Ces travaux de thèse concernent l’étude du comportement thermo-physique de mélanges de polymères biosourcés chargés de poudre d’Inconel 718 mis en forme par Moulage par Injection de poudre Métallique. Des matériaux et procédés innovants pouvant permettre une amélioration du procédé ont été étudiés. L’utilisation de polyéthylène glycol (PEG), choisi pour ses propriétés de solubilité dans l’eau, et de polymères biosourcés, pour diminuer l’impact environnemental, ont été choisi. Les nuances de polymères biosourcés ont été choisies adaptées aux conditions du procédé de moulage par injection, il s’agit d’acide polylactique et de polyhydroalcanoates. De même, l’utilisation du CO2 à l’état supercritique comme solvant, a pour objectif de diminuer le temps de déliantage ainsi que d’augmenter la qualité des composants réalisés. Les résultats obtenus ont montré une dégradation du PEG et de l’acide stéarique lors des cycles de mélangeage de de moulage par injection dans les conditions d’utilisation des polymères biosourcés. L’utilisation des mélanges chargés composés de polymères biosourcés ont permis d’améliorer l’homogénéité des composants injectés, mais ont engendré des défauts lors de l’étape de déliantage. Ces défauts ont pu être éliminés par l’utilisation de CO2 à l’état supercritique comme solvant du PEG. Ce dernier procédé a permis une diminution importante du temps de déliantage ainsi qu’une amélioration de la qualité des composants finaux. Les composants densifiés possèdent les propriétés mécaniques correspondantes à l’Inconel 718. / The works done during this PhD focuses on the study of the thermo-physical behavior of bio sourced polymer blends loaded with Inconel 718 powder (feedstock) to be shaped by the Metal Injection Molding process (MIM). First, a review of the researches related to the MIM process was conducted to identify innovative materials and processes that can improve the MIM process. Thus, the use of polyethylene glycol (PEG), selected for its properties of solubility in water, and bio sourced polymers, in order to reduce the environmental impact, were selected. The bio sourced polymers have been selected in accordance with the conditions of the injection molding process, and the choice was made to use polylactic acid (PLA) and polyhydroalkanoates (PHA and PHBV). Similarly, the supercritical CO2 as solvent was chosen to reduce the time of binder removal as well as increasing the quality of components produced. Thermo-physical, mechanical and rheological characterizations were made to determine the behavior of the different feedstock formulations. The results showed a degradation of the PEG and of the stearic acid under the conditions of use of the biopolymers, during the mixing and the injection stages. The use of feedstock made of bio sourced polymers have improved the homogeneity of the injected components, but they have generated defects during the debinding step. These defects have been eliminated by the use of CO2 in the supercritical state as solvent of the PEG. This method has significantly decrease the time of binder removal and improved the quality of the final components. Finally, densified components have the mechanical properties corresponding to Inconel 718.

Integrally moulded hinges and tension bands are important features in packaging components for plastic closures and their function is critically dependent on the flow induced micromorphology in the hinge section. Polymer characteristics and processing of the hinge also have an influence on the hinge properties obtained. This study is aimed at obtaining interrelationships between polymer characteristics, in-cavity flow, microstructure development and hinge properties, to produce hinges with enhanced functional properties. Three different virgin polypropylene (PP) grades were investigated (homopolymer PP-H, random copolymer PP-RC and impact copolymer PP-IC) and injection moulding simulation was carried out using Moldflow software. In-cavity data acquisition has been carried out for different sets of injection moulding conditions, using high performance transducers and a data acquisition system. A comparison between Moldflow simulation and practical injection moulding data suggests that, for thin wall injection moulded components the real time pressure data are in close agreement during the injection stage. During the packing stage there is some disagreement between these data, since the thickness of hinge and tension band sections are 0.4 mm and 0.5 mm respectively, suggesting that these dimensions are extending the capability of the software. An extensive study using a design of experiments (DoE) approach was carried out on both practical and predictive data. Injection velocity and melt temperature were the most influential factors on the component mechanical properties. From the optical micrographs it is observed that PP-RC has a finer micro-structure compared to PP-H and PP-IC and some micrographs confirm Moldflow simulation results in which hesitation effects are evident, as the flow converges into the thin hinge and tension band sections. PP-clay nanocomposites (PP-CN) were prepared using a twin screw compounder. Transmission electron microscopy (TEM) has shown some evidence of dispersion and exfoliation of the clay particles in the PP matrix. However, X-ray diffraction (XRD) results show a reduction in inter-layer spacing of PPCN s possibly due to clay compaction. The addition of nano-clay however has not resulted in any significant improvements in the mechanical properties of hinges and tension bands. The high degree of molecular orientation induced in the hinge and tension-band sections appears to mask any improvements attributed to the addition of nano-clay. From the reprocessed and post consumer recyclate (PCR) study conducted on hinges and tension bands, it is seen that with an increase in both the re-processing and PCR content there is a decrease in the component strength of around 14%, giving scope to potentially use PCR in future packaging applications. Investigations conducted on colour pigments (violet and green) reveal that the onset of crystallisation for green pigmented mouldings is considerably higher (16°C) than for natural and violet mouldings. Optical micrographs also reveal a finer microstructural texture for green components, indicating a high nucleating capability of the green pigment. Irrespective of the colour, both for hinges and tension bands, the yield stress values were around twice as high as the values quoted in the manufacturer s data sheet for isotropic PP, due to the high levels of molecular orientation in the hinge and tension band sections. In order to industrially validate the findings from the DoE study, commercial closures were produced in industry on a production tool then characterised. In the case of tension bands, there was a good agreement between the results obtained from lab scale and industrial study due to the relatively simple geometry. For hinges this agreement is not so clear. Finally a comparison of mechanical properties of the 3 PP grades shows that PP-H has a higher yield stress compared to PP-IC and PP-RC and yield stress is significantly higher (yield strain values are lower) than values quoted by the manufacturer. The PhD study has confirmed the process conditions that are able to optimise all the interactive effects to improve functional properties in high volume parts in the packaging industry.

Durant ces dernières décennies les matériaux composites organiques ont subi un très grand essor dans le domaine des structures aéronautiques. Leur principal avantage est d’alléger les structures tout en gardant de bonnes propriétés mécaniques. De plus, leur microstructure leur permet d’avoir un caractère multi-fonctionnel, ce qui facilite leur intégration pour remplacer les technologies existantes. Dans l’industrie aéronautique, il existe un besoin croissant de grande quantité de petite et moyenne pièces (clips, éléments de jonctions). Cependant, il est aujourd’hui difficile de fabriquer en série des pièces ayant des formes tridimensionnelles complexes par des procédés conventionnels (autoclave). Ainsi, l’orientation envisagée est d’utiliser les procédés de la « famille » automobile pour des applications aéronautiques « semi-structurales », comme le moulage par injection de composites thermoplastiques renforcés de fibres courtes. Cette application nécessite une maîtrise et une fiabilisation du procédé ainsi que des propriétés induites. Ceci a été réalisé par l’identification et la quantification des effets des paramètres qui influent significativement sur la microstructure et les propriétés macroscopiques, par un plan d’expériences. De plus, le dimensionnement de telles pièces requiert une modélisation robuste du comportement mécanique pour prédire au mieux leur capacité d’utilisation. Les données sur la microstructure ont permis d’alimenter un modèle micromécanique comportant un critère d’endommagement de l’interface fibre/matrice. Développé sur un code éléments finis industriel, il a permis de prédire les résultats expérimentaux d’une pièce industrielle. / During the last decades, organic composite materials have undergone great development in the field of aeronautical structures. Their main avantage is to reduce the structures weight while maintaining good mechanical properties. In addition, their microstructure allows them to have a multi-fuctional nature, which facilitates their integration to replace existing technologies. In the aviation industry, there is a growing need for large amount of small and medium parts (clips, connecting elements). However, nowadays it is difficult to produce parts with complex by conventional methods dimensional shapes (autoclave). Thus, the considered path is tu use methods of the automotive “family” for “semi-structual” aerospace applications such as injection-moulding of thermoplastic composites reinforced by short fibres. This application requires a mastery and reliability of the process and the induced properties. This was achieved by the identification and quantification of the parameters effects that significantly influence the microstructure and macroscopic properties, by a design of experiments. Moreover, the dimensioning of such parts requires a robust mechanical behabior modelling to predict the best use of their capacity. The data on the microstructure enable to feed a micromechanical model featuring damage criteria of the fiber/matrics interface. Developed on a industrial finite element code, it was used to predict the experimental results of an industrial part.

Conselho Nacional de Desenvolvimento Científico e Tecnológico / Aesthetic and functional excellence in dental prosthetic rehabilitation has been achieved with the increase of advanced ceramics in dentistry. Processing techniques such as heat press injection moulding and CAD/CAM (computer-aided design/computer aided manufacturing) impart decreased porosity to the microstructure, as well as simplicity and automation of the process. In order to examine the machining surface finish of a leucite glass-ceramic produced using Brazilian raw materials, heat-pressed performs were obtained. These preforms had dimensions close to those of the final crown infrastructure in order to allow fast and easy final matching and finish-milling by using a Brazilian milling machine (MTC Robotica), supported by DentMILL (SEACAM) CAM software. As a control and reference manufacturing process, four crown infrastructures were milled by using CEREC®-3 machine. Aimed at achieving a machinable microstruture, two different heating schedule were tested for ceramizing the feldsphatic glass ingots. X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), nanoindentation test and fracture toughness measurement by indentation method were used as characterization methods. Comparison of the properties of the experimental material with those published by other investigator on similar commercial materials conducted to the conclusion that it is a machinable glass-ceramic with acceptable features for application in dental prosthetic rehabilitation. Preforms milling simulation using MTC Robotica machine conducted to the prediction of very long milling time (18h), even considering preforms possessing dimensions similar to those of the desired milling end product, a manufacturing time much greater than those found in commercial CAD/CAM dental milling machines. / A reabilitação protética do elemento dentário com excelência estética e funcional tem sido alcançada através do amplo uso de cerâmicas avançadas na odontologia. Técnicas de processamento como moldagem por injeção a quente e usinagem por CAD/CAM (computer-aided design/computer aided manufacturing) conferem ao material uma microestrutura com menor porosidade, além de simplificar e permitir automação de sua execução. Com o objetivo de avaliar a superfície usinada de uma vitrocerâmica feldspática leucítica produzida a partir de matéria prima nacional, foram confeccionadas pré-formas deste material pela técnica de moldagem por injeção sob pressão a quente. Estas pré-formas têm dimensões aproximadas a da peça final com a finalidade de serem usinadas na fresadora CNC nacional de baixa rotação (MTC Robótica), auxiliada pelo software CAM DentMILL (SEACAM). Além disso, foram usinadas peças do mesmo material no sistema CEREC®, como forma de controle. Para a obtenção de uma microestrutura com melhor usinabilidade, foram testadas duas metodologias de ceramização das pastilhas de vidro feldspático. A caracterização do material foi realizada por meio da difração de raios X (DRX), microscopia eletrônica de varredura (MEV), microscopia de força atômica (AFM), ensaios de nanoindentação e de tenacidade à fratura pelo método da indentação. A partir da comparação das propriedades deste material aos dados obtidos na literatura sobre materiais similares existentes no mercado foi possível classificar o material como usinável e indicar sua aplicação na clínica odontológica reabilitadora. A simulação da usinagem das pré-formas na fresadora MTC Robótica, mesmo com dimensões aproximadas a da peça final, apresentou um tempo de usinagem muito longo (18h), o que a tornou inviável comparada aos sistemas CAD/CAM consolidados no mercado.

Injection moulding using the process of Shear Controlled Orientation Injection Moulding (SCORIM) to enhance the aesthetic characteristics of plastics was investigated. Unsightly surface weld lines were successfully removed from highly reflective aluminium flake pigmented plastics by the application of a single macroscopic SCORIM shear when used in series with Bright Surface Moulding (BSM). A gonio spectrophotometer (GSP) was used for the quantitative characterisation of the Al flake pigmented mouldings as a measure of surface reflectivity and preferred angle of reflection. The different directional properties of surface reflectivities to either side of a conventional weld line are unacceptable, but were successfully reoriented approximately uniformly with the use of SCORIM and BSM moulding (i. e. SBM) used in series. SBM therefore provided an acceptable quality of surface finish for mouldings originally containing a weld line, without deterioration of mechanical properties. Indeed, some improvements in mechanical properties were observed. Translucent two-colour mouldings were used to successfully demonstrate the flow paths taken by sheared material during the application of macroscopic shears. The use of intermittent shearing to encapsulate shear oriented material in the solidifying layers, manifested original and profound aesthetic effects. This resulted from mixing the two colours and was reproducible and widely variable. The morphology of isotactic polypropylene (iPP) processed in this way and examined by light and electron microscopy revealed how only one or two intermittent shears were required to orient a large volume of the moulding in the shear direction. Moreover, U-shaped flow paths demonstrated that the easiest shear route was close to the mouldings edges, an observation supported by x-ray analysis. The addition of Al flake pigment was found to act as a heterogeneous nucleant for ß-spherulites. This acted as a suitable marker for the clear identification of the displaced weld interface using polarised light microscopy, of filled and unfilled iPP. y-phase was identified with the use of only one or two intermittent shears which reflects an increase in molecular alignment and consequent improved mechanical properties. The intensity of the y-phase increased with the volume of material sheared. Strong evidence was also obtained of a linear relationship between the logarithm of the time lapse between two intermittent shears and the corresponding values of a-phase index, crystallinity index and percentage crystallinity. The values of each increasing proportionally with the length of time used. Microhardness characterisation revealed anisotropy within SCORIM samples consistent with preferred orientation and increased modulus in the shear direction. The skin layers were characterised as the softest region through the thickness of SCORIM mouldings. The results of this work were used to provide the basis of a computer simulation of the SCORIM process under development at the University of Wales Swansea.

Abstract The main object of this thesis was to research injection mouldable 0–3 type ceramic polymer composites and their dielectric and magnetic properties in the GHz frequency region. The work has been divided into three sections. In the first section, two–phase ceramic polymer composites containing dielectric and magnetic fillers have been investigated and their characteristics analysed by reference to pre–existing mixing rules. The exploitation of these composites in miniaturizing devices, such as antennae, is presented and discussed. The second part describes three phase composites containing different nanosize additives (silver, silicon and alumina fibres) towards improving their dielectric properties. In the third part, some periodical and multilayer structures for ceramic polymer composite layers are proposed. In the case of two–phase ceramic polymer composites, with 37 vol.% of dielectric filler (Barium Strontium Titanate, BST) embedded into a thermoplastic polymer (ER140) matrix, the highest measured relative permittivity was 15 with a dielectric loss value of 0.008 at 1 GHz. With 43 vol.% of magnetic filler (hexaferrite, CO2Z) in ER182 matrix, the highest achieved relative permeability was 1.8 with a magnetic loss value of 0.077 at 1 GHz. Composites with Co2Z filler provide a 77% size reduction, and could thus be used advantageously in antennae. It was found that a 2–6 vol.% nanoaddition in BST–ER140 composites enhanced the relative permittivity drastically with only a minor effect on the dielectric losses. In particular, with only 2 vol.% addition of nanosize silver particles into the BST–ER140 composite, a 52% increase in the relative permittivity was obtained, with no significant change in the dielectric losses (tan δε = 0.004). Vertically and horizontally periodical dielectric composite structures comprising layers of different dielectric properties have been fabricated as well as multilayered structures containing dielectric and magnetic layers. The measurement results indicate that such multimaterial multilayer structures are good candidates for components with reduced dielectric and magnetic losses. / Tiivistelmä Väitöstyön tavoitteena oli tutkia ruiskuvalettavien 0–3 –liitännäisten keraami-polymeerikomposiittien ominaisuuksia erityisesti niiden GHz-taajuusalueen dielektristen ja magneettisten ominaisuuksien kannalta. Työ on jaettu kolmeen osaan. Ensimmäisessä osassa on tutkittu kaksikomponenttisia keraami-polymeerikomposiitteja, joissa täytemateriaali on joko dielektristä tai magneettista materiaalia. Komposiittien ominaisuuksia on analysoitu jo olemassa olevien seosmallinnuskaavojen avulla. Komposiittien hyödyntämistä erilaisten sovellusten, kuten antennien, minityrisoinnissa on myös käsitelty. Toinen osa käsittelee kolmikomponenttisia komposiitteja, joissa lisäaineena on käytetty pieniä määriä nanomateriaaleja (hopea- ja piipartikkelit sekä alumiinioksidikuitu) tarkoituksena parantaa komposiitin dielektrisiä. Kolmannessa osassa on tutkittu periodisia ja monikerroksisia keraami- polymeerikomposiittirakenteita rakenteita. Kaksikomponenttisten keraami-polymeerikomposiittien tapauksessa suurin permittiivisyyden arvo 15 dielektristen häviöiden ollessa 0.008 (mittaustaajuus 1 GHz) saatiin komposiitille, jossa dielektristä täytemateriaalia (Barium Strontium Titanaatti, BST) oli 37 tilavuus-% termoplastisessa polymeerimatriisissa (ER140). Korkein saavutettu permeabiliteetin arvo 1.8 magneettisten häviöiden ollessa 0.077 (mittaustaajuus 1 GHz) saatiin komposiitille, jossa magneettista täyteainetta (hexaferriitti, Co2Z) oli 43 tilavuus-% ER182 -matriisissa. Tämä täyteaine mahdollistaa nykyistä jopa 77 % pienempien antennielementtien kehittämisen. Tukimuksessa todettiin 2–6 tilavuus-% nanomateriaalin lisäyksen BST-ER140 -komposiitteihin kasvattavan permittiivisyyttä merkittävästi juurikaan vaikuttamatta dielektrisiin häviöihin. Erityisesti 2 tilavuus-% hopeananopartikkeleiden lisäys BST-ER140 -komposiitteihin kasvatti permittiivisyyttä 52 % dielektristen häviöiden (tan δε =  0.004) kasvamatta. Työssä on myös tutkittu periodisesti (vertikaali ja horisontaali) koostettuja dielektrisiä komposiittirakenteita, jossa eri kerroksissa on erilaiset dielektriset ominaisuudet sekä monikerrosrakenteita, joissa vuorottelevat dielektriset ja magneettiset kerrokset. Mittaukset osoittivat, että monimateriaaliset monikerrosrakenteet ovat hyviä kandidaatteja komponentteihin, jotka vaativat pieniä dielektrisiä ja magneettisiä häviöitä.

This master’s thesis deals with influence of gas content in structure of polymer materials to mechanical properties. Test specimens were prepared by MuCell technology from polyphthalamide reinforced by 50 % of glass fiber content. The theorethical part of this thesis is focused on polymer materials with attention to polyamides and injection moulding technology. In the experimental part, the dependence between the characteristics obtained from the tensile test and the Charpy impact test on the amount of gas in the polymer is examined.

The thesis deals with the design of a robotic workplace for the operation of injection moulding machines. It is concerned with the design of the workplace component deployment and the evaluation of the best variant using a multi-criteria assessment. In detail, attention is paid to the end effectors of industrial robots and the assembly workplace, where finishing operations take place. Finally, the risk analysis and technical and economic evaluation of the proposed workplace are carried out.

The project elaborated design of injection mould for production of corner cover, which serves to protect a reprobox from mechanical damage. The production possibilities were considered at the beginning. The injection molding technology was chosen from available technologies. The first part of the thesis is theoretic, plastics and injection molding are investigated. The choice of suitable polymer and the entire draft of mold is in the second part of thesis. The final mold is two-cavity with cold runner system. The technical and economic assessment of the proposal is carried out in the last part of thesis.

Yes / A novel process chain for serial production of polymer-based devices incorporating both micro- and nano-scale features is proposed. The process chain is enabled by the use of Zr-based bulk metallic glasses (BMG) to achieve the necessary level of compatibility and complementarity between its component technologies. It integrates two different technologies, namely laser ablation and focused ion beam (FIB) milling for micro-structuring and sub-micron patterning, respectively, thus to fabricate inserts incorporating different length scale functional features. Two alternative laser sources, namely nano-second (NS) and pico-second (PS) lasers, were considered as potential candidates for the first step in this master-making process chain. The capabilities of the component technologies together with some issues associated with their integration were studied. To validate the replication performance of the produced masters, a Zr-based BMG insert was used to produce a small batch of micro-fluidic devices by micro-injection moulding. Furthermore, an experimental study was also carried out to determine whether it would be possible by NS laser ablation to structure the Zr-based BMG workpieces with a high surface integrity whilst retaining the BMG's non-crystalline morphology. Collectively, it was demonstrated that the proposed process chain could be a viable fabrication route for mass production of polymer devices incorporating different length scale features.