This study investigates analytically and experimentally extrusion processes of magnesium hollow tubes by a single-cylinder extrusion machine and double-cylinder extrusion machine. The first part of this study is to conduct analysis and experiment of hollow helical tube extrusion by single-cylinder extrusion machine. Firstly, a design criterion is proposed to determine the forming parameters and discuss the effects of product size, extrusion ratio, billet length, etc. on the mandrel surface stress. The effects of the die bearing part length, angle of rotation, extrusion speed, initial temperature, petal number, etc. on the radial filling ratio are also investigated. Better parameters are chosen from analytical results to conduct hot extrusion experiments for obtaining sound products. Microstructure observation and hardness test are conducted at the cross-section of the product. The experimental values of extrusion load and product¡¦s dimensions are compared with the analytical values to verify the validity of the analytical models. The second part of this study is to conduct analysis and experiment of hollow tubes extrusion by a double-cylinder extrusion machine. The effects of extrusion ratio, billet length, mandrel diameter, etc. on the drawing force on the mandrel and critical conditions without mandrel fracture are discussed.

This study focused on analysis and experiment of hot extrusion of aluminum and magnesium alloys, an extrusion die with an inclination angle leads to non- uniform velocity distribution at the cross-section of the die, and results in different strain and strain rate distributions. This kind of design can make the grain size at the material surface smaller and get a material with larger surface hardness. This study aims to conduct hot extrusion with different die inclination angles, and obtain a material with gradient micro-structures. At first, die with different inclination angles are designed, and the temperature at the die exit and effective strain, effective strain rate distributions are discussed using the finite element analysis. At last, aluminum and magnesium extrusion experiments are conducted and the micro-structures of the materials are observed to understand the effects of the die inclination angles at 15 degrees on the grain size distribution and hardness test at the cross-section of the material. The grain size is about 17.2£gm at around center of the cross-section and hardness is about 68.2HV. The smallest grain size is 4.1£gm at the edge of the cross-section and the highest hardness is 83.8HV.

This study is to analyze and test the extrusion process of a hollow spur gear and a solid helical product with magnesium alloy. In the hollow spur gear part, firstly, a design criterion to determine the forming parameters is proposed. Then, the Finite Element Analysis is used to simulate the flow pattern of the billet from separating channel, welding chamber to die bearing part. From a series of simulation results, the effect of separating channel length, mandrel entrance angle, welding chamber height, etc. on the radial filling ratio, welding pressure, extrusion load, etc. are found. By using the Taguchi Methods, we can find the most important parameters. Finally, a better die geometry is designed to obtain a sound product. In the helical product part, the Finite Element Analysis is used to get the understandings of radical filling ratio of magnesium alloy in the helical zone. Then, a better die geometry is designed from the results of analyses. Finally, hot extrusion experiments of a hollow spur gear and a solid helical product are conducted. The experimental values of the extrusion load and the product¡¦s dimension are compared with the analytic values to verify the validity of the analytic models.

Antibiotic use is a vital method for the treatment of most diseases involving bacterial infections. Unfortunately, in certain cases these agents are not effective in treatments against diseases for either some limitation in antibiotic usage because of the side effects or some distribution problems caused by physiological or pathological barriers in the body. Such problems are thought to be minimized by development of controlled release systems which involve implantation of antibiotic loaded polymeric systems directly to the site of infection. Present study involves Vancomycin, a very strong antibiotic with a wide spectrum of activity, and two biocompatible and biodegradable polymers, poly(3-hydroxybutyrate-co-3-valerate) PHBV and poly(L-lactide-co-glycolide) PLGA, in the construction of rod shaped controlled release systems designed for the aim of local treatment of osteomyelitis. Vancomycin carrying rods of either PHBV 8 or PLGA (50:50) polymers were prepared by the use of cold paste and hot extrusion methods in two different loading ratios (2:1 and 1:1 P:V). In situ release kinetics of each type of rod was determined by spectrophotometric measurement of vancomycin concentration. For determination of drug content of the controlled release rods initially and at the end of the release experiments, extraction and IR (infrared) studies were carried out. The efficacy of the system was measured in vitro on the bacterial strain, B. subtilis. Characterization of the rods was made by the use of stereomicroscopy and SEM (scanning electron microscopy). In situ release results of the controlled Vancomycin release formulations revealed that for both polymer types, hot extrusion process enabled the formation of a more compact system that provided slower release of the agent compared to the cold paste method. With the combined effect of variable loading proportion and polymer type the most prolonged release was obtained by PHBV rods having 2:1, P:V, ratio (prepared by hot extrusion method). In general, the release kinetics from the rods obeyed the Fickian diffusion kinetics except for PLGA rods prepared by cold paste method with 1:1 and 2:1 (P:V) loading ratios, which had a first order rate of drug release. According to in vitro bioactivity assays, all the groups effectively inhibited bacterial growth with the first day release samples. On the seventh day, however, only two cold paste samples, PHBV:Vancomycin 1:1 and PLGA:Vancomycin 1:1 had drug content barely sufficient for MEC while the others were in the ineffective range. The IR and grinding-extraction studies proved that Vancomycin was still present within the rods after a ten day release period. The PHBV rods with 2:1 (P:V) ratio prepared by hot extrusion method seem to be the most promising drug delivery system in terms of providing prolonged release as an implantable drug delivery system for the treatment of bacterial infections of the bone, namely osteomyelitis.

Made available in DSpace on 2015-05-08T14:59:49Z (GMT). No. of bitstreams: 1 arquivo total.pdf: 4777169 bytes, checksum: 71196705eb82b84523fd48e17cf15f5b (MD5) Previous issue date: 2013-10-04 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The composites metal matrix exhibit properties that are of great interest to the mechanical and aerospace industry, especially when it incorporates low weight with high strength. Currently, the composites ductile matrix reinforced with nanoparticles of amorphous and quasicrystalline alloys have been studied intensively. One reason is that quasicrystals exhibit aperiodic crystal structures, a fact that gives these materials unique properties such as low friction coefficient, high hardness, among others. In these work, the effect of extrusion variables in the production of aluminum composite reinforced with 0%, 3%, 6% and 20% quasicristal Al59,2Cu25,5Fe12,3B3 alloy has been studied. The composites were obtained by mechanical alloying with balls mass ratio 10:1, with rotation of 200rpm, in the period of 3h. The powder mixtures were conformed by hot compaction and extrusion. The analysis carried out by scanning electron microscopy (SEM) showed good distribution of quasicrystalline particles in the aluminum matrix, but was not detected the presence of formation of quasicristal interface with the matrix. It was observed that there was in increases in hardness of the composite increases with the fraction of reinforcement in the matrix, and also with increasing temperature and the rate of extrusion.The maximum resistance to traction was 196MPa, reached with 6% composite reinforcement. It was also found that the tensile strength increases with increasing temperature and mainly by increasing the rate of extrusion. It was found that for the pure aluminum the maximum resistance occurs for the extruded at 450°C. Thus it can be concluded that increasing extrusion temperature of 400°C to 500°C accompanied the increase in extrusion ratio from 2:1 to 3:1 provides improvements in the mechanical properties of the aluminum-quasicristal composite obtained by mechanical alloying and conformal by compaction and extrusion. / Os materiais compósitos, com matriz metálica, apresentam propriedades que são de grande interesse para a indústria mecânica e aeroespacial, principalmente, quando se incorpora o baixo peso com alta resistência mecânica. Atualmente, os compósitos com matriz dúctil reforçada com nanopartículas de ligas amorfas e quasicristalinas têm sido estudados intensivamente. Um dos motivos é que os quasicristais apresentam estruturas cristalinas aperiódicas, fato que confere a esses materiais propriedades única como o baixo coeficiente de atrito, elevada dureza, entre outras. Neste trabalho estudou-se o efeito de algumas variáveis de extrusão no processamento de compósito de alumínio com reforço volumétricas de 0%, 3%, 6% e 20% de quasicristal da liga Al59,2Cu25,5Fe12,3B3. Os compósitos foram obtidos por moagem de alta energia com razão massa bolas de 10:1, com rotação de 200rpm, no período de 3h. Os pós das misturas foram conformados por compactação e extrusão a quente. As análises realizadas por microscopia eletrônica de varredura (MEV) apresentaram boa distribuição das partículas quasicristalinas na matriz de alumínio, porém não foi verificada a presença da formação de interface do quasicristal com a matriz. Observou-se que houve aumento da dureza do compósito com o aumento da fração de reforço na matriz e, também, com o aumento da temperatura e da razão de extrusão. A resistência máxima a tração foi de 196MPa, atingida com compósito de 6% de reforço. Identificou-se também que resistência a tração eleva-se com o aumento da temperatura e principalmente com o aumento da razão de extrusão. Verificou-se que, para o alumínio puro a resistência máxima ocorre para os extrudados a 450ºC. Com isso pode-se concluir que o aumento da temperatura de extrusão de 400ºC até 500ºC acompanhada do aumento da razão de extrusão de 2:1 para 3:1 proporciona melhorias nas propriedades mecânicas dos compósitos alumínio-quasicristal obtidos via moagem de alta energia e conformado por compactação e extrusão a quente.

L'élaboration des aciers ODS fait appel à une étape de consolidation par filage à chaud. Les propriétés très anisotropes de ces matériaux à l'état filé, notamment les nuances purement ferritiques (>12% Cr), nécessitent une meilleure compréhension des effets du procédé de filage sur la microstructure. Ainsi, ce travail de thèse a pour objectif principal d'étudier les évolutions de la microstructure lors de la transformation à chaud des aciers inoxydables ODS ferritiques, et plus globalement de comprendre le comportement de ces matériaux sous sollicitation mécanique à haute température. Pour cela, des essais de filage interrompus et des essais thermomécaniques de torsion et de compression à chaud (1000-1200°C) ont été réalisés sur plusieurs aciers ferritiques à 14% de Cr présentant différents taux de renfort en titane et en yttrium. Les microstructures obtenues après déformation ont été caractérisées par EBSD.L'ensemble des analyses microstructurales effectuées montre que la mise en forme à chaud des aciers ferritiques par filage s'accompagne d'une recristallisation dynamique de type continue. Après formation des sous-joints par restauration, leurs désorientations continuent à croître, et ceux-ci se transforment graduellement en joints de grains au cours de la déformation. La cinétique de ce mécanisme semble néanmoins fortement influencée par les caractéristiques de la précipitation présente dans le matériau ; la recristallisation devenant moins complète lorsque les précipités sont plus fins et plus nombreux. En plus du taux de renfort, l'étude de la déformation de ces nuances en torsion et en compression dans des conditions proches de celles observées en filage révèle également une forte influence de la température sur leur comportement. Les microstructures de déformation présentent une évolution d'autant plus importante que la température et/ou le taux de renfort sont limités. À 1000°C, les évolutions observées indiquent la présence de la recristallisation dynamique continue. En revanche, lorsque l'on augmente la température et/ou le taux de renfort, la déformation s'accompagne d'une évolution limitée de la microstructure, notamment en torsion où un endommagement sévère aux niveaux des joints de grains est observé. Dans ce cas, les résultats sont interprétés par un mécanisme d'accommodation de la déformation au voisinage des joints de grains. Les paramètres rhéologiques calculés à partir de ces essais mécaniques confirment la tendance à une faible activité plastique au sein des grains dans les nuances renforcées. / The production of ODS steels involves a powder consolidation step usually using the hot extrusion (HE) process. The anisotropic properties of extruded materials, especially in the ODS ferritic grades (>wt%12Cr), need a better understanding of the metallurgical phenomena which may occur during HE and lead to the observed microstructure. The hot working behavior of these materials is of particular interest. The methodology of this work includes the microstructure analysis after interrupted hot extrusion, hot torsion and hot compression (1000-1200°C) tests of ferritic steels with 14%Cr and different amounts in Ti and Y2O3.The microstructure evolution during hot extrusion process is associated with continuous dynamic recrystallization (CDRX). It leads to the creation of new grains by the formation of low angle boundaries, and then the increase of their misorientation under plastic deformation. The investigations highlight also the role of precipitation on the kinetics of this mechanism; it remains incomplete in the presence of fine and dense nanoprecipitates. After hot deformation in torsion and compression, it is noticed that both precipitates and temperature deformation have a significant impact on the deformation mechanisms and microstructure evolution. Indeed, the CDRX is dominant when temperature and amount of reinforcement are limited. However, when they are increased, limited microstructure evolution is observed. In this case, the results are interpreted through a mechanism of strain accommodation at grain boundaries, with low dislocation activity in the bulk of the grains.

Transparent polycrystalline aluminum oxide is a promising optical material, particularly in applications that require ballistic protection. However, the rhombohedral crystal structure of alumina limits its transparency due to birefringent scattering. One method of reducing birefringent scattering is to align the particles along the same crystallographic direction, minimizing the refractive index mismatch. This dissertation explores the use of high aspect-ratio platelet-morphology alumina powder in order to process a crystallographically aligned polycrystalline alumina part, with improved optical properties. The optimal hot-pressing parameters of non-pre-aligned platelet alumina were explored, showing that a low pre-load pressure (0MPa), a high maximum temperature (1800°C), a low maximum pressure (10MPa), and a long isothermal hold time (>5hrs) yields dense, transparent parts. These parameters resulted in samples with a high in-line transmission (>65%) despite a large grain size (>60μm). This is due to a high degree of crystallographic orientation, which minimizes the refractive index mismatch between grains, reducing birefringent scattering. Pre-alignment resulted in a further increase in crystallographic orientation, indicating that the pre-alignment procedure effectively aligns the platelets along the same crystallographic orientation. However, pre-alignment resulted in a minimal improvement in optical properties due to the pre-aligned platelets decreasing the densification. Mechanical properties were characterized, resulting in a flexure stress and Vickers hardness of approximately 175MPa and 17GPa, respectively. These low mechanical properties are due to the large grain size. The Vickers hardness was also characterized along different alignment/hot-pressing directions, showing that the hardness matches that of sapphire along corresponding crystallographic directions. Modifications to the Rayleigh-Gans-Debye model were made, accounting for crystallographic orientation. The modified model more closely matches the experimental optical data, illustrating the importance of accounting for crystallographic alignment. This dissertation emphasizes the importance of characterizing optical losses in transparent ceramics and how they relate to the microstructure, as well as the significance of crystallographic alignment in a birefringent transparent ceramic like alumina.

No description available.

Le remplacement des systèmes de distribution d’énergie actuels dans les avions (pneumatiques, hydrauliques, mécaniques et électriques) par des systèmes 100% électriques est un enjeu majeur dans le cadre du projet de l’avion « plus électrique ». Le processus d’électrification de l’avion conduit à une augmentation de la puissance embarquée à bord des aéronefs, et par conséquent à une augmentation de la masse du réseau filaire. Afin de pallier à cette augmentation, un nouveau matériau composite possédant des propriétés électriques supérieures à celle du cuivre a été développé dans le but d’augmenter la capacité de courant admissible dans le conducteur à section constante. Ce travail de thèse présente le procédé d’élaboration du matériau composite cuivre-nanotubes de carbone développé ainsi que les techniques de caractérisation utilisées et les résultats associés. Différents paramètres tels que la qualité de la dispersion des renforts dans la matrice, le type de nanotubes de carbone utilisés (multi-parois vs mono-paroi), la nature de l’interface créée entre le cuivre et les renforts (mécanique vs chimique) ainsi que les techniques de mise en forme du matériau (pressage uni-axial à chaud, extrusion à chaud) et de post-traitements (recuit, laminage à chaud) ont été étudiés afin d’obtenir des propriétés physiques optimales. Il en résulte une augmentation des propriétés thermiques (+6,8% pour la conductivité thermique), mécaniques (+32% pour la dureté Vickers) et également électriques - pour la première fois observée- (+3,4 % pour la conductivité électrique) et ce en comparaison avec à une matrice de cuivre pur. / The substitution of the current energy chains in aircrafts (pneumatic, hydraulic, mechanical and electrical) by a 100% electrical chain is a major issue in the field of the “more electric” aircraft. The electrification process leads to an increase of the inboard power of aircrafts, and therefore to an increase of the wired network weight. To counterbalance this increase of mass, a new composite material with higher electrical properties that copper should be considered, in order to increase the current density in the conductor at constant cross section. Several parameters have been studied such as the quality of the carbon nanotubes dispersion, the type of CNTs used (single-walled vs. multi walled), the interface between the matrix and the reinforcements (mechanical vs. chemical), the shaping of material (uni-axial hot pressing, hot extrusion process) and the post treatments processes (heat treatment, hot lamination process). An enhancement of the thermal properties (+ 6.8% of thermal conductivity), the mechanical properties (+32% of Vickers hardness) and for the first time an increase of the electrical properties (+3.4 % for the electrical conductivity) have been observed in comparison with pure copper.

Les verres métalliques ont commencé à être produit dans les années 1960 et sous forme massive dans les années 1980. De nombreuses études se sont intéressées à ces matériaux sous leur forme amorphe et ont conclu qu’ils avaient une forte résistance mécanique mais présentaient un comportement très fragile. Dans le cadre du projet EDDAM débuté en 2011, ces matériaux ont été introduits sous forme de petites sphères dans une matrice d’aluminium. Le premier objectif de notre étude est de voir si le verre métallique sous cette forme permet de le rendre peu fragile. Le second objectif est de trouver une alternative aux renforts céramique dans les composites à matrice métallique qui présentent une faible cohésion à l’interface matrice/inclusion. Dans le but de caractériser l’endommagement dans des nouveaux composites amorphe-cristallins métalliques, la tomographie aux rayons X a été utilisée. Cette technique permet de caractériser de manière non destructive l’endommagement des matériaux et de le visualiser en 3D. Cela apporte une contribution à l’étude des matériaux composites par rapport aux techniques classiques utilisées. L’objectif général de cette thèse a été d’étudier l’endommagement en termes d’amorçage, de croissance et de coales- cence des matériaux composites amorphe-cristallins métallique par tomographie aux rayons X lors d’essais de traction monotone in situ. Les matériaux sélectionnés sont constitués d’une matrice aluminium ("molle" de type 1070A ou "dure" de type 5083) et de renforts en verre métallique Zr57Cu20Al10Ni8Ti5 de taille peu dispersée et répartis de manière homogène, avec différentes fractions volumiques (1%, 4% et 10%). Les matériaux composites ont été élaborés par la voie de la métallurgie des poudres au Spark Plasma Sintering (SPS) suivi d’une étape d’extrusion à chaud. Une attention particulière a été portée sur la caractérisation microstructurale des constituants de base. L’analyse qualitative a permis de comparer l’ensemble des composites fabriqués au SPS et ceux extrudés à chaud après SPS. Les différents modes d’amorçage de l’endommagement ont été observés ainsi que la croissance et la coa- lescence amenant la rupture des composites. L’analyse quantitative a été essentiellement consacrée au premier stade de l’endommagement. La croissance et la coalescence étant très rapide, il a été difficile de les suivre lors des essais interrompus. La modélisation d’un composite amorphe-cristallin métallique à matrice molle a été introduite dans le but de reproduire l’endommagement observé lors des analyses expérimentales. Cette première approche nécessite d’être approfondie dans le but de prédire, compte tenu des propriétés mécaniques des différentes phases et de la fraction volumique des renforts, le mode d’endommagement préférentiel apparaissant dans les composites étudiés. Elle montre cependant les prémices d’une modélisation innovante basée sur la microstructure expérimentale. / Metallic glasses have been produced in the 1960s and bulk metallic glasses in the 1980s. Many studies, focused on these materials in their amorphous state, concluded that they had high mechanical strength but shown low ductility. As part of EDDAM project that started in 2011, these materials were introduced as small particles in an aluminum matrix. The first objective of this study is to see if the metallic glass is less brittle in this form. The second objective is to find an alternative of ceramic reinforcements in metal matrix composites. These materials have low cohesion at the matrix/inclusion interface. In order to characterize the damage in new amorphous-crystalline composite, X-ray tomography was used. This allows to characterize damage in materials and to obtain a 3D viewing. The main objective of this thesis was to study damage (nucleation, growth and coalescence) in composite materials using X-ray tomography during tensile tests. Selected materials are constituted of an aluminum matrix and small metallic glass reinforcements (Zr57Cu20Al_10Ni8Ti5). Composites with different volume fractions (from 1vol.% to 10vol.%) were prepared by Spark Plasma Sintering (SPS) and hot extrusion. A particular attention was paid to the microstructural characterization of the basic constituents. Qualitative analysis was used to compare SPS composites with SPS plus hot extrusion composites. Damage nucleation, growth and coalescence were observed. Quantitative analysis was mainly devoted to the first damage step. Growth and coalescence were difficult to follow due to fast rupture and interrupted tensile tests. The modeling of an amorphous-crystalline composite has been introduced in order to reproduce experimental damage analyses. The first approach requires further investigation to predict damage with different volume fractions. However, this part shows the beginning of an innovative model based on the experimental microstructure.