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ItemBiomimetic and synthetic syntheses of nanostructured electrode materials(Georgia Institute of Technology, 2012-12) Berrigan, John DanielThe scalable syntheses of functional, porous nanostructures with tunable three-dimensional morphologies is a significant challenge with potential applications in chemical, electrical, electrochemical, optical, photochemical, and biochemical devices. As a result, several bio-enabled and synthetic approaches are explored in this work (with an emphasis on peptide-enabled deposition) for the generation of aligned nanotubes of nanostructured titania for application as electrodes in dye-sensitized solar cells and biofuel cells. As part of this work, peptide-enabled deposition was used to deposit conformal titania coatings onto porous anodic alumina templates under ambient conditions and near-neutral pH to generate aligned, porous-wall titania nanotube arrays that can be integrated into dye-sensitized solar cells where the arrays displayed improved functional dye loading compared to sol-gel-derived nanotubes. A detailed comparison between synthetic and bioorganic polyamines with respect to titania film properties deposition rate provided valuable information for future titania coating experimental design given specific applications. The development of template-based approaches to single-wall titania nanotube arrays led to the development of a new synthetic method to create aligned, multi-walled titania nanotube arrays. Lastly, peptide-enabled deposition methods were extended beyond inorganic mineral and used for enzyme immobilization by cross-linking the peptide with the multicopper oxidase laccase. Peptide-laccase hybrid enzyme coatings improved both the amount of enzyme adsorbed onto carbon nanotube “buckypaper” and allowed the enzyme to retain more activity upon immobilization onto the surface.
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ItemStress and microstructural evolution during shape-preserving silica magnesiothermic reduction(Georgia Institute of Technology, 2012-03-06) Davis, Stanley CaseyShape-preserving silica magnesiothermic reduction is a gas-solid reaction used to convert complex, 3-dimensional SiO₂ structures into replicas composed of a two-phase product of MgO and Si. The MgO/Si components of this reaction are found to form an interwoven aggregate product structure, which is suitably robust that the MgO phase can be selectively dissolved to yield porous Si. Here, the kinetics and mechanisms of growth of this robust product structure have been studied. The aggregate product structure was deduced to result because stacked layers of MgO/Si product phases with planar interfaces are geometrically unstable, owing to the growth kinetics of the products. The interwoven nature of the aggregate may be explained by the presence of an amorphous magnesium silicate phase ahead of the MgO/Si product during reaction. Complex composition gradients in the magnesium silicate can lead to tortuous and branching growth of MgO and Si phases as the magnesium silicate is consumed by reaction. In addition, a large residual stress (> 5 GPa) was measured in the MgO/Si product layer formed during reaction of planar quartz. Despite the presence of such a large stress, no distortion or cracking of reacted structures was found to occur after reaction in the temperature range 650-900 °C. XRD-based residual stress measurements and morphological observations of product films on reacted quartz substrates were used to evaluate possible mechanisms of stress relief in the structure. It was found that the migration of MgO to the external surface of the product layer could be correlated to the rate of stress relaxation that occurred in annealed product films. Finally, applications of silica magnesiothermic reduction and derivative processes were studied in the fields of chemical catalysis and optical chemical sensing.
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ItemMorphology-preserving chemical conversion of bioorganic and inorganic templates(Georgia Institute of Technology, 2012-01-17) Vernon, Jonathan P.The generation of nanostructured assemblies with complex (three-dimensional, 3D) self-assembled morphologies and with complex (multicomponent) tailorable inorganic compositions is of considerable technological and scientific interest. This research demonstrates self-assembled 3D organic templates of biogenic origin can be converted into replicas comprised of numerous other functional nanocrystalline inorganic materials. Nature provides a spectacular variety of biologically-assembled 3D organic structures with intricate, hierarchical (macro-to-micro-to-nanoscale) morphologies. Morphology-preserving chemical conversion of such readily available, structurally complex templates will provide a framework for chemical conversion of synthetic organic templates and, potentially, production of organic/inorganic composites. Four research thrusts are detailed in this dissertation. First, chemical conversion of a nanostructured bioorganic template into a multicomponent oxide compound (tetragonal BaTiO₃ via layer-by-layer surface sol-gel coating and subsequent morphology-preserving microwave hydrothermal processing was demonstrated. Second, photoluminescence was imparted to bioorganic template structures through morphology-preserving chemical conversion to exhibit both the dramatic change in properties such processing can provide, and the potential utility of chemically transformed templates in anti-counterfeiting / authentication applications. Third, the reaction mechanism(s) for morphology-preserving microwave hydrothermal conversion of TiO₂ to BaTiO₃, were studied with the aid of Au inert markers on single crystal rutile TiO₂. Finally, constructive coating techniques (SSG) and moderate temperature (< 500C) heat treatments were utilized to modify and replicate structural color and were coupled with deconstructive focused ion beam microsurgery to prepare samples for microscale structure/property interrogation. Specifically, the effects of coating thickness and coating composition on reflection spectra of structurally colored templates were examined. Also, the effects of the replacement of natural material with higher index of refraction inorganic materials on optical properties were studied. The three processing research thrusts constituting chapters 1, 2 and 4 take advantage of moderate temperature processing to ensure nanocrystalline materials, either for shape preservation or to prevent scattering in optical applications. The research thrust presented in chapter 3 examines hydrothermal conversion of TiO₂ to BaTiO₃, not only to identify the reaction mechanism(s) involved in hydrothermal conversion under morphology-preserving conditions, but also to introduce inert marker experiments to the field of microwave hydrothermal processing.
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ItemFabrication and characterization of optically emissive microresonators(Georgia Institute of Technology, 2011-05-24) Mansfield, EricMicroresonators are devices that confine light in small volumes through total internal reflection. Introducing an emissive species into a microresonator allows for resonance enhanced emission at frequencies where the spectrum of the emissive species overlaps with the resonant frequencies of the microresonator. Previous research has led to a good understanding of these phenomena in 1D and 2D microresonators, but many 3D microresonator geometries have not yet been investigated. This work details the successful creation and demonstration of a cubic polymeric optical microresonator.
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ItemNovel reaction processing techniques for the fabrication of ultra-high temperature metal/ceramic composites with tailorable microstructures(Georgia Institute of Technology, 2010-12-20) Lipke, David WilliamUltra-high temperature (i.e., greater than 2500°C) engineering applications present continued materials challenges. Refractory metal/ceramic composites have great potential to satisfy the demands of extreme environments (e.g., the environments found in solid rocket motors upon ignition), though general scalable processing techniques to fabricate complex shaped parts are lacking. The work embodied in this dissertation advances scientific knowledge in the development of processing techniques to form complex, near net-shape, near net-dimension, near fully-dense refractory metal/ceramic composites with controlled phase contents and microstructure. Three research thrusts are detailed in this document. First, the utilization of rapid prototyping techniques, such as computer numerical controlled machining and three dimensional printing, for the fabrication of porous tungsten carbide preforms and their application with the Displacive Compensation of Porosity process is demonstrated. Second, carbon substrates and preforms have been reactively converted to porous tungsten/tungsten carbide replicas via a novel gas-solid displacement reaction. Lastly, non-oxide ceramic solid solutions have been internally reduced to create intragranular metal/ceramic micro/nanocomposites. All three techniques combined have the potential to produce nanostructured refractory metal/ceramic composite materials with tailorable microstructure for ultra-high temperature applications.