No description available.

No description available.

The compressive creep behaviour of a high purity silicon nitride ceramic with and without the addition of Ba was studied at 1400°C. Two distinct creep stages were observed during high temperature deformation of these materials. The stress exponents for creep of the two materials indicate that they have different creep mechanisms during the second stage of creep. Cavitation during creep was determined by measuring the density change before and after creep using a water­-displacement method. The Ba doped material exhibited an obvious density decrease, indicating cavitation during creep, whereas the undoped material exhibited no cavitation. This is consistent with TEM observations. The microstructure of the materials, especially the amorphous grain-boundary phase was investigated for both as-sintered and crept specimans by means of transmission electron microscopy (TEM). Statistical analysis of a number of grain-­boundary films indicates that the film thickness is confined to a narrow range (standard deviation less than 0.15 nm) in the as-sintered materials. The average film thickness depends on film chemistry, increasing from 1.0 nm to 1.4 nm when Ba is added. The standard deviation of the film thickness of a given material after creep, however, is considerably larger than before (0.30 nm ~ 0.59 nm). This suggests that the grain-boundary glass phase is redistributed during creep. Viscous flow of the glass phase is proposed as die mechanism responsible for the first stage of creep. The data are compared with a model for viscous creep, yielding good correlation. / Thesis / Master of Engineering (ME)

The performance advances of radar-guided missiles have created a need for radome materials with improved strength, toughness, and thermal shock capabilities. Zirconium phosphate bonded silicon nitride (Zr-PBSN), which has a low and thermally stable dielectric constant, high rain erosion resistance and a low-cost processing method, has been developed for radome applications in advanced tactical missiles. Pressureless sintering reduces processing costs, but is untried for radome manufacturing. The tendency for catastrophic failure requires that each radome fabricated with this material/method be inspected for defects prior to use. Visible, thermographic and ultrasonic nondestructive evaluation (NDE) methods have been tested with Zr-PBSN discs containing fabricated flaws likely to be present in a radome. Ultrasonic C-scanning using a 0.25" diameter, 15 MHz focused transducer with a pulse-echo configuration was clearly superior at detecting cracks, delaminations, impurities, voids and porosity variation. A method for determining local porosity via the longitudinal elastic wave velocity was developed and can be incorporated into an ultrasonic scanning system. A system that uses a computer to perform all motion control, data acquisition, and data manipulation, but requiring a skilled operator for scan setup and interpretation of the data has been proposed. / Master of Science

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Lors de ce travail nous avons étudié la synthèse de nitrure de silicium en utilisant des décharges magnétron Ar/NH3 et Ar/H2/N2. Nous nous sommes intéressés particulièrement à la caractérisation de la décharge. Le paramètre de diagnostic le plus utilisé pour caractériser une décharge magnétron est la mesure de la tension de décharge, mais ces mesures ne donnent qu’une vue partielle du processus de pulvérisation même si le régime de pulvérisation peut être défini :métallique ou réactif. En effet, aucune information chimique ne peut être extraite des courbes de tension: d’autres techniques d’analyse sont donc indispensables. Nous avons utilisé la spectroscopie des photoélectrons X (XPS) pour analyser la chimie de la surface de la cible et la spectroscopie d’émission optique (OES) pour analyser la phase gazeuse.<p>La combinaison des mesures de tension et XPS a permis de mettre en évidence l’empoisonnement de la surface de la cible, consécutif à la formation d’une couche de nitrure de silicium lors de la pulvérisation dans un mélange Ar/NH3. Dans le cas du mélange Ar/H2/N2, les mesures de tension ne permettent pas avec certitude de confirmer un empoisonnement de la cible, néanmoins les mesures XPS mettent en évidence, comme pour le mélange Ar/NH3, la présence d’une couche de nitrure de silicium. Les mesures OES ont permis de détecter les mêmes espèces dans les deux types de mélange gazeux, seule l’espèce NH n’a pas été détectée dans le mélange Ar/H2/N2. Parmi les espèces détectées, certaines sont directement pulvérisées de la cible; il a été possible de relier l’intensité de celles-ci avec l’état de surface de la cible dans le cas du plasma Ar/NH3.<p>Nous avons également étudié l’instabilité du processus de pulvérisation en combinant des mesures de tension, OES et XPS. Avec une vitesse de pompage de 230 l/s, nous avons observé une très faible hystérèse de la tension pour les deux types de mélange gazeux. Dans le cas du plasma Ar/NH3, nous avons pu mettre en évidence que la bande de l’espèce NH peut être utilisée comme paramètre de contrôle de la décharge. Finalement, nous avons caractérisé les films obtenus par XPS et spectroscopie infrarouge. La stoechiométrie des films déposés va dépendre de la quantité d’ammoniac ou d’azote injecté dans la décharge, les films déposés avec NH3 sont contaminés par quelques pourcents d’oxygène alors que ceux déposés avec le mélange Ar/H2/N2 en sont dépourvus. / Doctorat en Sciences / info:eu-repo/semantics/nonPublished

<p dir="ltr">Antennas are used to transmit communication signals for many applications including for the navigation of aircraft. To protect the antennas from environmental conditions electromagnetic transparent structures called radomes are used. Advancements in technology have led to the development of hypersonic flight vehicles. These aircraft travel at speeds of Mach 5 and greater subjecting them to extreme environmental conditions. These aircraft require precise navigation making it important to have radome materials that can withstand the extreme conditions of high-speed flight while maintaining transparency to the incoming and outgoing signals of the antenna. Silicon nitride is a ceramic material of interest for high temperature radomes due to its mechanical properties, temperature stability, and satisfactory dielectric properties. Incorporating porosity into silicon nitride further enhances the transmission performance making porous silicon nitride a leading candidate material for high temperature radomes. In this dissertation slip casting with pressureless sintering is proposed as a route to fabricate porous silicon nitride ceramics for radomes. Modification of sintering aids and sintering temperatures are explored as a method to control the amount of porosity. Mechanical properties and dielectric properties of these materials are investigated. </p><p dir="ltr">First, an aqueous silicon nitride suspension developed for slip casting was optimized by investigating the rheological properties, zeta potential, and sedimentation behavior. It was determined that a suspension with 30 vol% solids, 0.5 wt% dispersant (PEI), and a pH of 7 was the optimized condition that resulted in uniform cast parts. This optimized suspension was used to fabricate silicon nitride samples with yttria and alumina sintering aids. An average density of 93% with an average strength of 659 MPa at room temperature and a strength of 472 MPa maintained up to 1200°C was achieved. Dielectric constant and loss tangent were measured on samples with 4-17% porosity to be 5.85-7.70 and <0.02, respectively. </p><p dir="ltr">To create samples with higher levels of porosity and therefore lower dielectric constants the yttria and alumina sintering aids were replaced with ytterbium oxide. Ytterbium oxide assists in forming porous silicon nitride due to the high melting temperature and high viscosity of the resulting glassy phase. Slip cast samples with 5% Yb₂O₃ were sintered at temperatures of 1700-1850°C resulting in porosities of 21-32% and strengths of 267-445 MPa. The dielectric constants of these materials were measured to be 4.56-5.80 with average loss tangents <0.006. The amount of ytterbium oxide was also studied to determine the effects on density, microstructure, mechanical properties, and dielectric properties. Slip-cast samples with 5-15% Yb₂O₃ were made having average porosities of 23-36% and strengths of 275-421 MPa. The dielectric constants of these materials were measured to be 4.13-4.65 with average loss tangents of <0.007. </p><p dir="ltr">Lastly, slip casting using the previously developed and evaluated suspensions was done to fabricate various radome shapes as well as layered structures. The processing method presented in this dissertation shows the potential for fabricating porous silicon nitride for high temperature radome applications with controlled porosity and relatively high strengths.</p>

Filmes finos de nitreto de silício com excesso de nitrogênio foram depositados sobre silício por sputtering reativo para obter estruturas emissoras de luz. As amostras foram modificadas por implantação iônica para verificar a influência dos dopantes arsênio (As) e boro (B) nos espectros de fotoluminescência (PL). As medidas de PL foram realizadas na faixa de temperatura entre 15-300 K e apresentaram uma emissão entre os comprimentos de onda 370-870 nm. Os dopantes introduziram uma emissão em 725 nm na banda de emissão, principalmente as dopadas com As. Foram realizadas medidas de microscopias para verificar a presença de nanoestruturas assim como a distribuição dos dopantes no material. As imagens de microscopias confirmaram a presença de nanocristais de nitreto de silício nas fases α, β e γ e identificaram a presença do dopante B nas fases cristalinas. O modelo de condução de Pool-Frenkel domina o transporte de portadores, indicando que a condução ocorre pelos níveis intrabandas, característica que definiu o modo que as recombinações radiativas ocorreram. As medidas de eletroluminescência (EL) apresentaram uma emissão centrada nos comprimentos de onda 760 e 880 nm (polarização negativa) e 1010 nm (polarização positiva) revelando diferenças significativas quando comparadas com as medidas de PL. Essa diferença esta associada à maneira como os elétrons populam os níveis intrabanda (excitação óptica para PL e elétrica para EL) que resulta em recombinações radiativas em diferentes comprimentos de ondas. A intensidade dos espectros de EL manifestou uma dependência quase linear com a densidade de corrente para ambas as polarizações. As medidas de EL em campos alternados exibiram um espectro de emissão composto pela soma das bandas obtidas separadamente em cada uma das polarizações. Medidas de EL em diferentes temperaturas (50-300 K) foram realizadas para investigar a influência da temperatura nos processos de recombinação radiativa. A intensidade exibiu uma redução com o aumento da temperatura, devido ao aumento do acoplamento elétron-fônon. / Silicon nitride with excess of nitrogen thin films were deposited on silicon substrate by reactive sputtering in order to obtain light emitting structures. Samples were modified by ion implantation of arsenic (As) and boron (B) to ascertain dopant leverage at photoluminescence (PL) spectra. PL measurements were performed at temperature ranging from 15 K up to 300 K and showed a band emission between wavelength 370 and 870 nm. An emission centered at 725 nm was observed in doped samples; especially in the presence of As. Microscope images showed crystalline structures of α-Si3N4, β-Si3N4 and γ-Si3N4 and confirmed boron dopant in nanocrystalline structures. Pool-Frenkel conduction model dominates electron transport in non-stoichiometric silicon nitride films due to intraband levels, phenomenon that has a huge contribution to electroluminescence (EL) emission. EL signals were composed by two peaks centered at 760 and 880 nm (negative bias – EL-N) and one peak at 1010 nm (positive bias – EL-P). Diffences between PL and EL spectra exhibit a clear dependence on the mode of excitation (photo and current source) on radiative recombination process. EL intensity had almost a linear increase with current density for both polarizations. EL measurements under AC voltage were composed by a superposition of the signals from EL-N and EL-P signals. Photo and electroluminescence measurements were collected at different temperatures (50 to 300 K) in order to investigate the temperature influence on the radiative recombination. The EL intensity was decreasing with temperature increasing, due to electron-phonon interactions.

Zhang Ailing. / "September 2004." / Thesis (Ph.D.)--Chinese University of Hong Kong, 2004. / Includes bibliographical references. / Electronic reproduction. Hong Kong : Chinese University of Hong Kong, [2012] System requirements: Adobe Acrobat Reader. Available via World Wide Web. / Mode of access: World Wide Web. / Abstracts in English and Chinese.

Abstract not available