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Electrochemical synthesis, characterization and applications of new types of 1D valve metal oxide nanostructures
Alijani, Mahnaz ; Prof. Lluis F. Marsal (referee) ; Tsuchiya, Hiroaki (referee) ; Macák, Jan (advisor)
Tato disertační práce představuje komplexní výzkum růstu TiO2 nanotrubicových (TNT) vrstev s vysokým poměrem délka/šířka (HAR) a jejich využití v pokročilých světelně-sensorických aplikacích. Výzkumné výstupy dosažené během tohoto doktorského studia zahrnují sérii článků, které se zabývají výzkumem syntézy a charakterizace vrstev HAR TNT na jedné straně a hodnocení výkonu těchto vrstev v různých senzorických modalitách na straně druhé. Počáteční studie se zaměřuje na anodizaci Ti fólií za účelem získání vrstev HAR TNT pomocí speciálně formulované elektrolytu obsahujícího NH4F/H2O/ethylene glycol s přídavkem mléčné kyseliny (LA). Výsledky ukazují, že regulací stáří a složení elektrolytu a použitím dostatečně vysokých potenciálů lze dosáhnout vrstev HAR TNT s vysokým poměrem délka/šířka (přibližně 450) v pozoruhodně krátkých časech anodizace ( 15 minut) ve srovnání s literaturou dostupnou před zahájením této disertační práce. Tento přístup nabízí slibnou cestu k získání robustních vrstev TNT bez dielektrického průrazu, eliminující potřebu řízení dalších procesních parametrů, jako je ohřev nebo ochlazování elektrolytu. Na základě úspěšných výsledků byla v následující práci zkoumána galvanostatická anodizace pro získání vrstev HAR TNT v elektrolytu obsahujícím LA. Bylo zjištěno, že mléčná kyselina účinně předchází dielektrickému průrazu při použití vysokých proudových hustot. Tento nález poukazuje na potenciál galvanostatické anodizace pro výrobu vrstev HAR TNT v podstatně zkrácených časech anodizace při pokojové teplotě. Navazující výzkum v disertační práci se zabývá mikrovlnnou fotoelektrickou vodivostí TNT vrstev s různou tloušťkou (15, 50, 80 a 110 m) při frekvencích X-pásma (~8 GHz) pro aplikace v senzorice a bezdrátové vesmírné komunikaci. Integrace anatasových TNT vrstev s rovinným rezonátorem se rozděleným kroužkem (SRR) umožňuje hodnocení jejich mikrovlnné fotoelektrické vodivosti. Experimentální výsledky odhalily významné variace v rezonanční amplitudě a frekvenčních odezvách TNT vrstev, přičemž TNT vrstvy o tloušťce 80 m vykazovaly nejvyšší citlivost. Byly stanoveny korelace mezi účinností fotoelektrické vodivosti, velikostí krystalitů a tloušťkou vrstev TNT, což podporuje využití optimalizovaných vrstev TNT pro co nejlepší mikrovlnného snímání. Kromě toho práce zkoumá vrstvy TNT na SRR pro detekci viditelného světla. Depozicí CdS tenkých vrstev na TNT vrstvy pomocí technologie depozice atomárních vrstev (ALD) se TNT vrstvy stávají velmi citlivé ve viditelné oblasti spektra, což umožňuje efektivní detekci UV a viditelného světla a detekci světlem indukovaných změn dielektrických vlastností TNT vrstev. Experimentální výsledky souhlasí s teoretickými modely a zdůrazňují výjimečný potenciál senzorů založených na TNT při detekci nebezpečí, monitorování znečištění, analýze materiálů a světelné komunikaci mezi satelity. Celkově tato práce poskytuje komplexní porozumění o růstu HAR TNT vrstev a jejich schopnostem pro pokročilé senzorické aplikace. Získané poznatky z tohoto výzkumu přispějí k rozvoji senzorů založených na nanomateriálech a otevírají nové možnosti jejich využití v různých odvětvích a nových technologiích.
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Oxidation barriers prepared by electrochemical procedures
Šťastná, Eva ; Pouchlý, Václav (referee) ; Jan, Vít (advisor)
A process with aim to prepare an oxidically and thermal resistant layer was performed on the samples from clear aluminium (99,99+ %, VÚK čisté kovy, s. r. o.) and on the samples from clear titanium (99,95 % Goodfellow) with a layer from sputtered aluminium (99,99 %, VÚK čisté kovy, s. r. o.), An oxidic layer was prepared on the samples by anodization in the oxalic acid. The layer had fine, hexagonally organized pores with the diameter of 30 nm. During the following processing was the structure prepared for the electrochemical deposition of copper to the pores. The aim of the electrodeposition was preparation of copper nanowires deposited into the pores of the oxidic layer. The process was performed in the solution of copper sulfate and sulfuric acid in water. The controlling parameter of the deposition was voltage which had a very asymmetric period. The period had to be optimized for a successful preparation of the wires. The result of the whole process was structure with oxidic matrix whose most of the pores were filled with copper.
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Anodizing of Aluminium and Its Alloys
Remešová, Michaela ; Julišová, Martina (referee) ; Čelko, Ladislav (advisor)
This thesis focuses on the hard anodic oxidation of aluminum and its alloys. As an experimental materials were used various aluminum materials, produced by cold forming and casting. The work contains information about chemical composition of the base materials, photographs of their microstructure, the results of surface roughness before and after anodic oxidation, photo anodized layer, measurements hardness oxide layers. For study were used methods light microscopy, scanning electron microscopy, surface profilometry and microhardness measurements.
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Measurement of corrosion resistance of anodized aluminum protective surface layers
Redr, Martin ; Jandová, Kristýna (referee) ; Chladil, Ladislav (advisor)
This master’s thesis is focused on anodic oxidation of an aluminium surface with subsequent sealing of the surface using mid-temperature sealing methods. The research in the theoretical part of the thesis is carried out in surface treatments of aluminium and its alloys, where attention is mainly paid to anodic oxidation, as it is the most widely used surface treatment. The second discussed and at the same time key topic is the sealing process of the anodic coating, which has a fundamental effect on the quality of the corrosion resistance of the resulting surface. In the practical part of the thesis, a number of anodic oxidation experiments with subsequent sealing of the coating on prepared aluminium samples and their subsequent evaluation according to ČSN EN ISO 3210 standard were carried out. Mid-temperature sealing experiments were mainly focused on the use of triethanolamine (TEA), which seems very promising in terms of the resulting sealing quality.
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Electrochemical impedance spectroscopy as a nanostructured bioelectrodes characterization method
Vrbová, Eva ; Urbánková, Kateřina (referee) ; Hrdý, Radim (advisor)
Diploma thesis deals of nanostructured surfaces, nanoparticles and electrochemical characterization methods such as cyclic voltammetry, differential pulse voltammetry and electrochemical impedance spectroscopy. The aim of this thesis is a theoretical research issues of production and characterization nanostructured modified electrodes. The practical part is the production of biomodified nanostructured electrodes by anodi- zation W/Al layers with galvanic deposition of gold or deposition of mercury, a modifi- cation of the electrodes by 11-mercaptoundecanoic acid and by bovine serum albumin (BSA). The thesis includes SEM images of nanostructured electrodes contact angle mea- surements of these electrodes and form an electrical circuit with subsequent simulation waveforms.
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Gas Microsensors Based on Self-Organized 3D Metal-Oxide Nanofilms
Pytlíček, Zdeněk ; Husák, Miroslav (referee) ; Kolařík, Vladimír (referee) ; Prášek, Jan (advisor)
This dissertation concerns the development, fabrication and integration in a gas sensing microdevice of a novel 3-dimensional (3D) nanostructured metal-oxide semiconducting film that effectively merges the benefits of inorganic nanomaterials with the simplicity offered by non-lithographic electrochemistry-based preparation techniques. The film is synthesized via the porous-anodic-alumina-assisted anodizing of an Al/Nb metal bilayer sputter-deposited on a SiO2/Si substrate and is basically composed of a 200 nm thick NbO2 layer holding an array of upright-standing spatially separated Nb2O5 nanocolumns, being 50 nm wide, up to 900 nm long and of 8109 cm2 population density. The nanocolumns work as semiconducting nano-channels, whose resistivity is greatly impacted by the surface and interface reactions. Either Pt or Au patterned electrodes are prepared on the top of the nanocolumn array using an innovative sensor design realized by means of microfabrication technology or via a direct original point electrodeposition technique, followed by selective dissolution of the alumina overlayer. For gas-sensing tests the film is mounted on a standard TO-8 package using the wire-bonding technique. Electrical characterization of the 3D niobium-oxide nanofilm reveals asymmetric electron transport properties due to a Schottky barrier that forms at the Au/Nb2O5 or Pt/Nb2O5 interface. Effects of the active film morphology, structure and composition on the electrical and gas-sensing performance focusing on sensitivity, selectivity, detection limits and response/recovery rates are explored in experimental detection of hydrogen gas and ammonia. The fast and intensive response to H2 confirms the potential of the 3D niobium-oxide nanofilm as highly appropriate active layer for sensing application. A computer-aided microfluidics simulation of gas diffusion in the 3D nanofilm predicts a possibility to substantially improve the gas-sensing performance through the formation of a perforated top electrode, optimizing the film morphology, altering the crystal structure and by introducing certain innovations in the electrode design. Preliminary experiments show that a 3D nanofilm synthesized from an alternative Al/W metal bilayer is another promising candidate for advanced sensor applications. The techniques and materials employed in this work are advantageous for developing technically simple, cost-effective and environmentally friendly solutions for practical micro- and nanodevices, where the well-defined nano-channels for charge carriers and surface reactions may bring unprecedented benefits.
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Reflex of Space
Šrom, Samuel ; František,, Dvořák (referee) ; Korbička, Pavel (advisor)
The diploma thesis named Reflections of Space aims to change the approach at material anodizing and to move this purely technological process to the artistic level. The first part of the thesis summarises concisely a process of anodising and seeks for its demonstrations in the field of culture. The second part of the thesis describes the intention itself and the results of the research in the framework of technological proofs which are presented in the figurative part of the thesis.
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Technology of Galvanic Anodization of Non-ferrous Materials and Its Alloys
Remešová, Michaela ; Hadraba,, Hynek (referee) ; Čelko, Ladislav (advisor)
The thesis is focused on the theoretical description of the technology of anodizing of aluminium, magnesium, zinc and their alloys. In this work, methods for formation of oxide layers and the used chemical processes are described in detail. The experimental part of this work deals with formation of oxide layers on aluminium, magnesium and zinc of high purity under different conditions. Oxide layers of different thicknesses were created on all three experimental materials. Aluminium was anodized in a bath of 10% H2SO4, magnesium in the bath of 1 mol/dm3 NaOH, and zinc in the bath of 0.5 mol/dm3 NaOH. Processes were carried out at laboratory temperature. On the aluminium, continuous oxide layer was formed. Furthermore rule "312" was verified, that can indicatively be used for calculating the thickness of the resulting oxide layer on the aluminium. When using lower current of 0.08 and 0.2 A for magnesium anodizing, dark colored layer was created comparing to higher current of 0.5 A. More rough appearance of the oxide layer was produced with increasing voltage. Further, it was observed for magnesium that the resulting layer comprises of two sublayers. For zinc, black colored layer was created when the voltage 20 V and current from 0.4 to 0.5 A were used. In the layer, two sublayers were also observed. For lower voltage and current (0.05 A, 0.17 V), formation of the oxide layer on the zinc does not occur, but the crystallographic etching was observed.
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Fabrication and Characterization of Templates for Fabrication of Nanowires
Lednický, Tomáš ; Čechal, Jan (referee) ; Škoda, David (advisor)
The bachelor thesis is focused on fabrication of alumina templates by anodization of pure aluminium. The theoretical part discusses the growing process of anodized oxide layers and its dependency on the crucial parameters (solutions, anodization voltage, time). The theoretical part is particularly based on literature retrieval. The experimental part is aimed to the fabrication of alumina membranes: the apparatus design, aluminium foils preparation, aluminium anodization, membrane modifications for next applications (nanowires deposition) and membrane characterization.
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