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This diploma thesis studies short fiber reinforced composites for dental applications. Barium particulate filler, nanosilica and short glass and polyvinylalcohol fibers were added to the matrix consisting of four dimethacrylate types of monomers. The effect on material properties was observed. For characterization of different types of composite materials following methods were used: thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), three point bending test for notched and un-notched samples and scanning electron microscopy (SEM). Viscoelastic properties, modulus of elasticity and strength, critical values of stress intensity factor and strain energy release rate and polymerization shrinkage of composite materials were determined. It is possible to improve these properties of composite materials by adding short fibres to particulate reinforced composite. To make this modification more efficient, it is necessary to change surface treatment of fibres and preparation method of short fiber reinforced composites. Viscosity of material has raised after adding short fibers and processing of these types of dental material in dental laboratory is considered difficult to provide.

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Yes / Composites have clinical application for their ability to mimic the hierarchical structure of human tissues. In tissue engineering applications the use of degradable biopolymer matrices reinforced by bioactive ceramics is seen as a viable process to increase osteoconductivity and accelerate tissue regeneration, and technologies such as additive manufacturing provide the design freedom needed to create patient-specific implants with complex shapes and controlled porous structures. In this study a medical grade poly(l-lactide) (PLLA) was used as matrix while apatite-wollastonite (AW) was used as reinforcement (5 wt% loading). Premade rods of composite were pelletized and processed to create a filament with an average diameter of 1.6 mm, using a twin-screw extruder. The resultant filament was 3D printed into three types of porous woodpile samples: PLLA, PLLA reinforced with AW particles, and PLLA with short AW fibres. None of the samples degraded in phosphate buffered solution over a period of 8 weeks, and an average effective modulus of 0.8 GPa, 1 GPa and 1.5 GPa was obtained for the polymer, particle and fibre composites, respectively. Composite samples immersed in simulated body fluid exhibited bioactivity, producing a surface apatite layer. Furthermore, cell viability and differentiation were demonstrated for human mesenchymal stromal cells for all sample types, with mineralisation detected solely for biocomposites. It is concluded that both composites have potential for use in critical size bone defects, with the AW fibre composite showing greater levels of ion release, stimulating more rapid cell proliferation and greater levels of mineralisation. / The research was funded in part by the UK EPSRC Centre for Doctoral Training in Additive Manufacturing and 3D Printing (EP/L01534X/1), the UK EPSRC Centre for Innovative Manufacture in Medical Devices (EP/K029592/1), and Glass Technology Services Ltd., Sheffield, UK.

End-gated and centre gated mouldings have been assessed with varying thickness and sprue geometries for the centre gate. Alternative image analysis techniques are used to measure the orientation and length of injection moulded short and long fibres composite components. The fibre orientation distribution (FOD) measurements for both geometries have been taken along the flow path. In shear flow the FOD changes along the flow path, however the FOD remains relatively constant during expansion flow. The core width and FOD at the skin within a long glass fibre (LGF) specimen is different in comparison to a short glass fibre (SGF) specimen. Fibre length measurements have been taken from the extrudate, sprue and 2 positions within the centre gate cavity. The size of the sprue has little influence on fibre breakage if the moulding is more than 1 mm thick The SGF FOD prediction models within Autodesk Simulation Moldflow Insight 2014 (ASMI) have been validated against measured SGF data. At present, by default, the models over-predict the < cos2θ > for most geometries. When the coefficients are tailored for each model, drastic improvements are seen in the FOD prediction. The recently developed SGF RSC model accurately predicts the FOD in shear, in a thin geometry, whereas the Folgar-Tucker model predicts the FOD accurately in expansion flow. The measured LGF fibre length distribution (FLD) and FOD have been validated against the LGF prediction models. The LGF models are currently under predicting the breakage and over-predicting < cos2θ >. The breakage prediction improves if measured FLD of the extrudate is input into the model.

End-gated and centre gated mouldings have been assessed with varying thickness and sprue geometries for the centre gate. Alternative image analysis techniques are used to measure the orientation and length of injection moulded short and long fibres composite components. The fibre orientation distribution (FOD) measurements for both geometries have been taken along the flow path. In shear flow the FOD changes along the flow path, however the FOD remains relatively constant during expansion flow. The core width and FOD at the skin within a long glass fibre (LGF) specimen is different in comparison to a short glass fibre (SGF) specimen. Fibre length measurements have been taken from the extrudate, sprue and 2 positions within the centre gate cavity. The size of the sprue has little influence on fibre breakage if the moulding is more than 1 mm thick The SGF FOD prediction models within Autodesk Simulation Moldflow Insight 2014 (ASMI) have been validated against measured SGF data. At present, by default, the models over-predict the <cos2θ> for most geometries. When the coefficients are tailored for each model, drastic improvements are seen in the FOD prediction. The recently developed SGF RSC model accurately predicts the FOD in shear, in a thin geometry, whereas the Folgar-Tucker model predicts the FOD accurately in expansion flow. The measured LGF fibre length distribution (FLD) and FOD have been validated against the LGF prediction models. The LGF models are currently under predicting the breakage and over-predicting <cos2θ>. The breakage prediction improves if measured FLD of the extrudate is input into the model. / Autodesk Ltd.

L’utilisation de composites à matrice thermoplastique renforcée par fibres courtes (TRFC) connait une forte croissance pour une large gamme d’applications industrielles pour des conditions de chargement extrêmes (e.g. pare-chocs d’automobiles). Il est donc indispensable de développer des modèles de comportement des TRFC tenant compte des spécificités du matériau pour une large gamme de vitesse de déformation. Toutefois, le comportement de ces composites est complexe. Cette complexité est due, en premier lieu, au comportement viscoélastique (VE)-viscoplastique (VP) de la matrice avec une sensibilité à la pression. A cela s’ajoute les caractéristiques complexes du renfort en termes de distributions d’orientation des fibres courtes. De plus, le comportement de ces composites est affecté par des phénomènes d’endommagement coexistants (e.g. endommagement de la matrice et décohésion l’interface fibre/matrice). Dans ce travail, un modèle permettant la prise en compte de l’ensemble de ces phénomènes est proposé. Sa formulation est basée sur la décomposition du matériau en un milieu matriciel et plusieurs milieux de fibres, sur la base d’une décomposition additive du potentiel thermodynamique. Cette approche permet une implémentation simplifiée avec une résolution successive (mais non indépendante) du comportement de chaque milieu. Un avantage immédiat est la possibilité de prendre en compte tout type de comportement matriciel et tout type d’orientation. L’interface fibre/matrice, siège de la transmission de l’effort est modélisée par un transfert par cisaillement, avec sur une hypothèse locale d’iso-déformation dans la direction de la fibre. L’endommagement ductile de la matrice est pris en compte par un modèle d’endommagement anisotrope. La dégradation de l’interface fibre/matrice est décrite par un modèle de décohésion initiée en pointe de fibres. Un critère de rupture se basant sur le taux maximal de vide crée par décohésion est enfin introduit. La caractérisation du modèle est basée sur des campagnes d’essais quasi-statiques et dynamiques pour le cas de polypropylène pur et renforcé par fibres courtes de verre, à différents angles de chargement par rapport à la direction d’injection. Ces essais sont complétés par des observations au microtomographe permettant la caractérisation des distributions d’orientation locale des fibres. Des observations au MEB ont enfin permis de constater une éventuelle influence de la vitesse de sollicitation sur les mécanismes d’endommagement. / Short fibre-reinforced composites are commonly used in a variety of engineering applications, including automotive and aerospace industry. Today, their use is progressively extended to parts possibly subjected to severe loading conditions (e.g. crash...), characterised by high strain rates. Therefore, an efficient modelling that takes into account material’s specificities at a large strain rate range is needed. A constitutive model of viscous behaviour of short-fibre reinforced composites (SFRC) where complex distributions of fibre orientations are taken into account is proposed in this work. The approach considered for the computation of composite macroscopic behavior is based on an additive decomposition of the state potential. The SFRC is assimilated to an assembly of several fibre media embedded in a polymeric matrix medium. One of the main assets of this approach is the possibility to model reinforcement with complex distributions of fibre orientations. Moreover, this decomposition allows the implementation of complex behaviour laws coupled with damage models. The polymeric matrix behaviour is typically strain-rate sensitive, i.e. viscoelastic-viscoplastic. This property has to be taken into account when the modelling of the composite behaviour over a large range of strain rate is intended. Therefore, a viscoelastic constitutive model, based on generalised Maxwell model, and a viscoplastic correction scheme, based on an overstress approach, are implemented for matrix material. The developed constitutive model is then coupled to two damage laws. The first one is introduced in the framework of Continuum Damage Mechanics in order to model the anisotropic ductile damage behaviour of the matrix material. The second one deals with fibre/matrix interfacial degradation through an interfacial debonding law. In order to identify the parameters involved in the present model, experimental tests are performed (case of polypropylene reinforced with short glass fibres). Microcomputed tomography is used for the characterisation of the fibres distribution of orientation. The efficiency of the proposed model is demonstrated by comparisons between numerical and experimental responses in different loading conditions, including dynamic loadings.

Nowadays, thin-walled load bearing structures can be realised using textile reinforced concrete (BRAMESHUBER and RILEM TC 201-TRC [1]). The required tensile strength is achieved by embedding several layers of textile. By means of the laminating technique the number of textile layers that can be included into the concrete could be increased. To further increase the first crack stress and the ductility as well as to optimize the crack development, fine grained concrete mixes with short fibres can be used. By a schematic stress-strain curve the demands on short fibres are defined. Within the scope of this study, short fibres made of glass, carbon, aramid and polyvinyl alcohol are investigated in terms of their ability to fit these requirements. On the basis of these results, the development of hybrid fibre mixes to achieve the best mechanical properties is described. Additionally, a conventional FRC with one fibre type is introduced. Finally, the fresh and hardened concrete properties as well as the influence of short fibres on the load bearing behaviour of textile reinforced concrete are discussed.

Ce travail porte sur la mise en forme des matériaux composites à matrice polymère renforcée par des fibres courtes dont les performances physiques et mécaniques sont directement reliées à la distribution spatiale et à l’orientation des renforts employés. Il se focalise sur l’étude des mécanismes de déformation se produisant au cours de l’écoulement de ces systèmes qui se comportent comme des suspensions de fibres non-newtoniennes. Le problème est abordé par une procédure originale combinant images 3D acquises en temps réel et simulations numériques avancées, réalisées à l’échelle des fibres. Dans le premier cas, des suspensions modèles avec fluide suspensif non-newtonien ont été déformées en compression dans des conditions confinées dans un microtomographe à rayons X synchrotron. Cette technique a permis l’acquisition en temps réel de clichés 3D à forte résolution spatiale de l’écoulement des suspensions. Dans le deuxième cas, un code de calculs éléments finis 3D a été utilisé, celui-ci étant capable de décrire finement des objets immergés dans des fluides non-newtoniens, par des level-sets et des techniques de remaillage anisotrope. La pertinence des simulations numériques dans les régimes de concentration dilués à semi-dilués a été jaugée par une comparaison expériences-simulations avancée.De là, dans le régime de concentration dilué, nous montrons que le confinement de l’écoulement et le comportement rhéofluidifiant du fluide suspensif ont une influence mineure sur la cinématique des fibres, si ces dernières sont suffisamment éloignées des plateaux de compression. Si ce prérequis n’est pas respecté, l’effet du confinement devient important. Des modifications au modèle heuristique d’haltère de la littérature ont été proposées pour corriger la cinématique de fibres. Dans le régime semi-dilué, des déviations de la cinématique de fibres sont également observées au cœur des suspensions. Ces déviations sont principalement liées aux interactions hydrodynamiques entre fibres suffisamment voisines. La cinématique des fibres prédite par le modèle de Jeffery et les approximations de champ affine sont mises en défaut. Dans le régime concentré, si l’évolution de l’orientation globale de la suspension est étonnamment bien décrite par l’équation de Jeffery, de très importantes fluctuations des champs de translation et de rotation des fibres sont observées à l’échelle des fibres. Celles-ci sont induites par les nombreux contacts entre fibres qui peuvent par ailleurs être correctement prédits par le modèle de tube. / This study focuses on the processing of short fibre-reinforced polymer composites. The physical and mechanical properties of these materials are mainly affected by the position and orientation distribution of fibres induced during their forming. Thus, we analysed the flow-induced micro-mechanisms that arose at the fibre scale during the forming stage of these complex systems which behave as non-Newtonian fibre suspensions. For that purpose, an original approach was developed by combining 3D imaging technique and direct numerical simulation, both performed at the fibre scale. Hence, several model fibre suspensions with a non-Newtonian suspending fluid and with a concentration regime that ranged from dilute to concentrated were prepared . They were subjected to confined lubricated compression loadings using a rheometer mounted on a synchrotron X-ray microtomograph. Thanks to very short scanning times, 3D images of the evolving fibrous microstructures at high spatial resolution were recorded in real-time. These experiments were also simulated using a dedicated Finite Element library enabling an accurate description of fibre kinematics in complex suspending fluids thanks to high performance computation, level sets and adaptive anisotropic meshing. The efficiency of the numerical simulation from the dilute to semi-dilute concentration regimes was assessed through experimental and numerical comparisons.Then, we showed that the confinement effect and the non-Newtonian rheology of the suspending fluid had a weak effect on the fibre kinematics, if the fibres were sufficiently far from the compression platens, typically the fibre-platen distance should be larger than twice the fibre diameter. Otherwise, confinement effects occurred. Some extensions of the dumbbell model were proposed to correct the fibre kinematics in this flow conditions. In semi-dilute concentration, deviations of the fibre kinematics compared to the Jeffery’s predictions were also observed and related to hydrodynamic interactions between fibres. In this case, the predictions of Jeffery’s model and the related assumption of affine fibre motions are less relevant. In the concentrated regime, even if the overall orientation of fibre suspension could be astonishingly well described by using the Jeffery’s model, strong fluctuations on each fibre motion and rotation were observed. These deviations were induced by the numerous fibre-fibre contacts, which could be correctly predicted by the tube model.

Magnesium alloys have emerged as a promising material for light-weighting due to their potential for higher weight saving compared with advanced high-strength steel, aluminium alloys and glass fibre reinforced polymer composites based on equal stiffness or strength. Even though magnesium alloys offer low density, high strength to weight ratio and excellent machinability their poor creep resistance and low yield strength at elevated temperatures (~150oC) restricts their use in automotive powertrain applications. Possible ways of improving the creep resistance include development of creep resistant alloys and/or reinforcing the alloy with ceramic particulates, fibres/whiskers. Several magnesium alloys such as – Mg-Zr based alloys, Mg-Al-RE alloys (RE: rare earth), Mg-Al-Ca alloys, Mg-Al-Sr alloys, Mg-Al-Sr-Ca alloys, Mg-Al-Si alloys offer improvement in creep resistance to different extent. However, these alloys are relatively expensive than the widely used Mg-Al-Zn alloys. Some of these alloys are unsuitable for die casting application due to cracking or die filling problems for example, in Ca and Sr containing alloys their content must be controlled to avoid castability problems. Discontinuous reinforcement of magnesium alloys opens up wide variety of casting techniques for production. Most of the components do not require high performance capability all throughout the component. Squeeze casting technique can be used to economically produce selectively reinforced composites having complex near-net-shape components. By selectively reinforcing only the regions of stress concentration, material property can be optimised at the same time lowering both the cost of manufacturing and machining. In the present study, wear behaviour of Saffil short fibre reinforced AZ91D Mg alloy composite prepared by squeeze casting is explored. The Mg-Saffil composite had a two dimensional planar random fibre orientation which was inherent to the fabrication process of porous fibre preform. In the as-polished specimen fibres protrude out of the Mg matrix due to differential polishing. The Mg-Saffil composites were subject to unidirectional sliding wear against steel counterface under nominally dry condition in ambient atmosphere at low velocities, to simulate the piston reversal at the top dead centre of an engine wherein lubrication starvation results in wear of engine cylinder. The fibres protruding out of the magnesium matrix prevent the softer Mg matrix coming in contact with the counterface material. The worn surface was examined by means of scanning electron microscopy and the physical and chemical changes caused by the wear processes were characterised using different spectroscopic techniques. The effect of fibre distribution and fibre orientation on wear of the composite was studied. Depending on the radius of curvature of the counterface, inhomogeneities in the fibre distribution up to a certain length scale were permissible without deteriorating the wear resistance of the composite. The normal fibre orientation proved deleterious to the wear of the counterface. But wear of the composite was independent of the fibre orientation of the wear surface. In contrast to unreinforced AZ91 Mg alloy which undergoes extensive wear, the steel counterface was machined by the hard alumina fibres protruding out of the matrix. With progressive sliding a discontinuous patch of transferred material formed on the worn surface. Eventually, an oxidised iron-rich transfer layer formed on the worn surface due to compaction of the transferred material and wear debris under the combined action of applied normal load and frictional force. The coefficient of friction plateaus following an initial rapid increase with the increase in the areal coverage of the transfer layer. The abrupt increase in friction coincides with the change in contact at the sliding interface from protruding alumina fibres/steel counterface to mostly between the transferred layer and steel counterface. The increase in friction due to the iron-rich transfer layer formed on the worn surface induced bending stresses in the fibre. A correlation between the incipient fibre fracture and build-up of the transfer layer was observed. Wear of the composite was governed by the dawn of the fibre fracture event, which in turn leads to three-body wear. Diamond-like carbon coatings are well-known for their low friction, high hardness and elastic modulus, chemical inertness and optical transparency. They have found widespread use due to their superior tribological characteristics as protective coatings for magnetic storage media (hard-disk drives), in micro-electromechanical devices (MEMS), biomedical applications (joint implants, artificial heart valves), optical windows (anti-reflection coating) and razor blades. The physical and mechanical properties of these coatings can be tailored by controlling the sp3 /sp2 ratio and modification via alloying with metals such as W, Ti, Cr, Al; or non-metallic elements such as B, N, F, Si. A tungsten doped hydrogenated diamond-like carbon coated steel counterface was used to rule out or minimise any chemical and physical interaction between the composite and the counterface. The composite exhibited a higher wear resistance when slid against a DLC coated steel counterface due to ease of interfacial sliding between the carbon-rich transfer layer and the DLC coated counterface. The transition from ultra-mild to mild wear was not altogether suppressed but delayed to higher loads, prolonging the ultra-mild wear regime. As a result of reduced friction the point of maximum shear stress recedes from the surface, which manifests as subsurface cracks. The dominant wear mechanism of Mg-Saffil composite sliding against the DLC coated counterface was delamination wear.