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Electrochemical synthesis, characterization and applications of new types of 1D valve metal oxide nanostructures
Alijani, Mahnaz ; Prof. Lluis F. Marsal (oponent) ; Tsuchiya, Hiroaki (oponent) ; Macák, Jan (vedoucí práce)
This thesis presents a comprehensive investigation of the growth of high-aspect-ratio (HAR) TiO2 nanotube (TNT) layers and their application in advanced light sensing technologies. The research outputs achieved during this Ph.D. study encompass a series of papers that collectively explore the synthesis and characterization of HAR TNT layers on one hand side, and performance evaluation of these layers in various sensing modalities on the other side. The initial study focuses on the successful anodization of Ti foil to obtain HAR TNT layers using a specially formulated electrolyte containing NH4F/H2O/ethylene glycol, with the addition of lactic acid (LA). The results demonstrate that by controlling the electrolyte age and composition, together with the application of sufficiently high potentials, HAR TNT layers with high aspect ratio (of approximately 450) can be achieved within remarkably short anodization times ( 15 minutes) compared to the literature available before the work on this thesis begun. This approach offers a promising pathway to obtain robust TNT layers without dielectric breakdown, eliminating the need for additional process control, such as heating or cooling of the electrolyte. Building up on the successful anodization results, the subsequent investigation explored the galvanostatic anodization for obtaining HAR TNT layers in an LA-containing electrolyte. It was observed that lactic acid effectively prevents dielectric breakdown when high current densities are applied. This finding highlights the potential of galvanostatic anodization to produce HAR TNT layers in significantly reduced anodization times at room temperature. Expanding the research scope, the thesis delves into the microwave photoconductivity of TNT layers with different thicknesses (15, 50, 80, and 110 m) at X-band frequencies (~8 GHz) for applications in sensing and wireless space communication. The integration of anatase TNT layers with a planar split ring resonator (SRR) microwave resonator enables the evaluation of their microwave photoconductivity performance. Experimental results revealed significant variations in the resonant amplitude and frequency responses of the TNT layers, with the 80 m thick TNT layers demonstrating the highest sensitivity. Correlations were established between the photoconductivity efficiency, crystallite size, and thickness of the TNT layers, supporting the development of optimized TNT layers for enhanced microwave sensing capabilities. Furthermore, the thesis explores TNT layers on SRR for visible light detection. By sensitizing the TNT layers to the visible spectral region through the deposition of a CdS coating using Atomic Layer Deposition (ALD), the results demonstrate effective detection of ultraviolet (UV) light, visible (VIS) light and light-induced variations in the dielectric properties of TNT layers. The experimental findings align with theoretical models and highlight the clearly outstanding potential of TNT-based sensors in hazard detection, pollution monitoring, material analysis, and light-based satellite-to-satellite communication. Overall, this thesis provides a comprehensive understanding of HAR TNT layers and their capabilities for advanced sensing applications. The knowledge gained from this research will contribute to the advancement of nanomaterial-based sensors and opens up new possibilities for their utilization in various industries and emerging technologies.
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