Alumina (Al2O3) matrix nanocomposites reinforced with a second nanometric phase have better mechanical properties, especially of hardness, fracture toughness and wear resistance compared to the monolithic alumina material. On the other hand, niobium carbide (NbC), as a second phase reinforcement, has properties that make it an ideal material for Al2O3 matrix ceramics, such as high melting temperature, high hardness, low chemical reactivity and a coeffi-cient of thermal expansion similar to the material of Al2O3, thus avoiding the appearance of cracks that diminish the resistance of the material. Currently, the largest reserves of niobium are in Brazil and the study on their use is a very important milestone for the country. Therefore, the aim of this thesis is to obtain and character-ize Al2O3 matrix nanocomposites with a second phase of 5% of vol-ume of NbC nanoparticles obtained by reactive high-energy milling, using conventional sintering, Spark Plasma Sintering (SPS) and Microwave. For this, the nanometric precursor powders of Al2O3-NbC were obtained reactive high-energy milling in SPEX mill, were sub-sequently deagglomerated, leached with hydrochloric acid, added to the Al2O3 matrix in the proportion of 5% of volume and dried under air flow. Powders of Al2O3-5vol.% NbC were sintered by different methods: conventional under an argon atmosphere, microwave and SPS using different temperatures. The precursor powders were characterized by X-ray diffraction (XRD), scanning electron micros-copy (SEM) and particle size measurement. Conventional and SPS sintered nanocomposites were characterized microstructurally, the bulk density and hardness was studied by nanoindentation. SPS sintered nanocomposites were characterized with respect to Young's modulus by nanoindentation, fracture toughness and flex-ural strength. On the other hand, conventionally sintered and SPS nanocomposites were characterized with respect to wear resistance by the pin-on-disc technique, using WC-6% Co spheres with loads 30 and 60 N and Al2O3 spheres with loads 15 and 30 N. The results show that reactive high-energy milling has been complete and effi-cient in obtaining nanometric powders with crystallite sizes of 9.1 and 9.66 nm for Al2O3 and NbC, respectively. In addition, the deag-glomeration, after the reactive high-energy milling process, was ef-fective in the dispersion of the NbC inclusions in the Al2O3 matrix. However, it has not been possible to obtain high density Al2O3-5vol.% NbC nanocomposites using conventional sintering and mi-crowave sintering processes. In the sintering process by SPS, the nanocomposites presented high densities, close to the theoretical and, consequently, better hardness and resistance to wear com-pared to the materials obtained in a conventional furnace. The re-sults corresponding to the wear resistance have confirmed that this property is influenced by several factors such as the sintering meth-od and temperature, the spheres used as counter-material and the loads applied during the test. The final results indicated that the Al2O3-5vol.% NbC nanocomposites obtained by SPS have a great potential for the different industrial applications, which require mate-rials of high mechanical and wear performance. / Los nanocomposites de matriz alúmina (Al2O3) reforzados con una segunda fase nanométrica presentan mejores propiedades mecáni-cas, especialmente de dureza, tenacidad a la fractura y resistencia al desgaste, en comparación con el material monolítico de alúmina. Por otra parte, el carburo de niobio (NbC), como refuerzo de segun-da fase, presenta propiedades que lo convierten en un material ideal para las cerámicas de matriz Al2O3, tales como alta temperatura de fusión, alta dureza, baja reactividad química y un coeficiente de expansión térmica similar al material de Al2O3, evitando así la apari-ción de grietas que disminuyen la resistencia del material. Actual-mente, las mayores reservas de niobio se encuentran en Brasil y el estudio sobre su uso es un hito muy importante para el país. Por lo tanto, el objetivo de esta tesis es obtener y caracterizar nanocompo-sites de matriz de Al2O3 con una segunda fase del 5% en volumen de nanopartículas de NbC obtenidos por molienda reactiva de alta energía, y utilizando la sinterización convencional, Spark Plasma Sintering (SPS) y microondas. Para ello, los nanométricos polvos precursores de Al2O3-NbC fueron obtenidos mediante molienda reactiva de alta energía en molino SPEX, desaglomerados, lixivia-dos con ácido clorhídrico, añadidos a la matriz de Al2O3 en la pro-porción de 5% en volumen y secado bajo flujo de aire. Los polvos de Al2O3-5vol.%NbC fueron sinterizados por diferentes métodos: con-vencional bajo una atmósfera de argón, microondas y SPS usando diferentes temperaturas. Los polvos precursores se caracterizaron por difracción de rayos X (XRD), microscopía electrónica de barrido (SEM) y la medición del tamaño de partícula. Los nanocomposites sinterizados convencionalmente y mediante SPS se caracterizaron microestructuralmente, se estudió la densidad aparente y la dureza por nanoindentación. Los nanocomposites sinterizados mediante SPS fueron caracterizados respecto el módulo de Young por nano-indentación, la tenacidad a la fractura y la resistencia a la flexión. Por otra parte, los nanocomposites sinterizados convencionalmente y mediante SPS fueron caracterizados respecto a resistencia al desgaste mediante la técnica de pin-on-disc, utilizando esferas de WC-6%Co con cargas 30 y 60 N y esferas de Al2O3 con cargas 15 y 30 N. Los resultados muestran que la molienda reactiva de alta energía ha sido completa y eficaz en la obtención de polvos nano-métricos con tamaños de cristalito de 9,1 y 9,66 nm para la Al2O3 y NbC, respectivamente. Además, la desaglomeración, después del proceso de molienda reactiva de alta energía, fue eficaz en la dis-persión de las inclusiones de NbC en la matriz de Al2O3. Sin embar-go, no ha sido posible obtener nanocomposites de Al2O3-5vol.%NbC con alta densidad usando procesos de sinterización convencional y microondas. En el proceso de sinterización mediante SPS, los nanocomposites presentaron altas densidades, cercanas a la teóri-ca y, en consecuencia, mejor dureza y resistencia al desgaste en comparación con los materiales obtenidos en un horno convencio-nal. Los resultados correspondientes a la resistencia al desgaste han confirmado que esta propiedad está influenciada por varios fac-tores tales como el método y temperatura de sinterización, las esfe-ras utilizadas como contramaterial y las cargas aplicadas durante el test. Los resultados finales indicaron que los nanocomposites de Al2O3-5vol.%NbC obtenidos mediante SPS tienen un gran potencial para las distintas aplicaciones industriales, las cuales requieren ma-teriales de alto rendimiento mecánico y al desgaste. / Els nanocomposites de matriu alúmina (Al2O3) reforçats amb una segona fase nanométrica presenten millors propietats mecàniques, especialment de duresa, tenacitat a la fractura i resistència al desgast, en comparació amb el material monolític d'alúmina. D'altra banda, el carbur de niobi (NbC), com a reforç de segona fase, presenta propietats que ho convertixen en un material ideal per a les ceràmiques de matriu Al2O3, com és l'alta temperatura de fusió, alta duresa, baixa reactivitat química i un coeficient d'expansió tèrmica semblant al material d'Al2O3, evitant així l'aparició de clavills que disminuïxen la resistència del material. Actualment, les majors reserves de niobi es troben a Brasil i l'estudi sobre el seu ús és una fita molt important per al país. Per tant, l'objectiu d'esta tesi és obtindre i caracteritzar nanocomposites de matriu d'Al2O3 amb una segona fase del 5% en volum de nanopartículas de NbC obtinguts per mòlta reactiva d'alta energia, i utilitzant la sinterització convencional, Spark Plasma Sintering (SPS) i microones. Per a això, les pols precursores d'Al2O3-NbC van ser obtinguts per mitjà de mòlta reactiva d'alta energia en molí SPEX, desaglomerats, lixiviats amb àcid clorhídric, afegits a la matriu d'Al2O3 en la proporció de 5% en volum i assecat baix flux d'aire. Les pols d'Al2O3-5vol.%NbC van ser sinteritzats per diferents mètodes: convencional davall una atmosfera d'argó, microones i SPS usant diferents temperatures. Les pols precursores es van caracteritzar per difracció de rajos X (XRD), microscòpia electrònica d'agranat (SEM) i el mesurament de la grandària de partícula. Els nanocomposites sinteritzats convencionalment i per mitjà de SPS es van caracteritzar microestructuralment, es va estudiar la densitat aparent, i la duresa es van estudiar per nanoindentació. Els nanocomposites sinteritzats per mitjà de SPS es van caracteritzar el mòdul de Young es van estudiar per nanoindentació, la tenacitat a la fractura i la resistència a la flexió. D'altra banda, els nanocomposites sinteritzats convencionalment i per mitjà de SPS van ser caracteritzats respecte a resistència al desgast per mitjà de la tècnica de pin-on-disc, utilitzant esferes de WC-6%Co amb càrregues 30 i 60 N i esferes d'Al2O3 amb càrregues 15 i 30 N. Els resultats mostren que la mòlta reactiva d'alta energia ha sigut completa i eficaç en l'obtenció de pols nanométrics amb grandàries de cristalit de 9,1 i 9,66 nm per a l'Al2O3 i NbC, respectivament. A més, la desaglomeració, després del procés de mòlta reactiva d'alta energia, va ser eficaç en la dispersió de les inclusions de NbC en la matriu d'Al2O3. No obstant això, no ha sigut possible obtindre nanocomposites d'Al2O3-5vol.%NbC amb alta densitat usant processos de sinterització convencionals i microones. En el procés de sinterització per mitjà de SPS, els nanocomposites van presentar altes densitats, pròximes a la teòrica i, en conseqüència, millor duresa i resistència al desgast en comparació amb els materials obtinguts en un forn convencional. Els resultats corresponents a la resistència al desgast han confirmat que esta propietat està influenciada per diversos factors com ara el mètode i temperatura de sinterització, les esferes utilitzades com contramaterial i les càrregues aplicades durant el test. Els resultats finals van indicar que els nanocomposites d'Al2O3-5vol.%NbC obtinguts per mitjà de SPS tenen un gran potencial per a les distintes aplicacions industrials, les quals requerixen materials d'alt rendiment mecànic i al desgast. / Ribeiro Rodrigues Alecrim, L. (2017). DESENVOLVIMENTO DE NANOCOMPÓSITOS DE ALUMINA-CARBETO DE NIÓBIO POR SINTERIZAÇÃO NÃO-CONVENCIONAL [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/90395 / TESIS

Master‘s thesis deals with the preparation and evaluation single-phase high-entropy alloy based on cobalt, chromium, iron, nickel and manganese and its variants strengthened by dispersion of oxidic particles. High-entropy alloy was prepared in powder form by mechanical alloying from the equiatomic proportions of atomic powders. Obtained powder was subsequently compacted by spark plasma sintering. By the method of mechanical alloying were successfully prepared single-phase high-entropy alloy and its variant strengthened by dispersion of nanometric yttria oxides. It has been found that the oxide particles present in the microstructure of high-entropy alloy significantly block mobility of grain boundary and dislocation at elevated temperatures. As a result of this behavior were observed doubling of alloy strength and decreasing of creep rate at 800 °C.

The subject of this thesis is preparation of CoCrFeMnNiNx high entropy mixtures via the methods of mechanical alloying and spark plasma sintering (SPS). Three series of specimens were fabricated in this thesis: samples milled in argon (benchmark materials), samples milled in nitrogen atmosphere (to observe their ability of nitrogen absorption) and samples microalloyed with CrN, FeN nitrides (to observe their dissociation into the solid solution potential). The fabricated powders and SPS compacts were subsequently observed by electron microscopy and their phase content by X-Ray diffraction (XRD) and elemental composition by EDS analysis were carried out. A method of reduction melting in inert atmosphere was used to determine the exact oxygen and nitrogen content in powders, while the respective particle size distribution measured by laser diffraction method. The influence of nitrogen content on the hardness of the samples was studied via the microhardness measured. After completing the process of mechanical alloying under the Nitrogen atmosphere was the maximal concentration of nitrogen in the structure 0,208% after 24 hours of milling (dependency on time was linear), which means, the method of milling under the Nitrogen atmosphere was successful. XRD of milled samples showed the existence of the only FCC single solid solution phase, while samples milled under the Nitrogen atmosphere showed the trend of the growth of the lattice parameter with the increasing nitrogen content. There was observed the presence of the chromium nitrides precipitates on the grain boundaries of the FCC phase in microalloyed samples. All specimen were contaminated by a mixture of metallic oxides and manganeese sulphides, which were present in the default manganeese powder. The greatest value of microhardness showed the duplex sample. The increase in values of microhardness (344 HV 0,3) in comparison with the standard sample (262,9 HV 0,3) was recorded on the samples milled under the nitrogen atmosphere, which conforms the positive influence of the nitrogen content on strength characteristics of this alloy.

This thesis gives a comprehensive characterization of lightweight non-oxide ceramic materials for ballistic applications, an overview of production technologies and processing of boron carbide B4C and its ceramic-based composites. A framework for evaluating the ballistic resistance of the material based on mechanical properties is shown there. It can be used in experiments without normalized equipment. The experiments including B4C + Si, B4C + Ti composites, and application of Spark plasma sintering (SPS) were designed according to outputs from the theoretical part. The volume fractions of Si, Ti dopants were optimized based on ongoing chemical reactions during sintering. The obtained samples were subjects of mechanical testing which results were compared to identify the ideal ratio of matrix and reinforcement. As the best suited material for ballistic protection, B4C + 1,0 obj. % reaches these values of parameters; hardness = 3502 ± 122 HV1; fracture toughness KIC = 2,97 ± 0,03 MPam^0,5.

This diploma thesis deals with the processing of the magnesium-based powder materials with the addition of zinc by the spark plasma sintering. The aim of this thesis is to evaluate influence of sintering parameters and zinc content on the microstructure and mechanical properties of the material. First part of the thesis is literary research which is divided into two main chapters. The first chapter describes magnesium-based materials and mentions their use as biomaterials. The second chapter discusses powder metallurgy, specifically magnesium powders and spark plasma sintering. In the experimental part the powders were sintered at temperatures 300 °C and 400 °C and an analysis was performed using optical microscope, scanning electron microscope, then also EDS analysis and hardness, microhardness and three-point bending tests were performed. An increase in hardness was observed with increasing zinc content and with increasing sintering temperature. The flexural strength was higher for materials sintered at a temperature of 400 ° C.

Thesis deals with design of the experimental single-cylinder spark ignition engines for research purposes. The main purpose of this work is the design crankcase. Summary of possible constructions of spark ignition engines is included. Basic dimensions and 3-D design of the experimental engine resulted from the summary. The numerical analysis of proposed crankcase in ADAMS (MBS) and ANSYS (FEM) software environment is also part of the work. Generally, the proposed solution of the experimental engine was focused on the universality and simplicity of the design.

The main aim of this diploma thesis is to design two different types of air throttles in the intake manifold and compare their influence on a loss of dynamics of the flow of drawn air. The main purpose is to compare the mass flow for wholly opened air throttle. It deals with creating CDF model of intake manifold by using 3D scanner Atos and software Pro/Engineer WF5. During the work, the results of the CFD analysis were used for a real testing.

This master’s thesis deals with the design of the throttle body of the intake manifold of a spark-ignition engine with regards to minimizing throttle loses at full engine load. The first part of this thesis focuses on the elements of intake tract structure on contemporary combustion engine including their design solutions and the theory of flow. The thesis also describes the creation of the 3-D CAD model of intake manifold with a throttle body and the description of the CFD flow simulation with the evaluation of resul.

L'optimisation des systèmes d'allumage est un paramètre critique pour la définition des foyers de combustion industriels. Des simulations aux grandes échelles (ou LES pour Large-Eddy Simulation) d'un brûleur de type bluff-body non pré-mélangé ont été menées afin de comprendre l'influence de la position de la bougie sur la probabilité d'allumage. La prise en compte de la combustion est basée sur une méthode de tabulation de la chimie détaillée (PCM-FPI pour Presumed Conditional Moments - Flame Prolongation of ILDM). Les résultats de ces simulations ont été confrontés des résultats expérimentaux disponibles dans la littérature. Dans un premier temps, les mesures de vitesse et du champ de richesse à froid sont comparées aux résultats de la simulation pour évaluer les capacités de prédiction en terme de structure de l'écoulement et de mélange turbulent. Un suivi temporel des vitesses et de la fraction de mélange est réalisé à différents points pour déterminer les fonctions de densité de probabilité (ou PDF)des variables caractéristiques de l'écoulement, à partir des champs résolus en LES. Les PDFs ainsi obtenues servent l'analyse des phénomènes d'allumages réussis ou déficients rencontrés expérimentalement. Des simulations d'allumage forcé ont été effectuées pour analyser les différents scénarios de développement de la flamme. Les corrélations entre les valeurs locales (fraction de mélange, vitesse) autour de la position d'allumage et les chances de succès de développement du noyau de gaz brûlés sont alors discutées. Enfin, une extension de la méthode PCM-FPI avec prise en compte des effets d'étirement est développée à l'aide d'une analyse asymptotique, puis confrontée aux résultats de mesures expérimentales. / The optimization of the ignition process is a crucial issue in the design of many combustion systems. Large eddy simulation (LES) of a conical shaped bluff-body turbulent non-premixed burner has been performed to study the impact of spark location on ignition success. The chemistry part of the simulation is done using tabulated detailed chemistry approach. This burner was experimentally investigated by Ahmed et al at Cambridge (UK). The present work focuses on the case without swirl for which detailed measurements are available. First, cold fkow measurements of velocities and mixture fraction are compared with their LES counterparts, to assess the prediction capabilities of simulations in terms of flow and turbulent mixing. Time history of velocities and mixture fraction are recorded at selected spots, to probe the resolved probability density function (pdf) of flow variables, in an attempt to reproduce, from the knowledge of LES resolved instantaneous flow conditions, the experimentally observed reasons of success or failure of spark ignition. A flammability map is also constructed from the resolved mixture fraction pdf and compared with its experimental counterpart. LES of forced ignition is then performed using flamelet fully detailed tabulated chemistry combined with presumed pdfs (PCM-FPI). Various scenarios of flame kernel development are analyzed and correlated with typical flow conditions observed in this burner. The correlations between velocities and mixture fraction values at the sparking time and the success or failure of ignition are then further discussed and analysed. The rate of flame development during successful or unsuccessful ignition events are analysed and compared against experimental observations. Finally, from asymptotic flame analysis, a novel approach has been proposed to include flame straining effects in the PCM-FPI method developped at CORIA-CNRS. The new model overcomes the problem associated with classical PCM-FPI closure to model kernel quenching due to intense local turbulence. Computations are done including the flame straining effects and the effect brought by the new model on kernel development is analysed in detail.

Bulk commercially pure titanium was prepared by powder metallurgy, namely by cryogenic milling and spark plasma sintering, with aim to produce ultra-fine grained material with enhanced strength. The microstructure of milled powders was investigated in detail by a novel method called transmission EBSD, which allowed the first direct observation of texture within the powder particles. This texture is similar to rolling texture, because of the similar nature of the defor- mation during milling. Microstructure observations revealed grains with the size under 100 nm. The influence of sintering parameters on material properties were studied by scan- ning electron microscopy including EBSD, X-ray diffraction and by microhardness measurements. The trade-off relationship between porosity and grain size was identified, fully dense material with ultra-fine grained microstructure could not be produced. Increased oxygen content was identified as a main strengthening factor, while porosity has significant deteriorating effect on mechanical properties. The texture of powder was retained in the bulk material. The possibility of stabilizing the microstructure by mechanical alloying of Ti with yttrium oxide nanoparticles was investigated with mixed results. The stabiliza- tion was successful, but several issues...