A furação é um processo caracterizado por apresentar dificuldades em relação à formação e remoção do cavaco da região de corte, e à geração de altas temperaturas devido ao cisalhamento e encruamento do material no fundo do furo, principalmente, na usinagem do aço inoxidável austenítico. Com isso a presença do fluido de corte com boas propriedades de refrigeração e lubrificação faz-se necessária para preservar a vida da broca e garantir um acabamento satisfatório do furo. Contudo, com a tendência mundial de diminuição da quantidade de fluido de corte dispendido, tem-se buscado técnicas diferentes de aplicação que utilize o lubrirrefrigerante em quantidades reduzidas. Associado a essas novas técnicas, vem sendo empregado cada vez mais o uso de partículas sólidas adicionadas ao fluido com o intuito de aumentar sua eficiência. Um tipo de partícula, que vem sendo aplicada em diversos setores produtivos devido a suas ótimas propriedades mecânicas, químicas e elétricas, é o grafeno. Sendo assim, pretende-se analisar o comportamento da furação do aço inoxidável austenítico AISI 304 utilizando flocos de multicamadas de grafeno dispersos em fluido de corte empregando o projeto de experimentos Box-Behnken A aplicação do fluido é feita externamente utilizando a técnica de quantidade reduzida com três vazões: 1,5 l/h; 2,0 l/h e 2,5 l/h. O comportamento do processo é avaliado pelos esforços de corte (força de avanço e momento torsor), pela rugosidade (média e total), e pelos desvios (dimensional e de circularidade) na entrada e na saída do furo. O desempenho do grafeno é avaliado pela comparação dos resultados da sua utilização com os de outras duas condições de aplicação do fluido de corte sem adições: em quantidade reduzida e em abundância. Teve-se como resultado que todas as variáveis respostas analisadas sofreram alguma influência da velocidade de corte e/ou da vazão do fluido aplicado em quantidades reduzidas. Os benefícios da lubrificação e refrigeração do grafeno são sentidos em alguns resultados, como nos menores valores médios de rugosidade e de desvio dimensional. Mas, na análise do processo como um todo, não se afirma que o fluido de corte com flocos de multicamadas de grafeno aplicado externamente em quantidade reduzida traz mais benefícios que o sem adições. / Drilling is a machining process characterized by difficulties in the formation and removal of the chip from the cutting region and the generation of high temperatures due to shearing and hardening of the material at the bottom of the hole, especially in the machining of austenitic stainless steel. Thus the presence of cutting fluid with good cooling and lubrication properties is necessary to preserve the drill life and ensure a satisfactory hole finish. However, with the worldwide trend of decreasing the amount of cutting fluid expended, different application systems have been sought which use the coolant in reduced amounts. Associated with these new techniques, the presence of solid particles added to the fluid has been increasingly used in order to enhance its efficiency. One of these particles, which have been applied in several productive sectors due to its excellent mechanical, chemical and electrical properties, is graphene. Therefore, it is intended to analyze the drilling behavior of AISI 304 austenitic stainless steel using multilayer graphene flakes dispersed in the cutting fluid using the Box- Behnken Design The application of the fluid is done externally by means of reduced quantity lubricant with three flows: 1.5 l/h, 2.0 l/h and 2.5 l/h. The behavior of the process is evaluated via thrust force and torque, average and total roughness, and dimensional and circularity deviations at the input and output holes. The performance of graphene is evaluated by comparing the results of its use with two other cutting fluid conditions: quantity reduced and abundance. It was found that all the analyzed responses variables had some influence of the cutting speed and/or the flow of the applied fluid in reduced quantities. The benefits of graphene lubrication and cooling are felt in some results, such as the lower values of average roughness and dimensional deviation. However, in the analysis of the process as a whole, it is not possible to state that the multilayer graphene flakes cutting fluid externally applied brings more benefits than without additions.

In this Diploma Thesis the recycling of the PET bottles in the company PETKA CZ, a.s. is under focus. Thesis describes the Italian technology AMUT designed for physical recycling of the PET bottles. The primary goal is the quality of the final recycled product, PET flakes, particularly in the context of undesirable admixtures such as PVC, other polymers and impurities. Due to the deteriorating quality of the PET flakes the equipment Polymer Separation System Purifier N 1024 has been tested, which had significantly reduced admixtures in PET flakes. As it turned out, the current procedures for solving problems with the PET flakes quality are no longer sufficient.

This thesis deals with the recycling of polyethylene terephthalate and its subsequent processing into the form of a regranulate meeting the parameters required for food use. A brief description of recycling technology, PET flake quality rating and input material contamination is provided. Additionally, legislation regarding recycling for food purposes is discussed and regranulation technologies are described. The suitability of these technologies for processing specific flake samples has been confirmed. In the experimental part, differences in the regranulate samples are compared using DSC and FT-IR. It has been found that there are no major differences between food quality samples. Tests were carried out on 200 PET bottles (bottle, label), on which the input material was divided into 16 groups. Groups that are unsuitable for recycling with this technology was defined. In addition, contaminants of the final product were examined. Their approximate composition was determined and the relationship between the labels of the bottles at the inlet and the impurities at the outlet was found. Appropriate solutions have been proposed to reduce this contamination

Cette thèse est consacrée à la réalisation de composites constitués d’inclusions ferromagnétiques dispersées dans une matrice diélectrique en vue d’obtenir des absorbeurs hyper fréquences dans la gamme 1 GHz – 5 GHz. La principale originalité de notre étude repose sur l’utilisation de particules à forte anisotropie géométrique dites sous forme de «pétales». En raison de leurs bonnes propriétés magnétiques (perméabilité et aimantation à saturation élevées), notre choix s’est porté sur l’utilisation d’alliages NiFeMo et FeSiAl pour cette étude. Dans un premier temps, les particules sous forme de pétales sont obtenues par mécanosynthèse. Un ajustement des paramètres de broyage a permis d’obtenir des pétales avec différents rapports de forme (longueur latérale sur épaisseur). Les particules sont ensuite incorporées à une barbotine constituée d’un liant et d’un plastifiant qui est par la suite coulée en bandes selon le procédé Doctor Blade. Les propriétés structurales et magnétiques des particules broyées ainsi que l’orientation des particules dans le composite ont été caractérisées. Dans une seconde partie, les spectres de perméabilité et de permittivité des composites ont été mesurés en cellule monospire et en ligne coaxiale APC7. Les évolutions des spectres en fonction de la quantité de particules dans le composite ainsi qu’en fonction du rapport de forme des particules ont été étudiées. Il a été montré que la transformation en pétales permettait d’obtenir des niveaux élevés de perméabilité et de permittivité. Ainsi, afin d’avoir un absorbeur de qualité, il est nécessaire de limiter les niveaux de permittivité en enrobant les particules. Les pétales NiFeMo ont été enrobés par de la silice selon le procédé Stöber et ceux à base de FeSiAl par oxydation partielle. Les propriétés magnétiques et électriques dynamiques de composites chargées par des pétales enrobés ont également été étudiées. Des modèles analytiques (loi de mélange de Maxwell-Garnett pour la perméabilité et lois d’Odelevsky et de Mclachlan pour la permittivité) ont été utilisés pour reproduire les principales caractéristiques radioélectriques des spectres de perméabilité et de permittivité Enfin, les performances électromagnétiques de ces composites ont été évaluées en considérant le problème générique de la réflexiond’une onde plane sur des revêtements recouvrant un support métallique. Le passage sous forme de pétales a permis de gagner en taux de charge et en épaisseur de couche absorbante par rapport aux composites chargés par des sphères. Cependant, un taux de charge élevé en pétales entraine une augmentation importante de la permittivité réelle et nuit à la condition d’accord. L’enrobage à la silice des pétales NiFeMo a permis de réduire la permittivité et d’atteindre un niveau d’absorption plus important. Ainsi, nous avons pu réaliser des matériaux composites plus légers et plus minces, absorbants dans la gamme de fréquence recherchée / This thesis deals with composites material containing ferromagnetic flaky-shaped particles (high length to thickness ratio) which exhibit improved microwave properties in terms of permeability spectra. It aims at obtaining effective absorbers in the 1 GHz – 5 GHz range. Because of their good magnetic properties (high permeability and saturation magnetization), NiFeMo and FeSiAl alloys were chosen as fillers. Firstly, composite sheets containing flaky-shaped particles were elaborated. Particles with different aspect ratios were obtained through a ball-milling process and then mixed with polymers in a slurry which is casted into sheets by using the Doctor Blade method. Structural and magnetic properties of milled particles and their orientation in the dielectric matrix were investigated. Then, permeability and permittivity spectra measurements were carried out using a single coil permeameter and a standard APC-7 coaxial line. Their evolutions with the particles aspect ratio and the particles volume content in the matrix were studied. It was shown that flaky shaped particles exhibit higher permeability and permittivity levels. Hence, to avoid impedance mismatch, lowering permittivity levels by using an insulating layer is necessary. Consequently,NiFeMo flakes were coated with a silica layer through the Stöber process and FeSiAl flakes with an oxide layer through oxidation. Electromagnetic properties of composites filled with coated flakes were also studied. In addition, permeabilityspectra were fitted combining the Landau-Lifshitz-Gilbert equation and the Maxwell-Garnet mixing rule. Permittivity spectra were fitted using Odelevsky and Mclachlan laws. Finally, their efficiency as a microwave absorber is estimated by calculating the reflection loss of a normal incident electromagnetic wave on an absorbing layer backed by a perfect conductor. Using flaky particles instead of spherical ones allowed the use of lighter and thinner layer. However, it resulted in high permittivity levels and lead to impedance mismatches. Insulating NiFeMo flakes with a silica layer reduced permittivity levels and allowed better absorbing properties. By using flaky shaped particles, we elaborated thinner and lighter microwave absorbers in the 1 GHz – 5 GHz range.

La période de 3500 à 2500 avant notre ère est marquée par une mutation profonde des sociétés. Dans l’espace provençal, on constate un éclatement du complexe néolithique moyen, Ces bouleversements se traduisent, au niveau des industries lithiques, par un changement d’ordre technologique, concernant notamment l’approvisionnement en matière première. Notre étude se concentre sur 6 sites d’habitat de l’espace provençal. Ces occupations sont les plus à même de révéler des informations d’ordre socio-économique. Elles présentent à la fois des industries produites sur les sites et des produits importés provenant d’ateliers spécialisés. L’intérêt est de prendre en compte tous les composants des assemblages lithiques, afin de noter quelles peuvent être les différences de gestion et de consommation entre ces outillages qui procèdent de deux chaines opératoires, d’une part à l’échelle du site, puis entre les sites. Pour cela, la méthode de sélection des outils a été lourde, demandant beaucoup de temps et a été fondée sur l’observation à l’œil nu et à faible grossissement, en amont des observations microscopiques. Les déterminations faites à partir des observations microscopiques ont été confrontées à des référentiels expérimentaux existants. Certaines comparaisons ont nécessité le recours aux référentiels expérimentaux ou ethnographiques d’autres chercheurs. De plus, après l’observation de certaines pièces archéologiques, des expérimentations spécifiques ont été réalisées afin de répondre précisément à certaines problématiques de notre étude, permettant de développer un corpus de pièces de référence encore très peu représentées pour le moment. / The period from 3500 to 2500 BC is marked by a profound transformation of societies. In the Provence area, there is a breakdown of the Middle Neolithic complex. Changes are reflected by lithic industries. We can observe technological changes, including raw material supply. New production methods are emerging . Large blades from specialized workshops begin to spread.Our study focuses on six settlement of the Provence area. These occupations give socio-economic information. Indeed, they have both stone industries produced on sites and blades imported from workshops. The interest is to take into account all the components of the lithic assemblages, to note what are the differences in consumption and management between the tools, first across the site and between sites.For this, the method of selection of tools was cumbersome, time-consuming and was based on observation with the naked eye and low magnification before microscopic observations. The determinations made from microscopic observations were compared with existing experimental repositories. Some comparisons have required the use of experimental ethnographic repositories. After the observation of certain archaeological tools, specific experiments were performed to specifically address some issues of our study to develop a new corpus poorly represented at the moment.

In this thesis a previously unknown mechanism of failure in multilayered slope profiles is identified. In some conditions this mechanism does not confirm to the known failure models (relating to circular failure) used in slope stability analysis. For this reason, major failures have occurred in the artificial cuts despite the fact that the limit equilibrium methods suggest that these cuts would be stable. The limit equilibrium methods were originally created to apply to earth dam walls. In the open pit mining environment, where we face inhomogeneous and inclined multilayered structures, the assumptions of these limit equilibrium methods appear to be inapplicable (e.g. assumption for the equal shear strength along the failure surface). Analysis starts with a general picture of the stress state in the highwall slope, given extant geological conditions and rock properties. The study then focuses on a comparison of the crack-tip stress changes in the rockmass with and without inclusions at the microscopic level. Basing some assumptions on binocular microscope observations of grain structures, it is possible to measure the size of the different inclusions and show that the microscopic carbon flakes present in the rock fabric make a major contribution to the failure process in a mudstone layer in the slope. The approach adopts the fracture-process zone ahead of a crack tip as the controlling parameter of flaw propagation in rock. Flaw coalescence, which is poorly accounted for in current fracture models, is attributable to two phenomena: the flaw propagation due to high level of applied stress; and the linking of fracture-process zones due to the small distance between neighbouring flaws. A condition of flaw coalescence is given based on these two mechanisms. This development allows defining of two zones along the failure surface (frictional and cohesive). In the slope-stability field the shear strength of the rock along the failure plane is a composite function of cohesive and frictional strength. For instance, the relaxation stress normal to bedding, induced by overburden removal, provides an investigation method for the determination of the weakest minerals, which may act as flaws for fracture propagation in low-porosity rock. A method has been developed to determine the critical stress for tensile fracture propagation due to the rock structure and the stress reduction normal to bedding. A proposed failure mechanism is based on the polygonal failure surfaces theory developed by Kovari and Fritz (1978), Boyd’s field observations (1983), Stead and Scoble’s (1983) analyses, Riedel (1929) Shear Fracture Model, Tchalenko and Ambraseys (1970), Gammond’s (1983) and Ortlepp (1997) observations for natural shear failures, computer modelling by McKinnon and de la Barra (1998), the results of many laboratory experiments reported by Bartlett et al. (1981) and the author’s experience. The proposed failure mechanism evaluates stability of the artificial slope profile due to the embedded weak layer structure, layer thickness, layer inclination and depth of the cut. On the basis of the observations and the above-mentioned modified fracture model, the slope profile is divided into two blocks; passive and active blocks. With this new model, it is possible to calculate slope safety factors for the slope failure cases studied in the industry. It has been found that, whereas the conventional slope stability models predict stable conditions, the new model suggests that the slope is only marginally stable (i.e. that failure can be expected). / Thesis (PhD(Mining Engineering))--University of Pretoria, 2007. / Mining Engineering / unrestricted

Roughly 123 million people worldwide are affected by conditions such as epilepsy, dementia, and cardiovascular diseases. Wearable electrodes are currently used to monitor these conditions short-term. Long-term monitoring would allow for predicting seizures and could be used as a preventive treatment. As opposed to the currently used electrodes, wearables that are intended for long-term use must be soft and flexible in order not to cause harm or discomfort for the user. The electrodes should also have high resolution, meaning that the electrode paths should be as narrow as possible without negatively affecting the performance of the electrode. In this thesis, soft and flexible electrode grids based on silicones are developed using UV laser patterning. Two different methods are evaluated: laser curing of silicones with the addition of a photoinitiator, and laser ablation of conductive composite. The results found in this thesis are that photocuring silicones gives a too low resolution to be useful for patterning soft electrode grids. UV laser ablation on the other hand showed high resolution while the electrodes retained stretchability. / <p>Examensarbetet är utfört vid Institutionen för teknik och naturvetenskap (ITN) vid Tekniska fakulteten, Linköpings universitet</p>

Transmission Electron Microscopy (TEM) on light element materials and soft matters is problematic due to electron irradiation damage and low contrast. In this doctoral thesis techniques were developed to address some of those issues and successfully characterize these materials at high resolution. These techniques were demonstrated on graphene flakes, DNA/magnetic beads and a number of water containing biomaterials. The details of these studies are given below. A TEM based method was presented for thickness characterization of graphene flakes. For the thickness characterization, the dynamical theory of electron diffraction is used to obtain an analytical expression for the intensity of the transmitted electron beam as a function of thickness. From JEMS simulations (experiments) the absorption constant λ in a low symmetry orientation was found to be ~ 208 nm (225 ± 9 nm). When compared to standard techniques for thickness determination of graphene/graphite, the method has the advantage of being relatively simple, fast and requiring only the acquisition of bright-field (BF) images. Using the proposed method, it is possible to measure the thickness change due to one monolayer of graphene if the flake has uniform thickness over a larger area. A real-space TEM study on magnetic bead-DNA coil interaction was conducted and a statistical analysis of the number of beads attached to the DNA-coils was performed. The average number of beads per DNA coil was calculated around 6 and slightly above 2 for samples with 40 nm and 130 nm beads, respectively. These results are in good agreement with magnetic measurements. In addition, the TEM analysis supported an earlier hypothesis that 40 nm beads are preferably attached interior of the DNA-coils while 130 nm beads closer to the exterior of the coils. A focused ion-beam in-situ lift-out technique for hydrated biological specimens was developed for cryo-TEM. The technique was demonstrated on frozen Aspergillus niger spores which were frozen with liquid nitrogen to preserve their cellular structures. A thin lamella was prepared, lifted out and welded to a TEM grid. Once the lamella was thinned to electron transparency, the grid was cryogenically transferred to the TEM using a cryo-transfer bath. The structure of the cells was revealed by BF imaging. Also, a series of energy filtered images was acquired and C, N and Mn elemental maps were produced. Furthermore, 3 Å lattice fringes of the underlying Al support were successfully resolved by high resolution imaging, confirming that the technique has the potential to extract structural information down to the atomic scale. The experimental protocol is ready now to be employed on a large variety of samples e.g. soft/hard matter interfaces.

For the automotive sector, plastics play the most important role when designing interior and exterior parts for cars. Currently, most parts are made from petroleum-based plastics but alternatives are needed to replace environmentally harmful materials while providing the appropriate mechanical performance and preferably reduce the cost for the final product. The objective of this work was to explore the use of soy flakes as natural filler in a composite with polypropylene and to investigate the mechanical properties, water absorption and thermal behaviour. For a better understanding of the filler, the soy flakes were characterized extensively with analytical and microscopic methods. Two types of soy fillers were investigated, soy flakes, provided by Bunge Inc., with a 48 wt-% protein content and an industrial soy based filler with 44 wt-% protein content and provided by Ford. The size of the soy flakes after milling was mainly between 50 and 200 µm and below 50 µm for the industrial filler. The aspect ratio for all filler was below 5. The soy flakes were used after milling and subjected to two pre-treatment methods: (1) one hour in a 50 °C pH 9 water solution in a 1 : 9 solid-liquid ratio; (2) one hour in a 50 °C pH 9 1M NaCl solution in a 1 : 9 solid-liquid ratio. A control filler, without pre-treatment was considered. The soy flakes were also compared to an industrial soy based filler provided by Ford (soy flour (Ford)). The thermogravimetric analysis showed an onset of degradation at 170 °C for the treated filler (ISH2O and ISNaCl) and 160 °C for the untreated filler. The biocomposites formulation consisted of 30 wt-% filler, and polypropylene with/without 0.35 wt-% anti-oxidant Irganox 1010 and with/without the addition of MA-PP as coupling agent. All biocomposites were compounded in a mini-extruder, pressed into bars by injection moulding and tested subsequently. The mechanical properties of the biocomposites are promising. An increase of the E-modulus was observed when compared to pure polypropylene. The addition of MA-PP as coupling agent increased the yield strength of the biocomposites. When pure polypropylene and the biocomposites were compared no difference could be seen for their yield strength. The thermal behaviour deduced from differential scanning calorimetry, revealed a similar behaviour for the biocomposites and the pure polypropylene. Only the samples treated in the presence of NaCl and without a coupling agent, appear to have a slightly higher degree of crystallinity. The melt flow index was slightly increased for the biocomposites containing soy flakes pre-treated with NaCl and decreased for biocomposites containing the soy flour. The water absorption behaviour of the biocomposites was quite similar at the beginning with a slightly lower absorption for the materials with coupling agent. After three months, all samples except the ones treated with water showed a weight loss that can be due to the leaching of the water soluble components in the untreated filler and the NaCl treated filler. In conclusion, soy flakes represent an attractive filler when used in a polypropylene matrix if an aqueous alkaline pre-treatment is performed. The aqueous alkaline extraction also leads to the recovery of the proteins that can be used in food products while the remaining insoluble material is used for the biocomposites, avoiding the competition with the use of soy for food products...

For the automotive sector, plastics play the most important role when designing interior and exterior parts for cars. Currently, most parts are made from petroleum-based plastics but alternatives are needed to replace environmentally harmful materials while providing the appropriate mechanical performance and preferably reduce the cost for the final product. The objective of this work was to explore the use of soy flakes as natural filler in a composite with polypropylene and to investigate the mechanical properties, water absorption and thermal behaviour. For a better understanding of the filler, the soy flakes were characterized extensively with analytical and microscopic methods. Two types of soy fillers were investigated, soy flakes, provided by Bunge Inc., with a 48 wt-% protein content and an industrial soy based filler with 44 wt-% protein content and provided by Ford. The size of the soy flakes after milling was mainly between 50 and 200 µm and below 50 µm for the industrial filler. The aspect ratio for all filler was below 5. The soy flakes were used after milling and subjected to two pre-treatment methods: (1) one hour in a 50 °C pH 9 water solution in a 1 : 9 solid-liquid ratio; (2) one hour in a 50 °C pH 9 1M NaCl solution in a 1 : 9 solid-liquid ratio. A control filler, without pre-treatment was considered. The soy flakes were also compared to an industrial soy based filler provided by Ford (soy flour (Ford)). The thermogravimetric analysis showed an onset of degradation at 170 °C for the treated filler (ISH2O and ISNaCl) and 160 °C for the untreated filler. The biocomposites formulation consisted of 30 wt-% filler, and polypropylene with/without 0.35 wt-% anti-oxidant Irganox 1010 and with/without the addition of MA-PP as coupling agent. All biocomposites were compounded in a mini-extruder, pressed into bars by injection moulding and tested subsequently. The mechanical properties of the biocomposites are promising. An increase of the E-modulus was observed when compared to pure polypropylene. The addition of MA-PP as coupling agent increased the yield strength of the biocomposites. When pure polypropylene and the biocomposites were compared no difference could be seen for their yield strength. The thermal behaviour deduced from differential scanning calorimetry, revealed a similar behaviour for the biocomposites and the pure polypropylene. Only the samples treated in the presence of NaCl and without a coupling agent, appear to have a slightly higher degree of crystallinity. The melt flow index was slightly increased for the biocomposites containing soy flakes pre-treated with NaCl and decreased for biocomposites containing the soy flour. The water absorption behaviour of the biocomposites was quite similar at the beginning with a slightly lower absorption for the materials with coupling agent. After three months, all samples except the ones treated with water showed a weight loss that can be due to the leaching of the water soluble components in the untreated filler and the NaCl treated filler. In conclusion, soy flakes represent an attractive filler when used in a polypropylene matrix if an aqueous alkaline pre-treatment is performed. The aqueous alkaline extraction also leads to the recovery of the proteins that can be used in food products while the remaining insoluble material is used for the biocomposites, avoiding the competition with the use of soy for food products...