning av hårdmetallverktyg är det osäkert i vilken grad pulvret sprider sig för att fylla matrisen och i vilken grad det komprimeras. Detta leder till inkonsekventa dimensioner och densitet i den färdiga produkten. Denna prestanda förändras med pulvrets sammansättning, inklusive mängden bindemedel som finns i blandningen, partikelstorleksfördelningen och partikelformen. Ett sätt att kvantifiera i vilken grad pulvret sprids för att fylla formen jämnt är att använda den egenskap som kallas "flytbarhet". Det finns flera tekniker för att mäta flytbarhet, och varje teknik ger inte alltid resultat som överensstämmer med andra tekniker. Det är därför viktigt att veta vilken eller vilka tekniker som förutsäger pulvrets slutliga beteende i denna tillämpning innan den används i kvalitetssäkring eller för att utforma en process. Vidare mäts pulvrets partikelstorleksfördelning och form med dynamisk bildanalys för att undersöka om det finns något samband mellan nyckelvärden för dessa egenskaper och komprimeringsbeteendet. I den här studien jämfördes statisk rasvinkel, tappdensitet, hallflödestid och pulverreometri samt med dimensionerna på pressar och sintrade verktygsinsatser i vätskefas för att förstå vilken teknik som hade det starkaste beroendet på kompatibiliteten, vilket definieras som förhållandet mellan den högsta dimensionen i insatsen och den minsta. Efter studien visade resultaten att en mer omfattande partikelstorleksfördelning förbättrar komprimeringsegenskaperna och att pulver med högre motståndskraft mot ett roterande blad tenderar att ha bättre komprimeringsegenskaper. Vidare kunde inte ett tydligt mönster för resultaten för alla mätmetoder och sambandet på komprimeringbeteendet för hårmetallverktygen urskiljas. Sammanfattningsvis visade studien på att det går att använda sig av mätmetoder för att kunna urskilja ett samband mellan resultaten på mätmetoderna och pulvers kompaktibillitetsegenskaper. Genom att använda sig av enkla mätningar för att kunna förutsäga kompaktibilitetsegenskaper samt komprimeringsbeteende kan både pengar respektive tid sparas. Vidare kan genomförandet av denna studie i framtiden leda till ännu bättre pressnings- samt kompaktibilitetsegenskaper för hårdmetallverktyg.