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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)

Metallic materials play important roles in providing electrical, thermal, and mechanical functions in electronic devices and systems. The understanding of the electrical-thermal-mechanical interaction caused by the passage of electric current with high density is important to improve the performance and reliability of electronic assembly and packaging. The electromechanical interaction on the deformation behavior of copper and tin is studied in this work. The electromechanical response of Cu strips was studied by passing a DC electric current. The electric resistance linearly increased with time before the occurrence of electric fusing. The electrothermal interaction led to the buckling of the Cu strips with the maximum deflection increasing with the increase of the electric current density. The total strain was found to be proportional to the square of the electric current density. A power law relation was used to describe the dependence of the time-to-fusing on the electric current density. Using the nanoindentation technique, the effect of electric current on the indentation deformation of copper and tin was studied. The reduced contact modulus of copper and tin decreased with increasing the electric current density. With the passage of a DC electric current, the indentation hardness of copper increased slightly with increasing electric current density. With the passage of an AC electric current, the indentation hardness of copper decreased with increasing the indentation deformation. With the passage of a DC electric current, the indentation hardness of tin decreased with increasing the indentation load, showing the normal indentation size effect. Both the limit of infinite depth and the characteristic length were dependent on the electric current density. Using the tensile creep technique, the creep deformation of pure tin was studied with the passage of a DC electric current. The steady state creep rate increased with the increase in temperature, tensile stress and electrical current density. For the same tensile stress and the same chamber temperature, the steady state creep rate increased linearly with the square of the electric current density. The electric current density has no significant effect on the stress exponent and activation energy of the tensile creep of tin for the experimental conditions.

Creep resistance is an important design criterion at high temperatures especially when continuous attempts are made to increase the efficiencies by increasing the operating temperatures. Alumina is an important high temperature material and in addition to that it is used in wide variety of applications such as substrates for electronic packaging, spark plugs, envelopes for sodium vapour lamps, cutting tools (when reinforced with silicon carbide) and in artificial joint prostheses. Studies on creep in alumina. have started as early as 1961. There are differing mechanisms proposed to explain the creep behaviour of alumina in the literature, but until now there is no any unanimous decision as to what the rate controlling mechanism is. Magnesia doped at ppm levels can produce significant changes in the microstructure of alumina, the most important consequence of that being the grain growth inhibition, which renders alumina superplastic. However, in a stoichiometric oxide like alumina, small impurities can create extrinsic defects which would change the diffusivities and creep rates. Therefore the background impurities in alumina should be kept to a minimum, if small dopant effects have to be studied. The present study was undertaken making use of high purity alumina powder and comparing the grain growth and creep properties of pure and magnesia doped alumina, especially since no such investigation was carried out in the recent past with high purity alumina. Pure alumina was processed by cold compaction followed by cold isostatic pressing (CIP) and pressureless sintering in air at 1773 K for 1 hour. Magnesia doped alumina was prepared by calcining a mixture of alumina and magnesium nitrate at 973 K for 2 hours followed by cold compaction, CIPing and pressureless sintering in air at 1773 K. Both pure and magnesia doped alumina were further annealed at 1873 K for various times to get grain sizes in the ranges of 1-5 μm. Grain growth kinetics of pure and magnesia doped alumina were studied at 1823 and 1873 K. The parameter Kg which quantifies the mobility of the grain boundary was got. It was found that Kg had decreased in the magnesia doped alumina (in comparison with pure alumina) by a factor of about 3 to 4 which was marginal and insignificant. The grain sizes followed a log normal distribution in both the cases, indicative of normal grain growth. Creep studies were conducted on pure and magnesia doped alumina in three modes, namely, constant stress, temperature jump and stress jump test. The temperature range used was 1673 to 1773 K and the stress range used was 10 to 100 MPa. The creep parameters were found to be n~1.6, p~3.7 and Q-545 kJ mol"1 for pure alumina and n~l .3, p~3.0 and Q~460 kJ mol-1 for magnesia doped alumina. The creep rates in the case of magnesia doped alumina were found to have increased by a factor of 2 to 3, in comparison with pure alumina. The increase in creep rates were found to be insignificant. The creep data were analyzed and the possibility of the dislocation and interface reaction controlled creep mechanisms were ruled out since they were inconsistent with the data. It was found, from creep parameters and the comparison of theoretical Coble and Nabarro-Herring creep rates with the experimental rates, that Coble creep might be rate controlling. The activation energy values suggested that aluminium ion diffusing along grain boundary might be the rate controlling species. However, when the theoretical creep rates considering various species were compared, the rate controlling species turned out to be oxygen ion diffusing along the grain boundary.

With the purpose of studying the mechanical properties of uncompacted rockfill and the creep deformation behaviour of rockfill under a load as well as finding a suitable method for estimation of creep deformation behaviour, a full scale embankment loading experiment was performed. The results of this experiment were then evaluated. During the course of this study it became evident to the author that the deformations which were seen in the collected data from the experiment could be classified as creep deformations due to the linear decrease of the deformation against the logarithm of time and the study therefore came to focus on creep. One constitutive equation and one model for estimation of creep deformations were studied, and parameters were obtained through back analysis of experiment data as well as calculation of soil stresses. The creep model was based on a logarithmic approximation of the creep deformations and the creep equation was based on a power function. The creep model could also be simplified and evaluated as an equation and when a comparison was made between the equations and the measured results this showed that the logarithmic equation resulted in estimates closer to the measured deformations than what the power function did, therefore a logarithmic function is a better approximation to the deformations of the rockfill at Norvik than the power function. When the creep model was evaluated as intended, based on the soil stresses, the resulting creep estimates were less accurate, they was however still within the limits of what can be considered as admissible. The conclusion is that a logarithmic function describes the creep deformation of the rockfill at Norvik better than a power function and that the creep model by Kristensen is suitable for estimating the creep deformations. This since the creep model also provides a way of estimating deformations occurring under stress conditions other than the ones for which the creep test was performed.

L'assiette de fibrage utilisée pour la production de la laine de verre d'isolation subit à haute température de nombreuses contraintes (chimiques, mécaniques et thermiques). La ruine des assiettes peut être due à l'oxydation par les gaz chauds, à la corrosion par le verre fondu ou à la déformation par fluage. La première partie des travaux de thèse a porté sur l'amélioration des propriétés mécaniques des alliages pour le fibrage à 1200°C. Dans un premier temps, la teneur en chrome au coeur d'alliages à base de cobalt a été réduite afin d'augmenter la réfractarité en conservant la microstructure. Cependant, cette réduction a dégradé le comportement en oxydation de ces alliages. Afin de conserver un bon niveau en oxydation, un enrichissement en chrome de la surface a été réalisé à l'aide de la technique de pack-cémentation. Le comportement en fluage de ces alliages a été maintenu à un niveau correct. Dans un second temps, de nouveaux systèmes métallurgiques ont été explorés, basés sur le nickel et le fer, et ont été renforcés mécaniquement par des éléments lourds en solution solide ou par des précipités intermétalliques. La réfractarité et le comportement en oxydation se sont révélés intéressants mais la tenue en fluage a été décevante. La seconde partie de ces travaux a consisté à améliorer le comportement en oxydation de l'alliage utilisé lors du fibrage à 1000-1050°C. Deux voies ont été explorées : un enrichissement en chrome de la surface de l'alliage par pack-cémentation ou l'addition d'un élément réactif, l'yttrium. La seconde solution a apporté des résultats intéressants avec une amélioration significative du comportement en oxydation cyclique / The spinner used to product glass wool for thermal building insulation undergoes several stresses (chemical, mechanical and thermal) at high temperature. The lifetime of the spinner is limited by oxidation by hot gases, corrosion by molten glass or creep deformation. The first part of this thesis has concerned the improvement of the mechanical properties of the alloys for the fiberizing at 1200°C. First, the bulk chromium content of the usual cobalt-base alloys has been decreased to increase their refractoriness at constant microstructure. However, this reduction has degraded the oxidation behavior of these alloys. To keep a good oxidation behavior, a surface chromium enrichment of the Cr-impoverished alloys is achieved by pack-cementation technique. The creep behavior of these alloys is kept at a good level. Secondly, several new metallurgical systems were explored: alloys based on nickel and iron and reinforced by heavy elements in solid solution or by precipitates inter metallic particles. The refractoriness and the oxidation behavior appeared to be interesting but the creep deformation was disappointing. The second part of this work has concerned the improvement of the oxidation and corrosion properties of the alloys for the process at 1000-1050°C. Two ways have been explored: a chromium enrichment on the sub-surface or an addition of a reactive element, as yttrium. The second solution has given interesting results with a significant improvement of the oxidation behavior, and particularly in cyclic oxidation

Die im Rahmen des Sonderforschungsbereiches SFB 920 entstandene Arbeit beschäftigt sich mit bruchmechanischen Vorgängen und der makroskopischen Beschreibung von offenzelligen Keramikschäumen unter Berücksichtigung des Materialverhaltens des Kompaktmaterials mithilfe von numerischen Simulationen. Dabei steht die thermomechanische Belastung einer solchen Struktur während eines Gießprozesses im Vordergrund. Im Rahmen der bruchmechanischen Untersuchungen konnte der Einfluss von verschiedenen Strukturparametern aufgezeigt werden. Die Belastungen entlang der scharfen Kerben im Inneren der Stege ergaben sich dabei als weniger kritisch als entlang der Stegaußenseiten. Das Kriechverhalten des kohlenstoffgebundenen Aluminiumoxides bei Hochtemperatur konnte erfolgreich beschrieben und für Schaumstrukturen angewendet werden. Das vorgeschlagene Modell kann dabei sowohl für virtuell erzeugte Schaumstrukturen als auch für reale Schaumproben angepasst werden. Mithilfe von homogenisierten Materialmodellen basierend auf neuronalen Netzen ergab sich eine drastische Reduzierung der Rechenzeit für komplexe Filterstrukturen. Es ist dabei eine Berücksichtigung von Plastizität und Schädigung für das Kompaktmaterial möglich. / This thesis developed within the collaborative research centre SFB 920 deals with fracture mechanical analyses and the macroscopic description of open-cell ceramic foams considering the material behaviour of the bulk material by means of numerical simulations. In the centre of interest is the thermomechanical loading of such a structure during a casting process. Within the framework of fracture mechanical investigations, the influence of various structural parameters is demonstrated. The loads along the sharp notches inside the struts turned out to be less critical than along the outer surfaces of the struts. The creep behaviour of the carbon-bonded alumina at high temperature were successfully described and the mathematical description is applied to foam structures. The proposed model can be adapted for virtually generated foam structures as well as for real foam samples. Using homogenized material models based on neuronal networks, a drastic reduction of the computing time for complex filter structures was achieved. Meanwhile, it is possible to consider plasticity and damage effects for the bulk material.