Ce travail porte sur l'étude du comportement rhéologique de fluide en milieu confiné. Pour cela le levier d'un microscope à force atomique (AFM) est utilisé pour sonder les propriétés rhéologiques d'un fluide confiné entre deux surfaces : la surface d'une sphère collée à l'extrémité du levier et une surface plane sur lequel le fluide est déposé. Le dispositif expérimental est constitué du système de mesure d'un AFM et d'un piézoélectrique permettant d'approcher ou d'éloigner de la sphère la surface plane. Un modèle analytique permet d'extraire les propriétés rhéologiques du fluide confiné à partir de la déflexion du levier induite par le pincement du fluide. Cette méthode a été validée pour les fluides newtoniens. Par contre pour les fluides non-newtoniens comme par exemple la solution de polyacrylami de nous avons trouvé que la viscosité dépend de la distance D et que le cisaillement n'est pas le seul paramètre pertinent pour interpréter les propriétés rhéologiques. / This thesis focuses on the study of the rheological behavior of confined fluids. For this purpose, the microcantilever of an atomic force microscope (AFM) is used to probe the rheological properties of a fluid confined between two surfaces, the surface of a sphere glued to the free-end of the AFM microcantilever and a flat solid surface on which the fluid is deposited. The set-up consists of an AFM, an electrical system for the deflection measurement and a piezoelectric device to move the solid surface (approach, oscillation, etc.). An analytical model allows to determine the rheological properties of the confined fluid from the measurement of the microcantilever deflection due to the hydrodynamic force exerted by the fluid on the sphere.This method has been validated for Newtonian fluids. For non-Newtonian fluids, such as polyacrylamide solution, we found that the viscosity depends on the distance D between the sphere and the plane surface and the shear rate is not the only relevant parameter for interpreting the rheological properties.

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This thesis contributes to a development of a method for rheological characterization of microfibrillated cellulose. The intended use of the method is to be able to distinguish between different grades of microfibrillated cellulose. The method that was developed had preparation procedure of suspensions, pH, dry content and conductivity as well as measuring geometry and measuring sequence in mind. The method resulted in using a propeller mixer for sample preparation and the most suitable properties of the samples for comparison of different qualities of microfibrillated cellulose was evaluated to be pH 8 with a dry content of 2.0 wt% and a conductivity of 110 µS/cm. The rheology of the microfibrillated cellulose suspensions was examined by using a dynamic rotational rheometer and a splined bob and cup (C25G/PC25G). The complex viscosity from amplitude sweeps is used as the parameter to distinguish between different grades of 2 wt% microfibrillated cellulose suspensions. At 1.0 wt% the pH of the suspensions appeared to have a very small impact on the results from rheological measurements while an increased conductivity of the suspensions resulted in an increased complex viscosity. The dry content dependency appeared to be exponential in the range of 0.5 to 3.0 wt% and it was thus easier to distinguish between different grades of microfibrillated cellulose when the dry content is 2.0 wt% compared to 1.0 or 1.5 wt%.

Today, the focus lies on the state of the environment and how we can choose more sustainable alternatives to oil based materials. One material of interest is microfibrillated cellulose (MFC).The microfibril exhibits interesting properties, which one is its excellent barrier properties, that is expected to come in good use for the conversion to a more sustainable society. It is believed that the use of biobased barriers will increase with these new materials and MFC is showing promising results. But in order to develop the material to its full potential, it is important to investigate how MFC behaves in different situations, which can be examined with rheological measurements. The aim of the thesis is to examine how the rheological properties of suspensions containing MFC are affected by temperature and time storing and how the learning from this work can be used for influencing dispersion properties. Four samples were investigated, containing different amounts of MFC and modified waxy maize starch. The samples were analyzed with a dynamic rotational rheometer (Kinexus Pro +) with a splined cup and bob. The following steps were included in the method development used in this work: sample preparation, the repeatability, rest time and statistical analysis. An oscillatory shear and steady shear measurement was performed on the samples, and selected samples were studied with microscopy. The results show that the temperature has affected the samples. The shear viscosity of all samples decreased with increasing temperature and the samples followed the temperature dependence of Arrhenius' equation. For samples containing MFC, the structure was affected, and the initial viscosity was not recovered. The complex viscosity did also decrease at the beginning to then suggestively increase, creating a stronger network at higher temperatures. With the raised temperature the bonding between the fibrils became weaker, which in turn made the dispersion less viscous. Then, depending on the applied force, the shear viscosity and complex viscosity acted differently. To conclude, both the shear viscosity and the complex viscosity in these dispersions containing MFC are dependent on the temperature and time storing. By the learnings from this work, a method has been developed to understand how to use temperature and storing time to lower the shear viscosity and lower, or increase, the complex viscosity. / Idag ligger det ett stort fokus på miljöns tillstånd och hur vi kan välja mer hållbara alternativjämfört med oljebaserade material. Ett material av intresse är mikrofibrillerad cellulosa (MFC).Denna mikrofibrill besitter intressanta egenskaper, varav en är enastående barriäregenskaper,som förväntas komma till god användning i omställningen till ett mer hållbart samhälle. Det tros att biobaserade barriärer kommer att användas mer i dessa nya material och här visar MFC lovande resultat. Men för att kunna utveckla materialet till sin fulla potential är det viktigt att undersöka hur MFC beter sig i olika situationer, som kan undersökas genom reologiska mätningar. Syftet med arbetet är att undersöka hur de reologiska egenskaperna för suspensioner innehållande MFC påverkas av temperatur och lagringstid samt hur lärdomen från det här arbetet kan användas för att påverka dispersionsegenskaper. Fyra prover undersöktes,innehållande olika mängd MFC och modifierad majsstärkelse. Proverna analyserades med en dynamisk rotations reometer (Kinexus Pro +) med räfflad kopp och bob. Följande steg ingick i metodutvecklingen som användes i detta arbete: provberedning, repeterbarhet, vilotid och statistisk analys. En oscillerande skjuvning och jämn skjuvmätning utfördes på de olika proverna samt att utvalda prover studerades med mikroskopi. Resultatet visade att temperaturen hade påverkat proverna. Skjuvviskositeten för alla prover minskade med en ökande temperatur och proverna följde temperaturberoendet av Arrhenius ekvation. För prover innehållande MFC påverkades strukturen och startviskositeten återficks inte. Den komplexa viskositeten minskade också till en början för att sedan suggestivt öka, vilket skapade ett starkare nätverk vid högre temperaturer. Med en högre temperatur blev bindningarna mellan fibrillerna svagare, vilket bidrog att dispersionerna blev mindre viskösa. Beroende på den applicerade kraften, verkade skjuvviskositeten och den komplexa viskositeten olika. Slutsatsen var att både skjuvviskositeten och den komplexa viskositeten i dessa prover innehållande MFC beroende av temperaturen och lagringstid. Från lärdomen av arbetet har en metod tagits fram för att kunna använda temperatur och lagringstid för att sänka skjuvviskositeten och sänka, eller öka, den komplexa viskositeten.