This diploma thesis summarizes knowledge from the fields of synthesis, characterization and application of titanium dioxide nanotubes and its combination with silver nanoparticles for biomedical purposes. Basic protocols of working with cell cultures and bacteria are also included. Experimental part of this diploma thesis focuses mainly on the synthesis of tubular structures made of titanium dioxide via anodic oxidation of 500nm titanium layer and their subsequent decoration with silver by electrodeposition. Last section of the experimental part is devoted to testing of antibacterial properties of the new material and examining the effect of different silver concentrations on the adhesion of MG-63 cells. All results are compared to reference samples consisting of titanium dioxide nanotubes without silver.

In the oil and gas industry, high corrosion resistance and hardness are needed to extend the lifetime of the coatings due to exposure to high stress and salt environments. Electrodeposition has become a favorable technique in synthesizing coatings because of low cost, convenience, and the ability to work at low temperatures. Electrodeposition of metal matrix composites has become popular for enhanced corrosion resistance and hardness in the oil and gas industry because of the major problems that persist with corrosion. Two major alloys of copper-nickel, 90-10 and 70-30, were evaluated for microbial corrosion protection in marine environments on a stainless steel substrate. Copper and copper alloys are commonly used in marine environments to resist biofouling of materials by inhibiting microbial growth. Literature surveying the electrodeposition of Cu-Ni incorporated with nano- to micro- particles to produce metal matrix composites has been reviewed. Also, a novel flow cell design for the enhanced deposition of metal matrix composites was examined to obtain the optimal oriented structure of the layered silicates in the metal matrix. With the addition of montmorillonite into the Ni and Cu-Ni matrix, an increase in strength, adhesion, wear and fracture toughness of the coating occurs, which leads to an increase corrosion resistance and longevity of the coating. These coatings were evaluated for composition and corrosion using many different types of instrumental and electrochemical techniques. The overall corrosion resistance and mechanical properties were improved with the composite films in comparison to the pure metals, which proves to be advantageous for many economic sectors including the oil and gas industry.

The new nickel/layered silicate nanocomposites were electrodeposited from different pHs to study the influence on the metal ions/layered silicate plating solution and on the properties of the deposited films. Nickel/layered silicate nanocomposites were fabricated from citrate bath atacidic pHs (1.6−3.0), from Watts’ type solution (pH ~4-5), and from citrate bath at basic pH (~9). Additionally, the new nickel/molybdenum/layered silicate nanocomposites were electrodeposited from citrate bath at pH 9.5. The silicate, montmorillonite (MMT), was exfoliated by stirring in aqueous solution over 24 hours. The plating solutions were analyzed for zeta potential, particle size, viscosity, and conductivity to investigate the effects of the composition at various pHs. The preferred crystalline orientation and the crystalline size of nickel, nickel/layered silicate, nickel/molybdenum, and nickel/molybdenum/layered silicate films were examined by X-ray diffraction. The microstructure of the coatings and the surface roughness was investigated by scanning electron microscopy and atomic force microscopy. Nickel/molybdenum/layered silicate nanocomposites containing low content of layered silicate (1.0 g/L) had increase 32 % hardness and 22 % Young’s modulus values over the pure nickel/molybdenum alloy films. The potentiodynamic polarization and electrochemical impedance measurements showed that the nickel/molybdenum/layered silicate nanocomposite layers have higher corrosion resistance in 3.5% NaCl compared to the pure alloy films. The corrosion current density of the nickel/molybdenum/layered silicate nanocomposite composed of 0.5 g/L MMT is 0.63 µA·cm-2 as compare to a nickel/molybdenum alloy which is 2.00 µA·cm-2.

The electrochemical behavior of nickel (Ni) in different concentrations of sulfuric acid (H2SO4) was studied via cyclic voltammetry (CV) over a range of potentials (0.0 V– 3.0 V) at room temperature. The presented work displays novel experiments where external forcing by a platinum (Pt) electrode changed the proton concentration at a Ni electrode surface in order to control the frequency and magnitude of periodic oscillations produced. When studying unique phenomena such as the Ni phenomena in this thesis, efficient, durable, and inexpensive technology is always beneficial. A coupled microelectrode array sensor or CMAS which has been used for over four decades to study pitting corrosion, crevice corrosion, intergranular corrosion, galvanic corrosion, and other heterogeneous electrochemical processes were fabricated in a novel, systematic, inexpensive, and time efficient process. The presented work shows how to make the CMAS and proved that they functioned properly.

Zn-Mo coatings are very promising environment friendly anticorrosive coatings as replacement materials for cadmium and chromium (VI) based conversion layers. Electrodeposition has become a favorable technique in fabricating coatings due to its low cost, ease of use, and overall experimental control of coating quality. Very little research so far has been done for the electrodeposition of Zn-Mo coatings under alkaline conditions. In this work, Zn and Zn-Mo coatings were electrochemically deposited on stainless steel from an aqueous alkaline citrate solution. An organic compound, vanillin, was added to the electrolyte as a leveling agent for improving interlayer adherence and corrosion resistance of Zn-Mo coatings. Ni-Mo alloys have been known to possess high tensile strength and excellent corrosion protection of steels, and MoTe2 layers have a potential for the application in anticorrosive coatings due to their hydrophobic properties. In this study, MoTe2-Ni-Mo coatings were deposited on stainless steel using both sputtering and electrodeposition methods. These coatings with high corrosion resistance and other desirable properties are in demand in the oil and gas industry since they can protect and thus extend the lifetime of the underlying materials when exposed to aggressive environments. The Zn-Mo and MoTe2-Ni-Mo coatings were evaluated for chemical composition and corrosion behavior using different types of instrumental and electrochemical techniques. The addition of vanillin to the electrolyte did not change the crystalline structure or composition of the Zn-Mo coating, however, the corrosion resistance of the coating was significantly improved by the leveling effect of vanillin during the electrodeposition. The corrosion resistance of the Ni-Mo coating was also enhanced by applying the hydrophobic MoTe2 monolayer on the top surface.

This dissertation describes the electrochemical behavior of nickel and iron that was studied in different acid solutions via linear sweep voltammetry, cyclic voltammetry, and potentiostatic measurements over a range of temperatures at specific potential ranges. The presented work displays novel experiments where a nickel electrode was heated locally with an inductive heating system, and a platinum (Pt) electrode was used to change the proton concentration at iron and nickel electrode surfaces to control the periodic oscillations (frequency and amplitude) produced and to gain a greater understanding of the systems (kinetics), oscillatory processes, and corrosion processes. Temperature pulse voltammetry, linear sweep voltammetry, and cyclic voltammetry were used for temperature calibration at different heating conditions. Several other metal systems (bismuth, lead, zinc, and silver) also produce periodic oscillations as corrosion occurs; however, creating these with pure metal electrodes is very expensive. In this work, metal systems were created via electrodeposition by using inexpensive, efficient, coupled microelectrode array sensors (CMASs) as a substrate. CMASs are integrated devices with multiple electrodes that are connected externally in a circuit in which all of the electrodes have the same amount of potential applied or current passing through them. CMASs have been used for many years to study different forms of corrosion (crevice corrosion, pitting corrosion, intergranular corrosion, and galvanic corrosion), and they are beneficial because they can simulate single electrodes of the same size. The presented work also demonstrates how to construct CMASs and shows that the unique phenomena of periodic oscillations that can be created and studied by using coated and bare copper CMASs. Furthermore, these systems can be controlled by implementing external forcing with a Pt electrode at the CMAS surface. The data from the single Ni electrode experiments and CMAS experiments were analyzed by using the Nonlinear Time-Series Analysis approach.

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<p><p lang="en-US">This experimental research thesis describes the combination of conjugated polymers and carbon nanotubes with the fields of electrophoretic deposition (EPD) and organic solar cells. Prior to these contributions, soluble conjugated polymers and carbon nanotubes that have been functionalized by them had not yet been deposited by EPD from solution or by using non-toxic solvents. Additionally, EPD had not yet been utilized to deposit the active layer in a solid organic photovoltaic device. <p lang="en-US">The EPD of soluble conjugated polymer functionalized carbon nanotubes from non-toxic solvents was achieved through an iterative process of experimentation and technique refinement. The developed EPD technique utilized the high pH region at the cathode substrate to neutralize positively charged weak polyelectrolytes macromolecules. Their functional groups were protonated using a minimized amount of acetic acid which also enabled their solubility. Deprotonation of the quaternary ammonium functional groups rendered them neutrally charged and insoluble tertiary amines. This mechanism facilitated the formation of coatings that were predictable and uniform in appearance and thickness. <p lang="en-US">Control over coating thickness was demonstrated by coatings spanning 100 nm to 10 μm. These coatings were produced by adjusting the applied voltage, solution concentration, and tuning the deposition duration. <p lang="en-US">Techniques for the fabrication of a photovoltaic device using an active layer produced by EPD were established though modifications of general organic photovoltaic device fabrication procedures. These modifications involved redesigning the photolithographic ITO etching pattern, adding an insulating barrier strip, thickening the aluminum electrode layer, and switching the top buffer layer from LiF to BCP.</p> / Master of Applied Science (MASc)

[ES] Este proyecto de investigación se centra en el campo de las energías renovables y más concretamente de la energía solar fotovoltaica. La tesis se ha focalizado en el desarrollo de películas delgadas de Cobre-Indio-GalioSelenio o Sulfuro (CuIn1-xGax(Se,S)2) con técnicas de bajo coste. La mayoría de las celdas basadas en CIGS utilizan el CdS como capa de búfer. En nuestro experimento, usaremos otra capa de tampón como SnS2 o ZnO1-xSx como alternativa a CdS para mejorar nuestra célula. El estudio se centrará en el contacto tampón/absorbedor para reducir la recombinación. En este trabajo, reportamos la investigación experimental del desarrollo y desarrollo de la caracterización de la calcopirita de cobre, indio, galio y selenio (CIGS) por la técnica de electrodeposición y pulverización. Además, nos hemos centrado en el contacto entre la capa generadora que es el absorbedor y el circuito externo. Las propiedades eléctricas de este contacto dependen principalmente del proceso de deposición de la capa absorbente en el contacto trasero utilizado. Por lo tanto, será necesario controlar el crecimiento de la capa interfacial de MoSe2 entre el absorbedor y el contacto posterior en el caso del molibdeno para obtener un rendimiento óptimo. Por supuesto, la eficiencia de la célula depende de un gran número de parámetros experimentales y varía según los métodos de fabricación, especialmente la capa absorbente CIGS. En nuestro caso, las técnicas utilizadas son la galvanoplastia y la pirólisis por pulverización para la deposición de películas CIGS. Estas técnicas son más baratas, prácticamente alcanzables en cualquier laboratorio y dan un buen rendimiento. Por lo tanto, mediante técnicas de deposición de bajo coste hemos estudiado el comportamiento de la célula solar con una capa de MoSe2 como capa interfacial y el efecto de la banda prohibida de la capa formada y la capa tampón utilizada sobre los parámetros de las células solares CIGS. Los resultados de este estudio podrían ayudar a mejorar el rendimiento de las células solares CIGS utilizando técnicas de bajo coste. / [CA] Aquest projecte de recerca es centra en el camp de les energies renovables i més concretament en l'energia solar fotovoltaica. La tesi s'ha centrat en el desenvolupament de pel·lícules primes de Coure-Indi-Gali-Seleni o Sulfur (CuIn1-xGax(Se,S)2) amb tècniques de baix cost. La majoria de les cel·les basades en CIGS utilitzen el CdS com a capa de búfer. En el nostre experiment, farem servir una altra capa de tampó com ara SnS2 o ZnO1-xSx com a alternativa al CdS per millorar la nostra cel·la. L'estudi es centrarà en el contacte tampó/absorbidor per reduir la recombinació. En aquest treball, reportem la recerca experimental del desenvolupament i la caracterització de la calcopirita de coure, indi, gali i seleni (CIGS) mitjançant la tècnica d'electrodeposició i pulverització. A més, ens hem centrat en el contacte entre la capa generadora que és l'absorbidor i el circuit extern. Les propietats elèctriques d'aquest contacte depenen principalment del procés de deposició de la capa absorbent en el contacte posterior utilitzat. Per tant, serà necessari controlar el creixement de la capa interfacial de MoSe2 entre l'absorbidor i el contacte posterior en el cas del molibdè per obtenir un rendiment òptim. És clar que l'eficiència de la cel·la depèn d'un gran nombre de paràmetres experimentals i varia segons els mètodes de fabricació, especialment la capa absorbent CIGS. En el nostre cas, les tècniques utilitzades són la galvanoplàstia i la piròlisi per pulverització per a la deposició de pel·lícules CIGS. Aquestes tècniques són més econòmiques, pràcticament assolibles en qualsevol laboratori i proporcionen un bon rendiment. Per tant, mitjançant tècniques de deposició de baix cost hem estudiat el comportament de la cel·la solar amb una capa de MoSe2 com a capa interfacial i l'efecte de la banda prohibida de la capa formada i la capa tampó utilitzada sobre els paràmetres de les cel·les solars CIGS. Els resultats d'aquest estudi podrien ajudar a millorar el rendiment de les cel·les solars CIGS utilitzant tècniques de baix cost. / [EN] Our research project aims at the field of renewable energies and more specifically, photovoltaic solar energy, i.e. solar cells, our study focuses on the elaboration of Copper-Indium-Gallium-Selenium or Sulfide (CuIn1-xGax(Se,S)2 thin films for solar cells with low-cost techniques also to develop the performance of the typical solar cell structure: n-ZnO/i-ZnO/n-tampon/p-CIGS/p+-MoSe2/back contact. Most of the CIGS based cells use CdS as a buffer layer. In our experiment, we will make use of another buffer layer such as SnS2 or ZnO1-xSx as an alternative to CdS to improve our cell. The investigation will be carried out on the buffer/absorber contact to reduce recombination. In addition, we will focus on the contact between the generating layer which is the absorber and the external circuit. The electrical properties of this contact depend essentially on the deposition process of the absorber layer on the back contact used. It will thus be necessary to control the growth of the MoSe2 interfacial layer between the absorber and the back contact in the case of Molybdenum in order to obtain an optimal yield. Obviously, the yield of the cell depends on a large number of experimental parameters and varies according to the fabrication methods, especially of the CIGS absorber layer. In our case the techniques used are electrodeposition and spray pyrolysis for the deposition of CIGS films, there techniques are cheaper, practically feasible in the laboratory and give good performance. Therefore, we will investigate, using low-cost deposition techniques, the performance of the cell with a MoSe2 layer as an interfacial layer and the effect of the bandgap of the formed layer and the buffer layer used on the parameters of the CIGS solar cells. The results of this study could help to improve the performance of the CIGS solar cell using low-cost techniques. / Armel Ignace, N. (2024). Elaboration et caractérisation de couches minces de cuivre, indium, gallium et sélénium (CIGS) pour cellules solaires [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/203613