Konsistensen på en gel bestående av tvärbunden hyaluronsyra beror av tre faktorer: total koncentration hyaluronsyra, gelningsgrad och tvärbindningsdensitet. För att utföra detta projekt erhölls tre olika geler med olika tvärbindningsdensitet. Dessa geler späddes dels med lösning av fri, icke tvärbunden, HA från 100 % gelningsgrad till 90 % och 80 %. De olika gelningsgraderna späddes också med natriumkloridlösning från den totala koncentrationen HA, 35 mg HA/g gel, till 25 mg/g och 15 mg/g. Projekts huvudfråga är att kartlägga gelens reologiska egenkaper då både total koncentration HA och gelningsgrad varieras. För att kunna kartlägga detta har en reometer brukats där följande tre tester körts: tidssvep, frekvenssvep och amplitudsvep. Från erhållen data har sedan två parametrar som representerar gelkompositionernas viskösa egenskaper (G'') och elastiska egenskaper (G') observerats. Även mätning av extruderingskraft har genomförts för att dra vidare paralleller och slutsatser mellan extruderingskraften och de reoligiska egenskaperna. Ur resultaten ses att förlusttangenten tenderar att sjunka när gelningsgraden ökar, d.v.s. gelerna blir då mer viskösa och mindre elastiska. Förlusttangenten sjunker även vid ökande total koncentration HA vilket betyder att G’ ökar mer än G’’ i vardera punkt som gör att förlusttangenten minskar.Det gick även att avläsa att de viskösa egenskaperna i gelen ökar då total koncentration hyaluronsyra minskar samt att de viskösa egenskaperna i gelerna minskar vid en sjunkande gelningsgrad. Mellan gelningsgrad 90-100 % och total koncentration HA 25-35 mg HA/g har analyserna som gjorts i detta projekt gett följande slutsatser. Konsistensen på gel A och C är mer påverkade av gelningsgraden än total koncentration HA. För gel B kan ingen dominerande parameter utläsas. / The softness of a gel made of crosslinked HA (HA = hyaluronic acid) depends onthree factors. One is the amount of free hyaluronic acid in the gel. Another is thedensity of the crosslinked network, which is the molecular entanglements in the gel.The third is the total concentration of HA. In this project a rheometer is used to measure the rheological properties by runningthe following tests: time sweep, frequency sweep and amplitude sweep. From theobtained data, parameters related to viscous properties (G’’) and elastic properties(G’) of the gels were observed. 27 different compositions of gels with three differentconcentrations (35 mg HA/g, 25 mg HA/g, 15 mg HA/g), three different gel contents(100%, 90%, 80%) and three different densities of crosslinked network (A, B, C) wereanalyzed. To draw further conclusions an analysis of extrusion force was performedas well. The results from the frequency sweeps show that the loss tangent for a gel increasedas the total concentration of HA was reduced and that the loss tangent for a gelincreased as the gel content was decreased. This indicates that the gels become moreviscous when either the concentration of HA or the gel content was decreased. Anincrease in concentration of HA results in an increase of G' and an increase of gelcontent also results in an increase of G'. The results from the amplitude sweeps showthat xG' (xG' = storage modulus at the crossover point between G' and G'') increasesas either the concentration of HA or the gel content is increased. For xStrain (xStrain= deformation of the gel at the crossover point) and xStress (xStress = the stressapplied to the gel at the crossover point) no clear trend can be seen regarding the gelcontent. But an increase in concentration of HA results in an increase of both xStrainand xStress. The results from the analysis of extrusion force show that an increase intotal concentration HA increases the force.

Dans le cadre de cette thèse, nous nous intéressons aux différents comportements de fluides structurés (solutions aqueuses de polymères, suspensions), sous écoulements cisaillés. Dans la première partie, nous donnons une description globale des objets constituant le matériau en utilisant une modélisation structurelle, d'une part et en effectuant des mesures de biréfringence pour qualifier l'anisotropie des objets, d'autre part. A travers la loi tentio-optique, nous montrons que le comportement des objets ne dépend que de la contrainte appliquée. En outre, nous étudions les conditions de mesures objectives pour mener une caractérisation rigoureuse, en comparant des mesures de fluage et d'oscillations et en utilisant une approche analytique. Ce qui va permettre de développer une méthode d'identification des paramètres viscoélastiques et leurs évolutions sous cisaillement, dans le régime linéaire et non linéaire. La deuxième partie concerne les écoulements bidimensionnels de ces fluides dans une géométrie de cylindres coaxiaux centrés et excentrés, à grand entrefer. Le dispositif expérimental est validé par des mesures sur un fluide newtonien. L'objectif est d'étudier le comportement local de différents fluides en utilisant la technique de la PIV. Pour cela, nous réalisons un dispositif expérimental fiable et suffisamment précis pour accéder au champs de vitesse instantané dans tous l'entrefer. Les mesures nous permettent d'accéder à la loi de comportement locale de chaque matériau que nous comparons avec la loi de comportement globale donnée par le rhéomètre dans le cas de la géométrie centrée. De plus, des simulations numériques sur Fluent, ont été effectuées pour compléter notre étude. Les résultats obtenus pour des écoulements laminaires, de différents fluides: newtonien, peu rhéofluidifiant, très rhéofluidifiant, montrent qu'il est possible de décrire et prédire le comportement des fluides newtoniens et faiblement rhéofluidifiants mais les modèles classiques existants dans Fluent ne sont pas capables de décrire le comportement des fluides très rhéofluidifiant qui présentent une très forte hétérogénéité des gradients de vitesse dans l'entrefer / Under this thesis, we look at the different behaviors of structured fluids (aqueous solutions of polymers, suspensions) under sheared flow. In the first part, we give a comprehensive description of the items constituting the material using a structural modeling, on the one hand and carrying out birefringence measures to qualify anisotropy objects on the other. Through the tentio-law, we show that the behavior of objects depends only on the applied stress. In addition, we study the conditions of objective measures to conduct a rigorous characterization, comparing creep and oscillations measures, and using an analytical approach. This will help develop a method for identifying viscoelastic parameters and their developments under shear, in both a linear and a no linear regime. The second part concerns the two-dimensional flows of fluids in a coaxial cylinder geometry centered and eccentred, in a wide gap. The objective is to study the local behavior of different fluids using the PIV technic. To do this, we realize an experimental reliable and accurate enough, in all the gap. The experimental device is validated by measurements on a Newtonian fluid. The measures allow to access the local law behavior of each material that we compare with the overall behavior of law given by the rheometer in the case of centered geometry . In addition, digital simulations on Fluent, were made to complement our study. The results for laminar flow, for different fluids: newtonian, little rhéofluidifiant and very rhéofluidifiant, show that it is possible to describe and predict the behavior of some fluid but the existing model in Fluent can not describe the behavior of very rheofluidifiant fluids which have a very strong heterogeneity gradients speed in the gap.

Ces travaux exposent et analysent les performances d’un composite à matrice thermoplastique semi-cristallin au passage et au-delà de la transition vitreuse. Il est nécessaire de donner des éléments objectifs afin d’évaluer et discuter dans quelles mesures ce matériau peut être utilisé de manière innovante. L’objectif visé est de donner des perspectives en termes de plage de températures d’utilisation des matériaux composites à matrice thermoplastique et plus spécifiquement pour des applications à hautes températures. Le composite à fibres continues de carbone et matrice polyétheréthercétone PEEK a ainsi été étudié sur une large gamme de température, avant et après sa température de transition vitreuse (Tg = 143°C).La phase de caractérisation quasi-statique a mis en évidence l’importance du renfort et le bon transfert de charge de la matrice au-delà de la Tg pour les différentes sollicitations. En particulier, la résistance à la rupture en compression s’est avérée intéressante dans l’optique d’une application structurelle. De plus, les observations fractographiques ont mis en évidence des comportements radicalement différents au passage de la transition vitreuse. Le caractère plus ductile de la matrice permet de limiter la propagation de fissures au travers des plis par dissipation de l’énergie : la plastification de la matrice augmente la capacité du composite à dissiper de l’énergie en limitant ainsi la fissuration. Cependant pour des chargements où la matrice pilote la réponse mécanique du composite tels que des efforts de cisaillement, les comportements non linéaires sont fortement accentués. Des mécanismes de déformations dépendant du temps ont été observés à travers des essais de charge-décharge et de fluage au-delà de la Tg : le caractère visqueux de la matrice joue un rôle prépondérant.Ces mécanismes non linéaires étant identifiables sur des temps longs, il était intéressant de proposer des méthodes de modélisation pour prédire le comportement du composite. C’est pourquoi des modèles à l’échelle du pli ont été adaptés en fonction de la température et de la prépondérance des caractères viscoélastique et viscoplastique. Différents essais de fluage-recouvrance en torsion rectangulaire menés sur un rhéomètre ont permis d’évaluer les composantes viscoélastiques et viscoplastiques de la déformation à des températures inférieures et supérieures à la Tg. / The present study shows and analyses the specifications of a semi-crystalline thermoplastic composite as function of temperature, below and above the glass transition. In order to assess and discuss about what extent this material could be innovately use, objective facts must be necessary exposed: the main target is to give the outlooks about the temperature range, in particular the high temperatures. The studied material is a continuous carbon fibre composite with a polyetheretherketone (PEEK) matrix. Its glass transition temperature is around 143°C. It has been characterized throughout a wide temperature range.For several kinds of quasi-static loadings, the load transfer from the matrix to the fibre reinforcement is good even above the glass transition temperature. The compression strength is indeed very interesting for an aeronautical application. In addition, the fracture surface analysis have significantly revealed a different behaviour above the glass transition temperature: the matrix is more ductile and thus the crack propagation is limited thanks to the energy dissipation. However when the mechanical response is driven by the matrix behaviour such as shear loadings, the nonlinear mechanical behaviour of the composite are highly increased. Therefore the time-dependent behaviours have been characterized by using creep experiments and loading-unloading tensile tests as function of the temperature.In order to predict those non-linear behaviours, meso-models have been developed as function of the temperature. Thus viscoelasticity and viscoplasticity have been taken into account to model the nonlinear mechanical behaviour of the composite material, thanks to creep-recovery tests which have been carried out with a torsion rheometer.

Polypropylene fibers are used in concrete mixtures to avoid early cracks during shrinkage. Low thickness of each fiber and low density are reasons, why these fibers are effective in small dosage. Their disadvantages are smooth surface and hydrophobic character of polypropylene, thus it is necessary to improve their surface for better spread during mixing and to reach needed adhesion between fibers and cement paste. In present time are using chemical solutions applied on surface of the fibers to provide better water absorption, but the trend is reducing of using chemicals in industry and this situation demands new technology. There is possible solution, polypropylene fibers treated by low-temperature plasma. This method was developer by cooperation Masaryk University in Brno with company KrampeHarex and Brno Universiry of Technology. The goal of this thesis is to bring comparison, of influence on rheology properties of fresh concrete, between admixed the fibers with applied chemical layer and low-temperature plasma treated polypropylene fibers.

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No. of bitstreams: 1 DissBDQ.pdf: 27222907 bytes, checksum: eb17b232bd0096bfa1e0fb1dd7f4bf74 (MD5) Previous issue date: 2015-10-06 / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / In this study nanocomposites of polyamide-6 (PA-6) reinforced with silica nanoparticles (SiO2) were prepared in order to promote improved mechanical properties for engineering applications. The nanoparticles’ surfaces were chemically modified with the silane agent 3-aminopropyltrimethoxysilane (3- APTMS) to improve the chemical and physical interactions between them and the PA-6 matrix. Nuclear magnetic resonance analysis (NMR) and Fourier transform infrared absorption spectroscopy (FT-IR) showed that 3-APTMS grafting on nanoparticles surface was accomplished. The nanocomposites mixing process was studied in two forms: by torque rheometry, using a torque rheometer internal mixer; and in a co-rotating and intermeshing twin-screw extruder. A preliminary study of the influence of processing variables at the torque rheometer on the degradation of polyamide-6 matrix was performed. The results showed that the greater the filling volume of the mixture in the chamber and the rotational speed of the rheometer’s rotors, the lower the degradation of the polyamide-6. Based on this preliminary study, compositions with 1, 2, and 4 % weight of SiO2 nanoparticles, both unmodified and chemically modified with 3-APTMS were prepared in the torque rheometer. The nanocomposites were compression molded and it was observed that nanocomposites reinforced with 1 wt.% SiO2, both unmodified and surface-modified, presented the best tensile properties. For the nanocomposite samples processed in the twin-screw extruder, the influence of relevant variables – nanoparticle content, chemical surface modification, physical form of the fed PA-6 (granule and powder), rotational speed of screws and extruder feed rate – on mechanical, thermal, and dynamic-mechanical properties were studied. The samples were afterwards injection molded and it was observed that the samples produced using 1 wt.% surface-modified and 100% finely ground PA-6 showed the higher tensile modulus and yield strength values. / Neste estudo foram preparados nanocompósitos de poliamida 6 (PA6) reforçados com nanopartículas de sílica (SiO2), com o objetivo de promover melhoria de propriedades mecânicas para aplicações de engenharia. A superfície das nanopartículas foi modificada quimicamente com o agente silano 3-aminopropiltrimetoxisilano (3-APTMS) para melhorar as interações químicas e físicas entre elas e a matriz de PA6. Análises de ressonância magnética nuclear (RMN) e espectroscopia de absorção no infravermelho por transformada de Fourier (FT-IR) mostraram que houve sucesso na funcionalização das nanopartículas com o agente silano. O processo de mistura dos nanocompósitos foi estudado de duas formas: por meio de reometria de torque em um misturador interno; e em extrusora com rosca dupla co-rotacional e interpenetrante. Um estudo preliminar da influência das variáveis de processamento no reômetro de torque sobre a degradação da poliamida 6, mostrou que quanto maior o volume de preenchimento da câmara de mistura e a velocidade de rotação dos rotores do reômetro, menor foi a degradação da poliamida 6. Com base neste estudo preliminar, foram preparadas no reômetro de torque composições com 1, 2 e 4% em massa de nanopartículas de SiO2 não modificadas e modificadas quimicamente com 3- APTMS. Os nanocompósitos obtidos foram moldados por compressão, tendo sido observado que os nanocompósitos reforçados com 1 %m. de SiO2 não modificada apresentaram as melhores propriedades mecânicas de resistência à tração e deformação na ruptura em ensaio de tração, enquanto os nanocompósitos com 1 %m. de nanosílica modificada apresentaram as melhores propriedades mecânicas de módulo elástico também no ensaio de tração. Para as amostras de nanocompósitos processadas na extrusora de rosca dupla, foram estudadas as influências do teor de nanopartículas, da modificação química superficial, da forma física da PA6 alimentada (grânulo e pó), da velocidade de rotação das roscas e da taxa de alimentação da extrusora sobre as propriedades mecânicas, térmicas e dinâmico-mecânicas. Posteriormente, os corpos de prova foram moldados por injeção e observou-se que a amostra cuja composição polimérica foi de 100% de PA6 fina e reforçada com 1 %m. de nanosílica modificada superficialmente pelo agente silano 3- APTMS apresentou os maiores valores de módulo de elasticidade e de tensão no escoamento no ensaio mecânico sob tração.

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%.

The subject of this diploma thesis is a study of the influence of cellulose ethers on the rheological properties of lime. The theoretical part focuses on rheological parameters, techniques and test equipment used in rheology measurements. Various types of cellulose ethers and their influence on the rheological properties of fresh mortars are described. The practical part deals with the study of the influence of different types and quantities of cellulose ethers on the properties of fresh lime pastes and mortars. The results were obtained from measurements on a rotational rheometer with a special geometry for building materials. Measuring methods used were flow and oscillatory tests. Yield stress, viscosity and flow index were determined by the flow measurement. The stability and stiffness of fresh materials were determined during the oscillation measurements. The measured results are then evaluated and compared.

The Diploma thesis is focus on polymer modified bitumen for warm mix asphalt. The theoretical part of the thesis describes additives which influence the properties of bitumen for their use and reduction of production and service temperatures. Further, the theoretical part describes the conclusions from the researches. This part also describes empirical and functional tests of bituminous binders. The practical part presents the results of individual tests. Tests were performed on samples of non-aged, aged by RTFOT and RTFOT + PAV methods. The results of the work and the assessment of the suitability of bituminous binders are summarized at the end of the thesis.

The diploma thesis is focused on polymer modified binders with different polymer doses. The theoretical part describes the history of the use of bitumen, the extraction of bitumen from oil and behavious of the polymer type SBS/SB, which is used in the diploma thesis on modified binders. Further, the theoretical part describes the empirical and functional tests of bitumen binders. In the practical part the results of indidual tests are presented and compared with the standard ČSN 65 7222-1. At the end of the diploma thesis are summarized results of work and evaluation of binders with the best achieved properties.

The Diploma thesis is focused on rheological properties of bituminous binders and mixtures. Above all, it describes the changes of these properties of samples of bituminous binders and mixtures. Those were brought by the process of laboratory aging, since it simulates the changes occurring in the in the real-life conditions. The theoretical part depicts the field of rheology and methods utilized for simulating the ageing of binders and mixtures. The practical part describes the process of preparation of samples and its testing. Firstly, the ageing of bituminous mixture by the means of BSA method (Braunschweiger Alterung) took place, which was followed by preparing the solids for testing the modulus of stiffness and main testing. The rest of the mixture was used for extracting the binder. Tests with the binder were focused on the usage of dynamic shear rheometer (complex shear modulus, dynamic viscosity). The last part of the work is dedicated to the comparison of the outcomes of testing.