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.

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...

Ionic conductivity of metal oxides is critical for the function of a broad range of different components, such as electrolytes in solid oxide fuel cells and alloys designed for high temperature applications. In both cases the ionic conductivity can be studied by in situ impedance spectroscopy, which is also able to reveal information on the dielectric properties of the metal oxides, and in some cases the influence of their microstructure. The focus of this thesis is on impedance spectroscopy measurements of α-alumina in the temperature range 400-1000 °C. This metal oxide has found extensive use as the protective scale on heat resistant alloys. Some unpublished work on oxygen ion conductivity of yttria-stabilized zirconia is also included. The low electrical conductivity of α-alumina can be a source for errors and misinterpretations during impedance spectroscopy measurements. A major disturbance originates from leakage currents that appear in the experimental setup. These leakage currents are due to conduction through the gas phase around the sample, conduction on the sample surface, or poor insulation in the sample holder. It was shown that below 700 °C, conduction on the sample surface could severely distort the measurement. The magnitude of the distortions appeared to be sensitive to the type of electrodes used. The use of a so-called guard electrode was shown to effectively block the surface conduction in the measurements. Conductivity of metal oxides is known to be dependent on their microstructure. Generally it is believed that ionic conductivity is favoured along grain boundaries and dislocations. The influence of microstructure on conductivity was studied for α-alumina in the temperature range 400-1000 °C. The conductivity of a series of highly pure and dense samples with narrow grain size distributions was measured by impedance spectroscopy. It appeared that the activation energy for conduction increased with decreasing grain size. Results based purely on impendence spectroscopy have some inherently weaknesses. For instance no information on the nature of the charge carrier can be found. Therefore the charge transport in single crystalline α-alumina was simulated by the molecular dynamics method. The results from the simulation were then compared to results from impedance measurements on single crystalline α-alumina. From the simulation it turned out that diffusion of aluminium ions had lower activation energy than diffusion of oxygen. The activation energy of oxygen was close to the measured activation energy, and the mobility of oxygen was higher than for aluminium. Therefore the dominating charge carrier was suggested to be oxygen ions.

Oxid uraničitý (UO2) je v současnosti nejčastěji používaným materiálem jakožto palivo v komerčních jaderných reaktorech. Největší nevýhodou UO2 je jeho velmi nízká tepelná vodivost, a protože se při štěpení UO2 v jaderném reaktoru vytváří velké množství tepla, vzniká v UO2 peletě velký teplotní gradient. Tento teplotní gradient způsobuje vznik velkého tepelného napětí uvnitř pelety, což následně vede k tvorbě trhlin. Tyto trhliny napomáhají k šíření štěpných plynů při vysoké míře vyhoření paliva. Tvorba trhlin a zvýšený vývin štěpného plynu posléze vede ke značnému snížení odolnosti jaderného paliva. Tato práce se zabývá problematikou zvyšování tepelné vodivosti jaderného paliva na modelu materiálu (CeO2). V této práci jsou studovány podobnosti chování CeO2 a UO2 při konvenčním slinováním a při „spark plasma sintering.“ Způsob jak zvýšit tepelnou vodivost použitý v této práci je včlenění vysoce tepelně vodivého materiálu, karbidu křemíku (SiC), do struktury CeO2 pelet. Od karbidu křemíku je očekáváno, že zvýší tok tepla z jádra pelety, a tím zvýší tepelnou vodivost CeO2. V této práci je také porovnávána podobnost chování SiC v CeO2 matrici s chováním SiC v UO2, které bylo popsáno v literatuře.

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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]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/90395