No presente trabalho foram obtidos e caracterizados filmes finos de SnO2 e SnO2:Sb preparados pelo processo sol-gel. Estes filmes foram estudados através da influência do número de camadas nas suas propriedades ótico-eletroquímicas. Foi observado que a densidade de carga para um filme de SnO2:Sb de 5 camadas foi de 40 mC/cm2, tornando-se um excelente candidato como contra-eletrodo para aplicação em janelas eletrocrômicas. Os filmes de SnO2 e SnO2:Sb também foram estudados utilizando técnicas eletroquímicas: cronoamperometria e voltametria cíclica cujo o enfoque na análise foi o de intercalação de lítio em função da carga inserida. As medidas de transmissão ótica na região de ultravioletainfravermelho próximo revelaram que estes filmes possuem leve coloração azul, evidenciadas pela mudança do espectro UV-Vis em 8% entre estado colorido e descolorido; Por espectroscopia no infravermelho dos sóis, foi possível observar bandas características dos grupos de moléculas presentes em alcóxido, confirmando a formação do alcóxido de estanho enquanto dos precipitados apenas evidências da formação do óxido de estanho. As morfologias dos filmes estudadas por Microscopia Eletrônica de Varredura (MEV) e Microscopia de Força Atômica (AFM) demonstraram que o filme apresenta pequenos riscos, provavelmente devido a presença de Sb, e por AFM obtidas informações da rugosidade e do tamanho de grão, sendo estes valores de 100 nm e 104 nm respectivamente. A partir do espectro do filme por EDX foi possível confirmar a presença de estanho e antimônio nos filmes. A estrutura dos xerogéis e dos sóis para deposição dos filmes estudada por difração de raios-X é a casseterite. Por fim Análises Térmicas (DSC/TGA) demonstram que à 60oC um pico endotérmico correspondendo à liberação de água e uma perda da massa de 6,3 %, e na faixa de 450C um pequeno aumento da linha de base no sentido exotérmico atribuído a cristalização do SnO2:Sb na fase casseterite, com perda de massa de 33%. / In this study were obtained and characterized thin films of SnO2 and SnO2: Sb prepared by the sol-gel process. These films were studied through the influence of the number of layers in its optical-electrochemical properties. It was observed that the density of charge for a film of SnO2: Sb, 5 layers was 40 mC/cm2, making it an excellent candidate as counter-electrode for use in electrochromic windows. The films of SnO2 and SnO2: Sb also were studied using electrochemical techniques: chronoamperometry and cyclic voltammetry with a focus on analysis of intercalation of lithium according to load inserted. Measures of optical transmission in the ultraviolet region of near-infrared revealed that these films have light blue colour, highlighted by the changing spectrum of UV-Vis by 8% between state and colorful discolour; In the infrared spectroscopy, in solution has been possible to see bands characteristics groups of molecules present in alkoxide, confirming the formation of alkoxide of tin while the precipitated only evidence of the formation formation of tin oxide. The morphologies of the films studied by Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM) showed that the film presents little risk, probably because the presence of Sb, and the information obtained by the AFM roughness and the size of grain, and these values of 100 nm and 104 nm respectively. From the spectrum of the film by EDX were unable to confirm the presence of tin and antimony in the films. The structure of xerogel and solution for deposition of films studied by X-rays diffraction is the cassiterite. Finally Thermal Analysis (DSC / TGA) show that the 60oC a peak endothermical corresponding to the release of water and a loss of the mass of 6.3%, and in the 450ºC a small increase from baseline in the sense attributed range of exothermically the crystallization of SnO2:Sb during casseterite, with mass loss of 33%.

Submitted by Rafael Santana (rafael.silvasantana@ufpe.br) on 2017-07-25T19:46:06Z No. of bitstreams: 2 license_rdf: 811 bytes, checksum: e39d27027a6cc9cb039ad269a5db8e34 (MD5) Dissertacao PRONTA.compressed-2.pdf: 7340420 bytes, checksum: 27358d102b9b7c405f37c9e2a0ceb516 (MD5) / Made available in DSpace on 2017-07-25T19:46:06Z (GMT). No. of bitstreams: 2 license_rdf: 811 bytes, checksum: e39d27027a6cc9cb039ad269a5db8e34 (MD5) Dissertacao PRONTA.compressed-2.pdf: 7340420 bytes, checksum: 27358d102b9b7c405f37c9e2a0ceb516 (MD5) Previous issue date: 2015-07-02 / Neste trabalho foi feito um estudo das propriedades estruturais e magnéticas de filmes granulares de cromita de cobalto sobre substrato de silicio. Aqui os filmes foram fabricados a partir do método químico sol‐gel, técnica de centrifugação spincoating e Tratamento térmico apropriado. Toda família de filmes foi fabricada sobre substrato de silício (100) e submetida a tratamento termico. A diferença de um filme para outro esta na quantidade de material depositado. Isto possibilitou o estudo das propriedades supracitadas em função da quantidade de material depositado para fabricação do filme. A cristalinidade de todas as amostras obtidas foi confirmada por difração de raios-X (XRD). A microscopia eletrônica de varredura (MEV) mostrou filmes granulares com boa homogeneidade e que a espessura de todas as amostras aumenta com a quantidade de gotas depositadas durante o spin‐coating. As propriedades magnéticas foram medidas usando magnetometria de amostra vibrante (VSM). O campo aplicado durante a medicao foi orientado paralelo ao plano do filme e observou‐se uma alta coercividade e que esta diminui quase linearmente com o aumento de temperatura. / In this work we have made a study of the structural and magnetic properties of cobalt chromite granular films over silicon substrate. Here the films were fabricated by the chemical method sol‐gel, spin coating technique and ppropriate heat treatment. The entire Family was deposited over silicon substrate (100) and submitted to heat treatment. The difference between a film to another is the quantity of deposited Material. This allowed the study of the above properties as a function of the deposited material. The crystallinity of all samples obtained was confirmed by X‐ray diffraction (XRD). The scanning electron microscopy (SEM) showed granular films with good homogeneity and the thickness of all samples increases when the number of drops increases during spin‐coating. The magnetic properties were measured using vibrating sample magnetometry (VSM). The applied field during the measurement was Oriented parallel to the film plane and observed a high coercivity and that decreases pproximately linearly with increasing temperature.

Conventional liquid lubricants are faced with limitations under extreme cyclic operating conditions, such as in applications that require lubrication when changing from atmospheric pressure to ultrahigh vacuum and ambient air to dry nitrogen (e.g., satellite components), and room to elevated (>500°C) temperatures (e.g., aerospace bearings). Alternatively, solid lubricant coatings can be used in conditions where synthetic liquid lubricants and greases are not applicable; however, individual solid lubricant phases usually perform best only for a limited range of operating conditions. Therefore, solid lubricants that can adequately perform over a wider range of environmental conditions are needed, especially during thermal cycling with temperatures exceeding 500°C. One potential material class investigated in this dissertation is lubricious oxides, because unlike other solid lubricant coatings they are typically thermodynamically stable in air and at elevated temperatures. While past studies have been focused on binary metal oxide coatings, such as ZnO, there have been very few ternary oxide and no reported quaternary oxide investigations. The premise behind the addition of the third and fourth refractory metals Ti and Zr is to increase the number of hard and wear resistant phases while maintaining solid lubrication with ZnO. Therefore, the major focus of this dissertation is to investigate the processing-structure-tribological property relations of composite ZnO, TiO2 and ZrO2 phases that form ternary (ZnTi)xOy and quaternary (ZnTiZr)xOy nanocrystalline coatings. The coatings were processed by atomic layer deposition (ALD) using a selective variation of ALD parameters. The growth structure and chemical composition of as-deposited and ex situ annealed ternary and quaternary oxide coatings were studied by combined x-ray diffraction/focused ion beam microscopy/cross-sectional transmission electron microscopy, and x-ray photoelectron spectroscopy/Auger electron spectroscopy, respectively. It was determined that the structure varied from purely nanocrystalline (ternary oxides) to composite amorphous/nanocrystalline (quaternary oxides) depending on ALD parameters and annealing temperatures. In particular, the ZnTiO3 ilmenite phase with (104) textured nanocolumnar grains, exhibiting high stacking fault/partial dislocation densities >1012/cm2, was responsible for the excellent tribological behavior. Steady-state sliding friction coefficients down to 0.12 in humid air and 0.2 in dry nitrogen were measured along with sliding and fretting wear factors in the range of 10-6 to 10-7 mm3/N·m, even after ex situ annealing to 550°C. Additionally, the quaternary oxide phase Zn(Ti,Zr)O3 in solid solution exhibited a low fretting wear rate of 1x10-6 mm3/N·m. In contrast, certain phases, such as Zn2TiO4 cubic spinel, that form at annealing temperatures >550°C were responsible for high friction and wear. Mechanistic studies using the above techniques revealed low friction and wear-reducing surfaces and subsurfaces were due to different velocity accommodation modes (VAM). In the case of the ternary system, sliding-induced plastic deformation was possible when ZnTiO3 (104) stacking faults, bordered by partial dislocations, serve as a pathway for the dislocations to glide parallel to the sliding direction and hence achieve low friction and wear via an intrafilm shear VAM. It was evident that the individual nanocolumnar ZnTiO3 grains were plastically sheared as opposed to being fractured during wear. Conversely for the quaternary system, an interfacial sliding VAM between the counterface and a mechanically mixed layer (tribofilm) composed of the refined coating and counterface material, that also served as a source for the formation of cylindrical rolls, was responsible for wear reduction. Therefore, these lubricious oxides are a potential candidate for solid lubrication at high temperatures (up to 550 °C) and in space environments.

This diploma thesis discusses laser cutting and the consecutive surface treatment of cut parts. The theory of laser cutting is described in the first part of this thesis, including laser history and the laser emergence principle. Cut parameters and the influence of the laser cutting on the material are described later on. The next part describes the laser cutting technological possibilities and other laser technology utilization options are outlined. In the last theory part, metal surface treatment used in the experiment is covered. Coating thickness is evaluated in the practical part of this thesis, as well as roughness, microhardness, chemical microanalysis and metalography. The evaluation of the results achieved, and optimal surface treatment execution suggestions are addressed in the last part of this thesis.

No description available.

The global market for waterborne coatings will continue to grow because alternative solventborne coatings emit environmentally hazardous volatile organic compounds (VOCs). However, most waterborne coatings are softer than solventborne crosslinked thermoset coatings because they feature thermoplastic polymer dispersions. To overcome these challenges, in this thesis we suggest a novel crosslinkable aqueous dispersion system that incorporates epoxy and amine particles into poly(methyl methacrylate) (PMMA); the particles will react when water (the solvent) evaporates, offering a potential one-component (1K) reactive system. Emulsion polymerization was used to synthesize the particles with the help of surfactants. Epoxy and amine particles were successfully incorporated during the synthesis of PMMA and formed a two-component (2K) aqueous dispersion. In this process, a non-ionic surfactant, Triton X405 (TX405), was used to prevent interactions with the amine particles. Nuclear magnetic resonance (NMR) was used to determine the actual incorporation ratios of epoxy and amine and we found an epoxy incorporation plateau. Dynamic light scattering (DLS) was used to determine the particle size distributions and a uniform distribution was observed. The pendulum test and the pencil test were used for coating hardness, which surpassed currently marketed waterborne coatings. The resulting aqueous dispersions could be cured under facile conditions, i.e., in air and at low temperatures. An increase in Tg was observed after crosslinking. Different mechanical properties were observed when the coatings were cured at different temperatures, 25°C, 70°C, and 100°C. These results suggest that we have successfully formed crosslinked coatings that contain our epoxy and amine incorporated particles, with mechanical properties comparable to the traditional solventborne coatings.

No description available.

High operation speeds and thin coating films are desirable in many industrial applications. But the quality of the product, which is primarily determined by an optimum process window, is affected by non-uniformities and instabilities originating at higher operation speeds. Unlike other academic works, because of associated industrial relevance, particular attention was given towards the use of industrially relevant coating systems or generation of model fluids, which replicate the real coating solutions. One of the novelties of the research proposed lie in an integrated approach, utilising a range of comparative rheometrical techniques, with a focus on measurement of: (i) high strain rate shear viscosity [η], (ii) high strain rate uniaxial extensional viscosity [ηE] (iii) high strain rate elasticity (N1). Deformable roll coating, in terms of classification, is the ultimate metered coating flow. The flow is controlled by the combination of hydrodynamic force and elastic deformation effect, which could be complicated by the presence of non-Newtonian fluid. This study necessitated the design and construction of a sophisticated deformable coating rig with the ability to operate over a wide range of conditions. Although the irregularities and instabilities associated with the roller coating process has been studied previously, the concerned speeds of operation in this study is around three times higher. The main objectives of this study was to carry out a comprehensive experimental programme establishing relationship exist between film thickness, film quality and operating parameters. Main identified operating parameters are roll speeds, roll gaps or applied load between the rolls, the elasticity with thickness of elastomeric layer and different rheological properties of the coating fluids. Surface instabilities and air entrainment are identified as the major limitations to being able to coat at higher speeds. / Tata Steel Europe / The full text was made available at the end of the embargo, 1st July 2020

Coating onto a moving substrate several films simultaneously on top of each other is a challenging exercise. This is due to the fact, depending on operating conditions (thickness and velocity of individual layers and the physical properties of the coating fluids), flow instabilities may arise at the interfaces between the layers and on the top layer. These instabilities ruin the application of the final multi-layered coating and must be avoided. This research addresses this coating flow situation and seeks to develop guidelines to avoid these instabilities. Following a critical literature survey, this thesis presents a novel experimental method that visualises multi-layered coating flow down an inclined multi-slot die. The visualisation is obtained using a unique configuration including a high-speed camera, telecentric objective lens and illumination. The results show for a single layer, as the die angle and Reynolds number increases, the flow becomes more unstable and for a dual layer flow, as Re increases the peak to peak amplitude and the frequency decreases at the free surface and interface. The latter was unexpected and does not conform with existing literature. The triple layer results show either a monotonically increasing or increasing from first to second layer viscosity stratifications are the most stable flows along with flow heights in the first and second layers of <22% and >18% of the total thickness respectively, which concur with current literature. The visualisation additionally obtained other instabilities including single layer back-wetting and vortices, and multilayer slot invasion with the findings concurring with current literature. / EPRSC/Tata Steel Industrial CASE Studentship; EP/J501840/1

Yes / This study examines experimentally and for the first time the effect of reduced air pressure on dynamic wetting. The purpose is to assess the role of air viscosity on dynamic wetting failure which hitherto has been speculated on but not measured. In this paper we used dip coating as the model experimental flow and report data on air entrainment velocity Vae we measured with a series of silicone oils in a range of viscosities in a vacuum chamber where the pressure can be reduced from atmospheric down to a few mbar when the mean molecular free path of air is large and air ceases to have a viscosity. To complement earlier work, we carried out the experiments with a range of substrates of varying roughness. The substrates were chosen so that for each one, their two sides differ in roughness. This enables simultaneous comparative observation of their wetting performance and reduces the experimental error in assessing the role of roughness. The data presented here capture the effects of viscosity, roughness and air pressure but the important result of this study is that Vae can be increased considerably (exponentially) when the pressure is reduced with the suggestion that Vae approaches infinity as pressure approaches zero. In other words, the role of the surrounding air viscosity is important in dynamic wetting. The data from this study have significant implication to the fundamental understanding of dynamic wetting. Indeed they form the missing data link to fully understand this phenomenon. The data presented in this work also confirm the complex role of roughness, in that it can increase or decrease the air entrainment speed depending on the value on the viscosity of the coating solution. The results presented in this paper are very useful in practice as they imply that if one chooses carefully roughness one can coat viscous formulation at unexpectedly very high speeds with a moderate vacuum (50 mbar typically).