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The lithium disilicate (LS2) glass system provides the basis for a large number of useful glass-ceramic products. Microwave processing of materials such as glass-ceramics offers unique benefits over conventional processing techniques. Variable frequency microwave (VFM) processing is an advanced processing technique developed to overcome the hot spot and the arcing problems in microwave processing. In general, two main questions are addressed in this dissertation: 1. How does microwave energy couple with a ceramic material to create heat? and, 2. Is there a "microwave effect" and if so what are the possible explanations for the existence of that effect? The results of the present study show that VFM processing was successfully used to crystallize LS2 glass at a frequency other than 2.45 GHz and without the aid of other forms of energy (hybrid heating). Crystallization of LS2 glass using VFM heating occurred in a significantly shorter time and at a lower temperature as compared to conventional heating. Furthermore, the crystallization mechanism of LS2 glass in VFM heating was not exactly the same as in conventional heating. Although LS2 crystal phase (Orthorhombic Ccc2) was developed in the VFM crystallized samples as well as in the conventionally crystallized samples as x-ray diffraction (XRD) confirmed, the structural units of SiO4 tetrahedra (Q species) in the VFM crystallized samples were slightly different than the ones in conventionally crystallized samples as the Raman spectroscopy revealed. Moreover, the observed reduction in the crystallization time and apparent temperature in addition to the different crystallization mechanism observed in the VFM process both provided experimental evidence to support the presence of the microwave effect in the LS2 crystallization process. Also, the molecular orbital model was successfully used to predict the microwave absorption in LS2 glass and glass-ceramic. This model was consistent with experiments and indicated that microwave-material interactions were highly dependent on the structure of the material. Finally, a correlation between the Fourier transform infrared reflectance spectroscopy (FTIRRS) peak intensities and the volume fraction of crystals in partially crystallized LS2 glass samples was established. / Ph. D.

With this research, we work towards the overall objective of being able to accurately simulate fiber orientation in complex flow geometries of composite fluids of industrial significance. The focus of this work is to understand the rheological behavior of these materials and its connection to fiber orientation as determined in simple shear flow. The work includes the development of a novel approach to characterizing the transient rheology; an experimental study of the relationship between the stress growth functions in startup of flow and the fiber orientation; a critical assessment of the limitations of current fiber suspension theory; and an approach to determining unambiguous model parameters by fitting. A key difference between the rheological studies performed in this work and others is the use of a cone-and-plate device combined with "donut" shaped samples (CP-D) to prevent boundary effects on the measurement. The conventional method for obtaining transient rheological data is to use parallel disk (PP) geometry set at a gap where the measurements are independent of disk spacing. However, this work suggests that the inhomogeneous velocity gradient imposed by the PP geometry induces excessive fiber-fiber contact contributing to exaggerated measurements of the stress growth functions. An experimental study of the transient rheological behavior of a 30 wt% short glass fiber-filled polybutylene terephthalate was performed using the CP-D. Stress growth measurements during startup of flow were performed in combination with direct measurement of the fiber orientation to determine the relationship between the transient rheology and the fiber microstructure. The well defined fiber orientation and rheological experiments allowed for a quantitative assessment of current fiber suspension theory. Comparison between the experimental fiber orientation and predictions based on Jeffery's equation and the Folgar-Tucker model show that the fiber orientation evolves much slower than predicted. In addition, the addition of a "slip" term improved the agreement between the predictions and experimental results. Predictions using the Lipscomb model coupled with the Folgar-Tucker model, with slip, were fit to the transient stresses to determine the feasibility of fitting unambiguous model parameters for a specific composite fluid. Model parameters determined by fitting at a shear rate of 6 s-1 allowed for reasonable predictions of the transient stresses in flow reversal experiments at all the shear rates tested. / Ph. D.

This dissertation presents the first reported identification and analyses of the phase relations in the YBa2Cu3O7-x (YBCO)-SiO2 system at elevated temperatures. In this regard, a rigorous characterization study of the reaction phases within YBCO glass fibers, heat-treated YBCO+SiO2 pellets, rapid thermally annealed YBCO+SiO2 rods and rapid thermally annealed YBCO powder inside a fused silica tube is provided. These analyses are based on a vast set of generated novel results obtained using energy dispersive spectroscopy analyses on an environmental scanning electron microscope, X-Ray diffraction analyses, Raman spectroscopy, X-ray photoelectron spectroscopy analyses and a cross-polarized light study. First, original drawings of YBCO into glass fibers using the molten-core approach on a fiber draw tower in air and oxygen atmospheres are presented and analyzed. The performed analyses reveal the occurrence of reactions between the YBCO core and the silica cladding in as-drawn fibers as well as after additional heat-treatments. A detailed analysis and characterization of the occurring dissolution and diffusion based reaction processes is, then, provided along with the identification of the arising phase separation. Moreover, in order to analyze drawing YBCO glass fibers at lower temperatures, the use of borosilicate as the preform material is also investigated. This varied set of experiments and associated analyses reveal that the as-drawn YBCO fibers contain an amorphous core and that cuprite (Cu2O) is the first phase to crystallize out of the amorphous silicate matrix upon heat-treatment. Furthermore, the obtained results demonstrate the dissolution of the fused silica cladding into Si4+ and O2- ions and their subsequent diffusion into the molten YBCO core, leading to phase separation due to an occurring miscibility gap in the YBCO-SiO2 system as well as to silicate formation and amorphization of the YBCO core. This, as a result, prohibits the formation of the superconductive YBCO (Y-123) phase upon annealing. In addition, heat-treatment analyses show that higher temperatures or prolonged dwelling times at lower temperatures lead to the formation of barium copper and yttrium barium silicates. The analysis focusing on the use of borosilicate as the preform material reveals that drawing at lower temperatures reduces the dissolution and diffusion based reactions, but does not prevent them. Furthermore, the analysis on YBCO glass fibers with a fused silica cladding drawn in oxygen atmosphere shows that a higher oxygen content increases the dissolution of the fused silica cladding into its ions and their subsequent diffusion into the molten YBCO core. In addition, the performed heat-treatments on YBCO+SiO2 pellets in air and oxygen atmospheres demonstrate the gradual decomposition of the Y-123 phase with an increase in SiO2 content. Moreover, the rapid thermal annealing experiments with a subsequent quenching step on YBCO+SiO2 rods and on YBCO powder inserted inside a fused silica tube show the decomposition of the Y-123 phase and the formation of phases similar to the phases obtained in the YBCO glass fiber study, thus corroborating the results thereof. In summary, this dissertation enables the determination of the phase relations and reaction processes within the YBCO-SiO2 system, the identification of the direct effects of the silicon content on the Y-123 phase decomposition, as well as a rigorous characterization of the dissolution and diffusion based reactions within the YBCO-SiO2 glass-clad fiber system. The generated results and drawn conclusions build a fundamental understanding of phase relations in the YBCO-SiO2 system, which enables a definite assessment of the feasibility of manufacturing long-scale purely superconductive YBCO glass fibers using the molten-core approach and introduces advanced contributions to general glass-clad fiber systems manufactured using this method. / Doctor of Philosophy / This dissertation provides the first reported identification and analysis of the phase relations in the YBa2Cu3O7-x (YBCO)-SiO2 system at high temperatures. In this regard, a thorough characterization study of the reaction phases within YBCO glass fibers drawn using the molten-core approach on a fiber draw tower is provided. In addition, heat-treatment analyses considering YBCO+SiO2 pellets, rapid thermally annealed YBCO+SiO2 rods and rapid thermally annealed YBCO powder inside a fused silica tube are performed to gain further fundamental insights. The performed analyses are based on a wide set of characterization methods including energy dispersive spectroscopy on an environmental scanning electron microscope, X-Ray diffraction analyses, Raman spectroscopy, X-ray photoelectron spectroscopy and a cross-polarized light study. Our experimental results and performed analyses identify the phase relations and reaction processes within the YBCO-SiO2 system at elevated temperatures, demonstrate the direct effects of the silicon content on the superconductive YBCO phase decomposition, enable drawing definite conclusions regarding the feasibility of manufacturing long-scale purely superconductive YBCO glass fibers using the molten-core approach, and, characterize the dissolution and diffusion based reactions occurring within the YBCO-SiO2 glass-clad fiber system. In a nutshell, this dissertation provides a fundamental understanding of phase relations in the YBCO-SiO2 glass-clad system as well as key insights covering general glass-clad fibers drawn using the molten-core approach, paving the way for improved glass-clad fiber manufacturing using this method.

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The ancient glass collection of the National Museum has more than 200 completely intact and so far - beside few exceptions - unpublished vessels which encompass a wide chronological framework from the 5th century BC until the end of antiquity. The core of the collection is composed of mold-blown and free-blown glass. The analysis of the collection offers a view into the history of the ancient glass production; examples of all kinds of production methods can be found in it - from a corn-formed glass, through a glass made by sagging into a form, and up to a mold-blown and free-blown glass. A great number of various decoration techniques and styles used in antiquity are represented in the collection; also, it contains vessels from various places within the Roman Empire, as well as outside of it. The major part of the work comprises blown glass from the Roman imperial period (chapter four), both free-blown and mold-blown, and from this virtually half are unguentaria of various types. Almost all types of vessel produced in this period are found in this chapter. The vessels were ordered according to types - e.g. open shapes, closed shapes and in the framework of these types they are arranged further - according to other criteria which create other sub-groups - as for example forms without a foot or on a...

The demand for flat glass is high and increasing significantly in the building industry as a direct result of architectural requirements for lightness, transparency and natural light. Current architectural trends require glass in curvilinear forms for smooth free-form façades. Two principal challenges arise from this: to cost-effectively produce the desired curvature and; to ensure its safe performance after exposure to ageing. The recent availability of high strength glass provides an opportunity to address the first challenge by developing cold bent glass. Cold bending involves the straining of relatively thin glass components, at ambient temperatures, and is a low energy and cost effective manner of creating curvilinear forms. However, cold bending is not yet widely established as a reliable method. The aim of this thesis is to develop the understanding of cold bent glass during the bending process and to evaluate its post-ageing performance. This thesis, firstly, investigates the mechanical response of monolithic glass plates during the cold bending process. The stability of cold bent glass is investigated experimentally by bending it in double curved anticlastic shapes. A parametric numerical analysis involves different boundary conditions, geometrical plate characteristics and bending parameters. The principal outcome is that a local instability, now termed cold bending distortion, occurs when certain displacement limits are exceeded and could degrade the optical quality of the glass. An evaluation procedure is also formulated to set limits and aid designers/manufacturers to predict the mechanical response and the optical quality of the glass. Cold bent glass is subjected to permanent bending stresses throughout its service life and therefore, its strength degradation after ageing needs to be quantified. Analytical, experimental and numerical investigations are undertaken in this thesis to identify the most effective method for estimating glass strength (evaluation of destructive tests, required number of specimens, statistical analysis methods and sub-critical crack growth). The limited availability of naturally aged toughened glass and the absence of a reliable ageing standard impede the evaluation of its aged performance. Therefore, a parametric experimental investigation of artificial ageing methods on glass is undertaken in this thesis. A procedure for the evaluation of the strength of aged glass is finally, formulated to allow the selection of artificial ageing parameters that correspond to a target level of erosion. The knowledge on artificial ageing and strength prediction acquired above is finally implemented on different types of glass to determine their strength after ageing and assess their safe use in cold bending / load bearing applications. The investigation showed that fully toughened glass has a superior performance to chemically toughened or annealed glass. Overall, the research presented in this thesis demonstrates that high quality cold bent toughened glass can be created when certain applied displacement limits are respected. These can be used as a safe, cost-effective and energy efficient replacement to the more conventional hot bent glass. However, cold bending / load bearing applications in which the stressed glass surface is exposed to ageing, require glass with a relatively high case depth such as fully toughened or bi-tempered glass.