Thesis (M.S.)--University of Texas at El Paso, 2009. / Title from title screen. Vita. CD-ROM. Includes bibliographical references. Also available online.

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Thesis (MTech (Mechanical Engineering))--Cape Peninsula University of Technology, 2005 / The objective of this project was to monitor the high temperature creep behaviour of 441 stainless steel. Two different alloys of 441 were investigated; the main difference between them being the Niobium content. Particularly imporlant to the project was how the Niobium content and grain size affected the creep resistance of the material. Creep tests were performed using purpose built constant load creep test rigs. Initially the rigs were not suitable for the testing procedures pertaining to this project. This was due to persistent problems being experienced with regards the reliability and reproducibility of the rigs. After various modifications were made the results produced from the rigs were consistent. Creep test data was used in order to determine the mechanism of creep that is operative within the material (at a predetermined temperature) under a predetermined load. Particular attention was paid to the resulting stress exponents. in order to identify the operative creep mechanism. The identification of the operative creep mechanisms was also aided by microscopical analysis. This analysis was also necessary to monitor how the grain size had altered at various annealing temperatures. Heat treatment was used as a method to alter the high temperature strength and microstructure of the material. Heat treatments were performed at various temperatures in order to determine the ideal temperature to promote optimum creep resistance of 441. All heat treatments were performed in a purpose designed and built high temperature salt bath furnace. The commissioning of the salt bath formed part of the objectives for this project. Sag testing was also conducted, using purpose built sag test rigs. It was necessary to design and manufacture a sag test rig that could be comparable to the industry accepted method of sag testing known as the two-point beam method, as this method is believed to produce inconsistent results. Conclusions have been drawn from the results of the data and from previous research on the subject matter.

Made available in DSpace on 2014-10-09T12:55:44Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:05:13Z (GMT). No. of bitstreams: 0 / Avanços tecnológicos geram a necessidade de materiais com propriedades cada vez melhores, de acordo com a sua aplicação final. Compósitos de alumina com adição de partículas de carbeto são uma opção promissora de aplicação estrutural. Neste trabalho foi estudada a influência da diferença de distribuição e tamanho de partículas de duas aluminas comerciais, a adição de 1,5 e 6% em volume de carbeto de nióbio e a adição de 500 ppm de óxido de magnésio, nas propriedades microestruturais e mecânicas de compósitos à base de alumina. Foram preparados corpos de prova por prensagem uniaxial e isostática, sinterizados em forno de resistência de grafite a temperaturas de 1600, 1650, 1700 e 1750°C, por trinta minutos, em atmosfera com pressão positiva de argônio. As amostras obtidas foram avaliadas quanto à densidade, microestrutura e propriedades mecânicas. Também foram realizados ensaios de difusão para verificar a reatividade química entre pares formados por amostras de alumina e ferro fundido cinzento. As características físicas e químicas das aluminas comerciais utilizadas acarretaram diferenças nos materiais finais; os compósitos produzidos com alumina A16 apresentaram densidade maior do que os produzidos com alumina A1000, nas mesmas condições; assim como os valores de dureza também foram maiores. A adição de 6vol% de carbeto de nióbio à matriz de alumina retarda o início da sinterização, enquanto que a adição de 1,5vol% não provoca mudanças sensíveis na cinética de densificação em relação aos materiais sem adição. Os valores de densidade e dureza dos compósitos contendo 1,5vol% de NbC foram superiores nas menores temperaturas de sinterização utilizadas. Os melhores resultados de densificação (>96% Dt) e dureza (>15GPa) foram obtidos para compósitos produzidos com alumina A16 e adição de 1,5% de NbC. / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Les mécanismes de déformation plastique des matériaux cubiques à corps centré sont étudiés depuis plus d’un demi-siècle. Il est maintenant bien établi que les dislocations vis contrôlent la plasticité de ces matériaux. Ceci est dû à une structure non-plane du cœur de ces dislocations, qui induit une forte friction de réseau communément appelée ‘pseudo-Peierls’. Le mécanisme supposé est la nucléation thermiquement activée de paires de décrochements. Cette structure de cœur particulière limite également les plans de glissement possibles. Les traces de glissement aux échelles méso et microscopiques apparaissent ‘ondulées’, ce qui a amené à proposer toute une variété de plans de glissement.Dans ce contexte, nous avons analysé à une échelle plus fine, i .e. à l’échelle atomique, les traces de glissement obtenues par déformation en compression de monocristaux de niobium à des températures situées dans le régime de température thermiquement activé: 293 K, 200 K et 90 K. L’analyse par microscopie à effet tunnel sous environnement ultra vide indique qu’à la résolution atomique chaque trace de glissement peut être décomposée en segments associés à des plans de type {112} et {110}. De manière surprenante, il est mis en évidence qu’à 293 K et 200 K du glissement se produit à la fois dans le sens maclage et antimaclage. De plus, toutes les traces de glissement impliquent du glissement sur des plans de type {110}, étayant ainsi la structure de cœur compact prévue par simulations atomistiques ab initio.L’étude in situ de la surface sous contrainte, à T = 293 K et 200 K, a aussi mis en évidence des réorganisations, voire des disparitions, de terrasses atomiques au voisinage de dislocations émergentes. Le calcul des forces d’interaction en élasticité linéaire isotrope montre que les dislocations proches de ces terrasses ne jouent pas de rôle prépondérant sur la position d’équilibre des terrasses. En revanche, celles-ci modifient localement le potentiel chimique de surface, favorisant la diffusion atomique à l’origine des réorganisations de surface constatées expérimentalement. / The plastic deformation of body-centred cubic metals is the subject of extensive studies since more than half a century. It is now well established that the screw dislocations control the plasticity of these metallic metals. The reason for this is attributed to a non-planar configuration of the core of these dislocations, which induces a high friction force usually referred to as ‘pseudo-Peierls’. The underlying elementary mechanism is the thermally activated nucleation of kink pairs. While perfect screw dislocations do not have specific glide plane, the non-planar core configuration limits the number of possible slip planes. The slip traces observed at the meso and microscopic scales are wavy, which has leaded to the proposal of several possible slip planes.In this context, we propose an analysis at a finer scale, i.e. the atomic scale, of the slip traces produced by compressive stress on niobium single crystals at three temperatures in the thermally activated temperature regime, namely: 293 K, 200 K and 90 K. The analyses were carried out using a scanning tunnelling microscope under ultra-high vacuum environment. At this scale of observation, the slip traces are made up of crystallographic segments that can be associated with {011} and {112} planes. It is also noticeable that at 200 K and 293 K dislocation glide is observed in both the twinning and the anti-twinning directions. More importantly, all slip traces include segments that belong to {011} planes strongly supporting the latest ab initio atomistic simulations predicting a compact core configuration for screw dislocation.In this study, we also established that, at T = 293 K and 200 K, the sample surface may undergo drastic changes of its vicinal terraces, when they are close to emerging dislocations. The calculation of interaction forces, in the frame of isotropic linear elasticity, indicates that dislocations close to vicinal terraces do not play a major role regarding the stable positions of the vicinal terraces. However, they locally modify the chemical potential of the surface, thus enhancing atomic diffusion which is at the origin of the surface reorganisations experimentally observed.

No description available.

The research work presented in this thesis reports for the first time the fabrication of Titanium Niobium complex oxide (TiNb2O7 (TNO)) thin films by employing pulsed laser deposition and their use as the anode material in Li-ion micro batteries. Chapter 1 provides a brief introduction to complex metal oxides as multifunctional materials. In the first section of this chapter, a brief introduction is given about the history of TNO complex oxide material. The complex structure and properties of TNO oxide are also discussed briefly. In the second section, the importance and need of thin film batteries in emerging applications is discussed. Finally, the specific objectives of the current research are outlined in the last section. Chapter 2 gives the details about various experimental methods and characterization tools used in this research. The first part gives a brief overview about the principles and the use of different experimental methods involved in the growth of TNO thin films using pulsed laser deposition. Details, including the laboratory setup designed for PLD growth, also described briefly. In the second part, the different state-of-the-art characterization tools used in this research are described in terms of their principles and their applications such as measuring structural, morphological, chemical and electrochemical properties. Chapter 3 describes the synthesis and characterization of TNO bulk targets prepared via solid state reaction. In the first part, the detailed descriptions of experimental conditions are given. In the second part, the study of as-prepared TNO targets by various characterization tools such as XRD, Raman, SEM and XPS for understanding its structure, morphology and chemical properties are discussed briefly. The emphasis is made on the preparation of a quality target by careful observations. Chapter 4 mainly describes the comprehensive studies carried out on the fabrication and characterization of TNO thin films using PLD. In the first part, the preliminary experimental conditions for the growth of TNO thin films on Pt (200)/TiO2/SiO2/ Si (100) substrates are explained briefly. The importance of primary understanding about target-laser interaction through the structural, morphology changes observed by various characterization tools is discussed. In the latter part of the chapter, the effects of systematic variation of deposition parameters on the properties of the grown TNO thin films are described extensively. Various advanced characterization tools are used to study the changes in as-grown TNO thin films in terms of their structural, morphological and chemical changes by various advanced characterization tools. Chapter 5 is an account of the state-of-the-art characterization tools that are used on the as-grown TNO thin films for determining structural, compositional and elemental information with nanometer spatial resolution. In the first part, the effects of various processing conditions used during FIB are discussed briefly, along with observed results. An attempt has been made to solve the experimental difficulties during FIB for cross sectional sample preparation for HRTEM analysis. Later, the imaging, diffraction and spectroscopic studies carried out on TNO thin films using HRTEM, STEM HAADF, and EDXS elemental mapping are discussed in detail. Finally, obtained results are correlated to the experimental conditions during PLD growth. Chapter 6 focuses on the usage of as-grown TNO thin films as a new anode material in rechargeable Li-ion micro batteries. The various experimental details, battery cell fabrication, etc are described in the first part of the chapter. Then the comprehensive studies are carried out for demonstrating TNO thin films as anode material in micro batteries. Besides this, the basic cyclic voltammogram and charge-discharge tests carried out on a TNO electrode are discussed in detail. The structural, morphological studies are done before and after the electrochemical cell reaction to understand the crystal stability of TNO as an anode electrode. The effects of important experimental parameters on their electrochemical properties are also described briefly. Finally, the observed results are compared with existing literature. Chapter 7 summarizes the present research reported in this thesis and discusses the future research that could give insight into the understanding and optimization of TNO thin films for better usage in battery applications.

Niobium and rare earth elements (REE) are considered as strategic metals in industrialised countries, and are mainly derived from carbonatite-related deposits. Indicator mineral methods for carbonatites using of portable XRF and Quantitative Evaluation of Materials by Scanning Electron Microscopy (QEMSCAN®), shows promise in exploration for Nb and REE. Portable XRF analysis of stream sediments from the Aley, Lonnie, and Wicheeda carbonatites identified 125-250 μm as the ideal size fraction for indicator mineral studies. QEMSCAN® provides (with no additional processing) detection and characterisation of indicator minerals (when found in high concentrations) from carbonatite deposits. Preconcentration by Mozley C800 separator is recommended for sediment samples with low concentrations of indicator minerals. Discrimination diagrams for pyrochlore supergroup and columbite-tantalite series minerals show that minerals from carbonatites occupy the pyrochlore field and extend slightly into the betafite field. Columbite-tantalite series minerals from carbonatites have Mn/(Mn+Fe) atomic ratios ≤0.25 and Ta/(Ta+Nb) ≤0.20. The compositional fields for pyrochlore supergroup and colubmite-tanatlite series minerals from different deposit types partially overlap. / Graduate / 0996 / 0411 / 0372

Materials with potential for high temperature inorganic pigment applications (e.g. ceramics) have been synthesised using solid state methods and characterised using powder X-ray and neutron diffraction, magic angle spinning NMR, Mossbauer spectroscopy, UVNis spectroscopy and colour measurement techniques. A number of compounds containing tin (H) and niobium (V) have been modified and doped with various constituents to tailor and widen the colour properties of the bright yellow parent phases. The dark yellow (L*(91.28), a*(13.74), b*(54.76)) tin niobium oxide pyrochlores have been re-characterised using neutron diffraction techniques. These materials exhibit both cation and anion disorder caused by a stereoactive lone pair on the tin (H) metal centres. Solid state NMR and Mossbauer studies have shown the presence of tin (IV) on a symmetric site within the primary phase of the pure oxide pyrochlore and methods have been investigated to minimise the tin (H) disproportion method from where the tin (IV) is derived.

Complexos de coordenação de Cu(II), Ni(II), Zn(II) e Nb(V) foram obtidos com os íons acetato, citrato e oxalato como ligantes (complexos ex-situ) para serem aplicados em banhos de eletrodeposição. O objetivo é usar estes complexos como fontes de metais sem adição de aditivos os quais são os ligantes que estão coordenados. Como estudos de referência, foram investigados banhos de eletrodeposição contendo sais de sulfatos dos íons metálicos na presença de ligantes nas razões metal:ligante de 10:1 e 1:5; assim, complexos de coordenações similares podem ser gerados em solução (complexos in-situ). Os complexos ex-situ foram analisados por análise elementar, espectroscopias nas regiões do infravermelho e ultravioleta-visível e voltametria cíclica (em Pt). As eletrólises foram realizadas em substrato de aço 1020 com um ou dois complexos metálicos presentes no banho. Banhos de eletrodeposição de nióbio usando como substrato aço 1020 coberto com Cu e/ou Zn foram bem sucedidos. Os depósitos foram analisados por microscopia eletrônica de varredura (MEV), espectroscopia de dispersão de raios X (EDX), reflectância difusa, espectroscopia de difração de raios X (DRX) e por curvas de polarização anódica (estudos de corrosão). Os banhos com complexos in-situ 10:1 fomeceram depósitos com aspectos morfológicos ruins em relação aos depósitos obtidos de banhos com complexos in-situ 1:5 e ex-situ. As morfologias dos depósitos obtidos dos banhos com acetato foram dendríticos e com baixa aderência. Os depósitos dos banhos com complexos citrato e oxalato foram lisos, compactos, com boa aderência e brilhantes. Diferentes fases estruturais foram observadas nos depósitos e a maioria deles protege contra a corrosão. Os estudos concluíram que os ligantes analisados influenciam diferentemente nos processos de eletrodeposição. / Cu(II), Ni(II), Zn(II) and Nb(V) coordination complexes were obtained with acetate, citrate and oxalate ions as ligands (ex-situ complexes) to be applied in electrodeposition baths. The aim is to use these complexes as metal sources without further addition of additives which are the coordinated ligands. As reference study, electroplating baths with sulfate salts of the metal ions in presence of the ligands were investigated in the metal:ligand ratio of 1:5 and 10:1; then, similar coordination complexes can be generate in solution (in-situ complexes). The ex-situ complexes were characterized by elemental analysis, infrared and UV-vis spectroscopies and cyclic voltammetry (in Pt). The electrolyses were performed in 1020 steel as substrate with one or two metal complexes present in the bath. Niobium electroplating baths with 1020 steel previously covered with Cu and/or Zn as substrates were also successfully performed. The deposits were analyzed by scanning electron microscopy (SEM), energy dispersive spectroscopy X-ray (EDS), diffuse reflectance, X-ray diffraction (XRD) and polarization curves (corrosion studies). The bath with 10:1 in-situ complexes provided deposits with poor morphologic aspects in relation to the deposits obtained from bath with 1:5 in-situ and ex-situ complexes. The morphologies of the deposits obtained from bath with the acetate complexes were dendritics and with low adherence. The bath with both citrate- and oxalate-complexes were smoothes, compacts, with good adherence and brightness. Different structural phases were observed in the deposits and the most of them provided protection against corrosion. It was concluded that coordinated ligands influence differently in the electrodeposition processes.