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Efeito do conteúdo de titânia e da alteração da superfície por meio da aplicação do recobrimento biomimético nas propriedades mecânicas do compósito Y-TZP/TiO2 / Effect of titania content and the change of the surface by applying the biomimetic coating on the mechanical properties of the composite Y-TZP/TiO2Miranda, Ranulfo Benedito de Paula 18 July 2014 (has links)
Os objetivos desse trabalho foram: 1) determinar o efeito do conteúdo de titânia em mol % (zero, 10 e 30) na área de superfície específica (SBET), no tamanho dos aglomerados e na intensidade dos picos correspondentes às fases cristalinas presentes no pó cerâmico de Y-TZP/TiO2; 2) determinar o efeito do conteúdo de titânia em mol % (zero, 10 e 30) na microestrutura, densidade, densidade relativa, módulo de elasticidade, coeficiente de Poisson, módulo de Weibull (m) e resistência à flexão (f) de pastilhas cerâmicas sinterizadas de Y-TZP/TiO2 e, 3) determinar o efeito do recobrimento biomimético no módulo de Weibull (m) e na resistência á flexão de pastilhas cerâmicas sinterizadas de Y-TZP/TiO2. Os pós foram produzidos por meio de uma rota de co-precipitação, obtendo-se três composições do compósito Y-TZP/TiO2, que foram de zero (T0), 10 (T10) e 30 (T30) % mol de titânia. O pó produzido foi prensado (50 MPa) para produzir pastilhas de 15 mm de diâmetro e sinterizado a 1400 °C por 2 horas. Após o polimento com solução diamantada de 45 m, as pastilhas (n=60 para cada grupo) ficaram com aproximadamente 12 mm de diâmetro e 1,0 mm de espessura. Metade das pastilhas foram submetidas ao recobrimento biomimético (sete dias em solução de silicato de sódio e sete dias em solução de 1,5 SBF-simulated body fluid). Os pós foram caracterizados por difração de raios-X (DRX), espalhamento a laser, adsorção gasosa e microscopia eletrônica de varredura (MEV). As pastilhas foram caracterizadas pelo método de Archimedes, pulso-eco ultra-ssônico, MEV, DRX e para a análise de Weibull, as pastilhas foram submetidas ao ensaio de resistência à flexão biaxial em saliva artificial a 37°C. Os resultados mostraram que todos os pós apresentaram zircônia monoclínica e tetragonal na sua composição e uma área de superfície específica superior a 42 m2/g. A adição de titânia favoreceu a formação de aglomerados maiores e com uma distribuição bimodal. Em todas as pastilhas foram detectadas zircônia monoclínica e tetragonal, enquanto no grupo T30 também foi detectada a fase de titanato de zircônia (ZrTiO4). O grupo T0 apresentou os maiores valores de densidade medida (6,05 g/cm3), densidade relativa (99,0%), módulo de elasticidade (213 GPa) e resistência à flexão (815 MPa). A adição de titânia reduziu significativamente a densidade medida (5,45 g/cm3 para T10 e 5,15 g/cm3 para T30) a densidade relativa (94,4% para T10 e 96,3% para o T30) o módulo de elasticidade (156 GPa para T10 e 134 GPa para o T30) e a resistência à flexão (455 MPa para o grupo T10 e 336 MPa para o grupo T30) do compósito Y-TZP/TiO2. O grupo T30 apresentou um módulo de Weibull (11,7) e um coeficiente de Poisson (0,34) significativamente superior ao grupo T0 (6,4 e 0,31, respectivamente). Foi observado que o recobrimento biomimético promoveu a formação de glóbulos de hidroxiapatita distribuídos de forma heterogênea na superfície do material e que esse tratamento não alterou significativamente a resistência à flexão e o módulo de Weibull do compósito Y-TZP/TiO2. Conclui-se que a adição de titânia afetou as propriedades estudas do pó e das pastilhas do compósito de Y-TZP/TiO2. Além disso, o compósito pode ser recoberto com uma camada hidroxiapatita sem ter sua confiabilidade estrutural afetada. / The objectives of this study were: 1) to determine the effect of titania content in mol% (zero, 10 and 30) in the specific surface area (SBET), the size of the agglomerates and the intensity of the peaks corresponding to crystalline phase present in the ceramic powder of Y-TZP/TiO2; 2) to determine the effect of the content in mol% of titania (zero, 10 and 30) in the microstructure, density, relative density, modulus of elasticity, Poisson\'s ratio, Weibull modulus (m) and flexural strength (f) of ceramic discs sintered from Y-TZP/TiO2 and 3) to determine the effect of biomimetic coating on the Weibull modulus (m) and the flexural strength of the sintered ceramic discs of Y-TZP/TiO2. The powders were produced by a co-precipitation route, in order to obtain the composite Y-TZP/TiO2 with three compositions, containing zero (T0), 10 (T10) and 30 (T30) mol% titania. The produced powder was pressed (50 MPa) into discs of 15 mm diameter and sintered at 1400 °C for 2 hours. After polishing with diamond solution of 45 m, the discs (n = 60 for each group) were approximately 12 mm in diameter and 1.0 mm-thick. Half of the discs were subjected to biomimetic coating (seven days with sodium silicate solution and seven days in 1,5 SBF-simulated body fluid solution ). The powders were characterized by X-ray diffraction (XRD), laser scattering, gas adsorption and scanning electron microscopy (SEM). The discs were characterized by the Archimedes method, ultrasonic pulse-echo, SEM, XRD and for the Weibull analysis, the discs were subjected to the test of biaxial flexural strength in artificial saliva at 37 °C. The results showed that all powders had monoclinic and tetragonal zirconia in their composition, and a specific surface area greater than 42 m2/g. The titania addition favored the formation of larger agglomerates and a bimodal distribution. In all discs monoclinic and tetragonal zirconia were detected, while in the T30 group zirconium titanate (ZrTiO4) was also detected. T0 group had the highest measured density (6,05 g/cm3), relative density (99,0%), elasticity modulus (213 GPa) and flexural strength (815 MPa). The addition of titania significantly reduced the measured density (5,45 g/cm3 for T10 group and 5,15 g/cm3 for T30 group), the relative density (94,4% for T10 group and 96,3% for T30 group), elasticity modulus (156 GPa for T10 group and 134 GPa for T30 group) and flexural strength (455 MPa for T10 group and 336 MPa for T30 group) of the Y-TZP/TiO2 the composite. The T30 group showed a Weibull modulus (11,7) and Poisson\'s ratio (0,34) significantly higher than those of T0 group (6,4 and 0,31). It was observed that the biomimetic coating resulted in the formation of apatite globules heterogeneously distributed on the surface of the material and that this treatment did not significantly alter the flexural strength and Weibull modulus of the composite Y-TZP/TiO2. It is concluded that the addition of titania affects the studied properties of the powder and discs of the composite Y-TZP/TiO2. Also, the composite can be coated with a layer of calcium phosphate without affecting its structural reliability.
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Influência de um revestimento de nióbio sobre a resistência à sulfetação das ligas FeCr e FeCrY / Influence of a niobium coating on sulfidation resistance of FeCr and FeCrY alloysGeribola, Guilherme Altomari 01 December 2014 (has links)
Nióbio e suas ligas são utilizados atualmente em muitas aplicações industriais por oferecerem excelente resistência à degradação em diversos meios corrosivos. Estes meios incluem atmosferas gasosas em temperaturas elevadas, como as encontradas em plantas de gaseificação de carvão existentes em usinas termelétricas para geração de energia. As atmosferas encontradas nestes meios são misturas gasosas complexasque contêm, entre outros compostos, oxigênio e enxofre. Os sulfetos são compostos menos estáveis, possuem pontos de fusão mais baixos e apresentam, freqüentemente, maiores desvios de estequiometria em relação ao óxido correspondente. Apesar de existirem estudos relacionados à aplicação de metais refratários em atmosferas sulfetantes a temperaturas elevadas, o uso de compostos de nióbio ainda não foi devidamente avaliado como revestimento protetor, havendo poucos dados disponíveis na literatura. O objetivo deste trabalho foi avaliar o efeito proporcionado por um filme de nióbio, obtido por pulverização catódica,sobre o comportamento de sulfetação isotérmica das ligas Fe-20Cr e Fe-20Cr-1Y.Os testes de sulfetação foram realizados a 500, 600 e 700°C pelo período de 2h em atmosfera H2/2%H2S. A avaliação da resistência à sulfetação foi feita por meio do ganho de massa por unidade de área exposta. Observou-se que o comportamento de sulfetação a 500ºC das ligas FeCr e FeCrY sem e com revestimento é similar. Nesta condição, nenhuma das ligas sofreu escamação. A 700ºC a liga FeCr sofreu leve escamação na forma de um pó fino, enquanto que o produto de reação formado sobre a liga FeCrY escamou na forma de placas. O efeito do nióbio se torna pronunciado a 700ºC. A camada de produto de reação formada sobre as ligas revestidas é mais fina e plástica que na liga sem revestimento. O ganho de massa por unidade de área diminuiu sensivelmente para as ligas recobertas, que não sofreram escamação. / Niobium and niobium based alloys are currently used in many industrial applications because they offer excellent resistance to degradation in various corrosive environments. These media include gaseous atmospheres at high temperatures such as those found in existing coal gasifying plants in power plants for energy generation. These atmospheres are complex gas mixtures that contain sulfur and oxygen, among other compounds. Sulphides are thermodynamically less stable, have lower melting points and often have larger deviations from stoichiometry compared to the corresponding oxides. Although there are studies regarding the use of refractory metals in high temperature sulphidizing atmospheres, the use of niobium compounds has not been adequately evaluated and there is very little studies available in the literature about its use as a protective coating. The aim of this study was to evaluate the effect of a niobium film, deposited by magnetron sputtering on the isothermal sulphidation behavior of Fe-20Cr and Fe-20Cr-1Y alloys. The sulphidation tests were carried out at 500, 600 and 700° C for 2h in H2/2% H2S atmosphere. The sulphidation resistance was determined by mass gain per unit area. The sulphidation behavior of the coated and uncoated alloys was similar at 500ºC, and none of the alloys spalled. At 700ºC FeCr alloy scalled in the form of a fine powder, while the reaction product formed on the alloy FeCrY scalled in the form of plates. The effect of niobium became pronounced at 700°C. The reaction product layer formed on the coated alloy was thinner andmore plastic than that formed on the uncoated alloy. The mass gain per unit area of the coated alloys decreased significantly and they did not scaled.
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Modificação da superfície de aço eletrozincado para proteção contra a corrosão por revestimentos isentos de cromo / Surface modification of electrogalvanized steel for protection against corrosion for coatings free chromeFerreira Júnior, José Mario 15 January 2014 (has links)
Os revestimentos eletrozincados empregados como proteção galvânica ativa sobre os aços são utilizados industrialmente há longo tempo. Entretanto, como o zinco é um elemento muito reativo, o tratamento da sua superfície é necessário para aumentar sua vida útil. O tratamento mais utilizado consiste em imersão em solução de conversão contendo cromo hexavalente, o qual vem sendo banido por gerar substâncias tóxicas e carcinogênicas, tendo sua utilização proibida pelas normas europeias. Neste trabalho, foram estudados tratamentos alternativos ao cromato para o aço eletrozincado que não geram resíduos tóxicos. O tratamento escolhido foi desenvolvido em etapas. A primeira etapa envolveu o uso de um composto orgânico, o 2 butino-1,4 diol propoxilato, em solução com sais oxidantes e com nitrato de cério como aditivo. A etapa seguinte consistiu em imersão da superfície tratada pela etapa anterior, em um agente oxidante, o peróxido de hidrogênio. A terceira etapa consistiu na imersão em solução com 2 butino-1,4 diol propoxilato e oxalato de nióbio amoniacal (ANO). As superfícies tratadas, após cada uma das etapas, foram caracterizadas por microscopia óptica e eletrônica de varredura (MEV), difração de raios X (DRX), espectroscopia por infravermelho (FTIR) e espectroscopia fotoeletrônica de raios X (XPS). A caracterização quanto à corrosão das superfícies tratadas foi feita por ensaios de névoa salina e espectroscopia de impedância eletroquímica (EIE). Os resultados mostraram que cada uma das etapas teve uma contribuição no aumento da resistência à corrosão e esta foi dependente do tempo de tratamento em cada uma das três etapas. A composição química das camadas obtidas foi caracterizada por FTIR e XPS. Esta última técnica permitiu analisar a distribuição dos elementos nas camadas formadas ao longo da espessura da mesma, usando a técnica de desbaste (sputtering), obtendo perfis de profundidade. A presença de ácido carboxílico ligado ao substrato metálico (zinco) foi observada. Os resultados mostraram que ocorreu formação de camada orgânica e a incorporação de cério e de nióbio a esta camada. Estes se apresentam distribuídos em toda a extensão da camada, na forma de óxidos em dois estados de oxidação, III e IV, no caso do cério, e IV e V, no caso do nióbio. As camadas formadas após as várias etapas adotadas contêm uma estrutura polimérica formada por filme orgânico e uma mistura de óxidos, particularmente óxido e hidróxido de zinco, os quais ficam retidos na estrutura da camada e conferem proteção à corrosão do substrato metálico por períodos prolongados de imersão. Os resultados quanto a proteção à corrosão mostraram que o tratamento com o melhor desempenho (T10_10_10) proporcionou proteção ao substrato por longos períodos de tempo e esta foi superior em comparação à promovida por camada de cromato, tanto pelo ensaio de névoa salina como o de EIE. Este tratamento mostrou-se, portanto, uma alternativa promissora para substituição de camada de cromato na proteção de aço eletrozincado, tanto do ponto de vista ambiental, por não gerar resíduos tóxicos, como de resistência à corrosão. / Electrogalvanized coatings are employed as active galvanic protection to steel and its applications have been used industrially for a long time. However, as zinc is a very reactive element, the treatment of the surface is necessary to increase its lifespan. The most common treatment consisted of a conversion treatment in solution containing hexavalent chromium, which has been banned by generating toxic and carcinogenic substances, and its use prohibited by European standards. In this work, surface treatments alternative to chromating for electrogalvanized steel that do not generate toxic waste were studied. The chosen treatment was developed in stages. The first stage involved the use of an organic compound, 2 butyne 1,4 diol propoxylate in solution with oxidizing salts and cerium nitrate as an additive. The next step involved immersing the treated surface by the previous step in an oxidizing agent, hydrogen peroxide. The third step consisted of immersion in solution with 2-butyne 1,4 diol propoxylate and ammonium niobium oxalate (ANO). Treated surfaces after each step were characterized by optical microscopy and scanning electron microscopy (SEM), X-ray diffraction (XRD), infrared spectroscopy (FTIR) and photoelectron spectroscopy X- ray (XPS). The characterization for corrosion of the treated surfaces was made by salt spray tests and electrochemical impedance spectroscopy (EIS). The results showed that each step has a contribution in increasing the corrosion resistance and this was dependent on the treatment time adopted in each of the three stages. The chemical composition of the layers obtained was characterized by FTIR and XPS. This last technique allowed to analyze the distribution of the elements in the layer formed along its thickness, by sputtering the surface to obtain depth profiling. The presence of carboxylic acid bonded to the metal substrate (zinc) was observed. The results showed that there was formation of organic layer and the incorporation of cerium and niobium this layer. These elements were distributed throughout the length of the layer in the form of oxides in two oxidation states; in the case of cerium, as III and IV, and IV and V, in the case of niobium. The layers formed after the various steps contain a polymeric structure and a mixture of oxides/hydroxide, particularly of zinc, which are retained in the structure of the layer and provide corrosion protection to the metal substrate for prolonged periods. The corrosion results showed that the best treatment (T10_10_10) provided protection to the substrate for long periods of time and that was higher compared to that promoted by the chromate layer, either by the salt spray test as the EIS test. Therefore, this treatment proved a promising replacement to chromate layer in the corrosion protection of electrogalvanised steel, either from its corrosion properties or from an environmental point of view.
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SURFACE ENGINEERING AND MONOMER DESIGN FOR LIGHT-MEDIATED RING OPENING METATHESIS POLYMERIZATIONFursule, Ishan A. 01 January 2018 (has links)
Stimuli-responsive materials are changing the landscape of actuated materials, optoelectronics, molecular machines, solar cells, temporary memory storage, and biomedical materials. Specifically, photo-responsive polymers have gained acceleration in research and application since the last two decades in the form of a surface coating and micro-patterns. Light as a stimulus can be coherent, mono or polychromatic, tunable for power (intensity) and energy (wavelength), and has precise spatiotemporal control. Conventional surface coating techniques such as spin coating are unable to impart properties to the coatings in terms of sturdiness, homogeneity, uniformity over the complex surface, post deposition modification, and process efficiency. Also, in the field of photoreponsive polymers, there is no simple technique for surface-patterning of photo-responsive polymers, which is an important missing link between current research and future potential applications.
This dissertation designs new strategies for light-mediated ring opening metathesis polymerization (ROMP) to synthesize a diverse class of stable photo-responsive polymers and coatings.
Firstly, we propose a new synthetic route to functionalize surface-initiated ring opening metathesis polymerization (SI ROMP) coatings. The backbone of ROMP polymers has internal carbon-carbon double bonds which are potential sites to introduce additional functionalities like stimuli-responsive functional groups. We leverage these unsaturated bonds to incorporate functionalized side chains using thiol-ene click chemistry. Thiol-ene chemistry is a versatile approach to attach diverse functional groups at the site of a carbon-carbon double bond. This approach was tested by grafting 3 types of thiols with different functional tail groups and can be readily used for any polyolefin coatings.
Secondly, oxidative degradation of SI ROMP coatings in the organic solvent is a common problem resulting in a decrease in the film thickness due to polymer chain cleavage. We incorporated a custom designed crosslinker to the polynorbornene (pNB) coatings to prepare in situ crosslinked pNB coatings. This approach provides a crosslinked coating of pNB with significantly increased stability against organic solvents by decreasing the film loss from 73 % to 28 %.
Lastly, a novel approach of making photo-responsive polymer by light mediated ROMP is demonstrated. Light mediated control over rate of polymerization is the key feature required for patterning surface with photoresponsive polymers. We achieved this goal by designing and synthesizing a monomer that effectively controls the activity of the catalyst by temporarily deactivating it on irradiation with UV 365 nm light and reactivating it back by irradiation with blue 455 nm light to resume the ROMP.
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Improvement of Electromagnetic Railgun Barrel Performance and Lifetime by Method of Interfaces and Augmented ProjectilesPavlov, Aleksey D 01 June 2013 (has links)
Several methods of increasing railgun barrel performance and lifetime are investigated. These include two different barrel-projectile interface coatings: a solid graphite coating and a liquid eutectic indium-gallium alloy coating. These coatings are characterized and their usability in a railgun application is evaluated. A new type of projectile, in which the electrical conductivity varies as a function of position in order to condition current flow, is proposed and simulated with FEA software. The graphite coating was found to measurably reduce the forces of friction inside the bore but was so thin that it did not improve contact. The added contact resistance of the graphite was measured and gauged to not be problematic on larger scale railguns. The liquid metal was found to greatly improve contact and not introduce extra resistance but its hazardous nature and tremendous cost detracted from its usability. The simulated resistivity augmented projectiles were able to mitigate harmful current build-up on the back of a projectile using different conductivity gradients. Within the range of conductivity of aluminum alloys no simulated gradient was able to fully level the current density, however, once the range was expanded to include the lower conductivity of titanium, nearly uniform current density was achieved.
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Mise en oeuvre et optimisation d'un revêtement conducteur poly(époxy) : fils submicroniques d'argent pour la protection foudre de structures aéronautiques / Processing and optimisation of a conductive poly(epoxy) : silver submicronic wires coating for lightning strike protection of aircraft structural composite partsBedel, Vincent 21 September 2018 (has links)
Ce travail s'inscrit dans une problématique de mise en œuvre et d'étude d'un revêtement conducteur polymère extrinsèque pour la protection foudre des structures aéronautiques de type composite polymère renforcé fibres de carbone (CFRP). Le revêtement est composé d'une matrice poly(époxy) haute performance bi-composant fluide à température ambiante et de fils submicroniques d'argent à haut facteur de forme (AgNWs) obtenus par un procédé polyol. Une attention particulière a été portée à l'étude de l'influence des AgNWs sur la modification de la cinétique de réticulation du système, sa structure physique et sa mobilité moléculaire. La mesure des niveaux de conductivité volumique et surfacique du revêtement met en avant un seuil de percolation électrique pour un taux volumique en AgNWs inférieur à 1%. Une approche originale permettant la détermination des mécanismes de conduction a été effectuée au moyen des mesures de densités de courant imposées dans le revêtement en fonction du taux de charge en AgNWs et de la température. L'analyse du comportement électrique des échantillons aux valeurs critiques de densités de courant a permis d'appréhender les phénomènes responsables des mécanismes de dégradation. Enfin des essais foudres ont été effectués sur des substrats représentatifs d'une structure aéronautique avec différents types de protection foudre. L'analyse des échantillons par ultrasons après essais foudres a mis en avant l'efficacité du revêtement composite polymère conducteur poly(époxy)/AgNWs développé pour lutter contre le délaminage structurel du CFRP. / This work deals with the processing and the study of an extrinsic conductive polymer coating for the lightning strike protection of the aircraft carbon fibre reinforced polymer (CFRP) structural parts. The coating consist in a low viscosity bi component high performance poly(epoxy) matrix and silver submicronic wires with a high aspect ratio (AgNWs) obtained by a polyol process. The kinetic parameters, the physical structure and the molecular mobility of the matrix had been investigated as a function of the filler content. The surface and bulk conductivities had been measured as a function of filler content. It exhibits a percolation threshold below 1% in volume. The conduction mechanisms had been studied following an uncommon method of current density measurement as a function of the AgNWs content and the temperature. The critical electrical behaviour of each sample had been investigated through the current density method. It has permitted to understand the phenomenon responsible for the composite's degradation. Finally, lightning strike tests on representative configurations had been carried out. The ultrasonic inspections have highlighted the efficiency of the poly(epoxy)/AgNWs coating to avoid the structural delamination of the CFRP.
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Electrical, Optical and Thermal Investigations of Cobalt Oxide-Antimony Doped Tin Oxide (CoO-ATO) Thin Films and Nanofiber MembranesRoy, Nirmita 02 November 2017 (has links)
The main aim of this thesis work is to investigate the electrical, optical and thermal impact characteristics of cobalt oxide doped antimony tin oxide (CoO-ATO) in the form of thin films and nanofiber membranes. CoO-ATO is a novel composite material that has the potential to be used as reinforced aircraft coatings, military garment coatings, or more specifically as an anti-reflective (AR) top coating for photovoltaic (PV) cells. This work will be critical in determining the effectiveness of using a CoO-ATO layer in these applications. Electrospun nanofibers and spin coated thin films consisting of a polymeric solution of CoO-ATO will be used. Thin films are created using spin coating techniques, and nanofiber membranes are created using an electrospinning technique. Polystyrene (PS) will be used as a solute, and chloroform as a solvent, to create the solution. It is hypothesized that coatings of this material will have improved optical characteristics as compared to traditional ATO coatings and minimum impact from thermal cycling making it a favorable candidate for PV cells. This work will do an electrical, optical and thermal cycling impact characterization of CoO-ATO thin films and nanofiber membranes for a doping range of x% CoO where x ranged from 0.2
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Sellado dentinario inmediato y resin coating como técnicas de protección dentinariaMaestri Fernández-Concha, Renato Stefano 14 December 2018 (has links)
El objetivo de esta revisión fue recopilar información sobre las técnicas de Sellado Dentinario Inmediato (SDI) y Resin Coating (RC) como incremento de las fuerzas de adhesión. Asimismo, el siguiente trabajo describe las principales características de cada técnica, así como sus ventajas y desventajas. / The aim of this review was to collect information about the Immediate Dental Sealing (IDS) and Resin Coating (RC) techniques to achieve an increase in bond strengths. Also, this article describes its main characteristics as well as advantages and disadvantages. / Tesis
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Efeito autorreparador em primer carregado com inibidor de corrosão encapsulado em haloisita. / Self-healing effect of primer loaded with corrosion inhibitor encapsulated in halloysite.Carvas, Gabriela Silva Ferreira 14 June 2019 (has links)
O objetivo deste trabalho é avaliar o efeito autorreparador de um primer alquídico base solvente (SB) e um primer acrílico base água (WB) aditivados com nanocontainers de haloisita carregados com inibidor de corrosão dodecilamina (DDA) aplicados em aço carbono. O efeito inibidor da dodecilamina foi avaliado através de ensaios eletroquímicos de espectroscopia de impedância eletroquímica (EIS) em diferentes condições, sendo verificada que a sua eficiência aumenta em meio ácido. Com o intuito de aumentar o lúmen da haloisita, gerando mais capacidade de carregamento de inibidor, a haloisita foi tratada com ácido sulfúrico 2 mol/L por 6 h a 55 °C. A haloisita tratada foi caracterizada através de análises termogravimétricas (TGA) e microscopia eletrônica de varredura (MEV). Em seguida, a dodecilamina foi carregada em haloisita tratada, através da técnica de pulso de vácuo. A cinética de liberação do inibidor de dentro da haloisita foi estudada através da técnica de EIS, onde foi constatada que a sua atuação é dependente do pH, com maior velocidade de liberação em pH 2. Os nanocontainers foram adicionados em um primer alquídico base solvente e um primer acrílico base água para a avaliação da resistência à corrosão dos sistemas através de espectroscopia de impedância eletroquímica (EIS), técnica de varredura com eletrodo vibratório (SVET) e ensaios acelerados de corrosão em câmara de névoa salina (SSC). A aderência dos dois sistemas foi avaliada através do ensaio de aderência por tração (pull-off). Para os dois sistemas avaliados foi possível verificar o efeito autorreparador, porém ele não foi tão longo, provavelmente devido à baixa eficiência no carregamento da dodecilamina na haloisita. A análise de custo da haloisita carregada com dodecilamina mostrou a necessidade de otimização dos processos de carregamento a fim de viabilizar o projeto na indústria de tintas. / The aim of this work is to evaluate the self-healing effect of a solvent based (SB) alkyd primer and a water based (WB) acrylic primer loaded with dodecylamine (DDA) corrosion inhibitor encapsulated in halloysite nanocontainers on carbon steel. The inhibitor effect of dodecylamine was evaluated by electrochemical impedance spectroscopy (EIS) under different conditions, and it was verified that its efficiency increases in acid medium. To enlarge halloysite lumen and increase its loading capacity, halloysite was treated with 2 mol/L sulfuric acid for 6 h at 55 °C. Halloysite before and after treatment was characterized by thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). Thereafter, the dodecylamine was loaded into treated halloysite by the vacuum pulse technique. The release kinetics of the inhibitor from within halloysite nanotubes were studied through the EIS technique where it was found that the action of halloysite is pH-dependent, with a higher release kinetics at pH 2. The nanocontainers were loaded in a solvent based alkyd primer and a water based acrylic primer for the evaluation of the corrosion resistance of the systems through electrochemical impedance spectroscopy (EIS), scanning vibration electrode technique (SVET) and accelerated corrosion tests in a salt spray chamber (SSC). The adhesion of the two systems was evaluated through the pull-off adhesion test. For the two systems evaluated, it was possible to verify the self-healing effect, but this effect was not long, probably due to the low loading efficiency of dodecylamine in halloysite nanotubes. The cost analysis of halloysite loaded with dodecylamine showed that the loading process needs an optimization in order to make this project feasible in the coating industry.
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Fonctionnalisation anti-bactérienne passive ou active de tissus textiles par voie sol-gel ou photochimique - L'association du TiO2 et de la chimie douce / Antibacterial functionalization of textile fabrics through sol-gel routesMessaoud, Mouna 11 February 2011 (has links)
Au cours de cette thèse, plusieurs approches de fonctionnalisation anti-bactérienne passive, de type"bactériostatique" utilisant des espèces hydrophobes, et active (selon un standard ISO), de type"bactéricide" utilisant des nanoparticules d’argent métallique ou des espèces à base d’ammoniumquaternaire, ont été testées sur des tissus textiles. Des solutions liquides ont été élaborées par voie sol-gelet photochimique, en association ou non. Elles ont tout d’abord été caractérisées d’un point de vuephysico-chimique, morphologique et structural, afin d’optimiser leur formulation et les caractéristiquesdes espèces en solution vis-à-vis de différents cahiers des charges industriels. Ce travail d’optimisation aen particulier conduit à des solutions stables permettant leur utilisation reproductible au cours du temps.Les solutions ont ensuite été imprégnées sur des échantillons textiles, par un dispositif simplifié de "padcoating"mis au point au cours de la thèse, afin de tester la fonction anti-bactérienne des textiles traités.Selon la nature des espèces imprégnées, l’optimisation des solutions conduit à une fonctionnalité antibactériennepassive ou active respectant l’aspect visuel du textile et ne dénaturant pas son toucher. Destests de lavage de laboratoire ou de lavage ménager en conditions réelles ont également montré unaccrochage notable des espèces imprégnées sur les textiles. Des options ont finalement été proposées pouraccroître cet accrochage afin de répondre à des conditions de lavage industriel. En conclusion, ce travail met en évidence le potentiel des approches d’élaboration par chimie douce en vue de fonctionnaliser des textiles, en permettant en particulier de proposer des méthodologies originales et simplifiées en adéquation avec des impératifs industriels. / In this thesis, several approaches have been tested for the passive ("bacteriostatic") and active (as definedby an ISO standard, "bactericidal") anti-bacterial fonctionalization of textile fabrics by using hydrophobicspecies and nanoparticles of metallic silver or quaternary ammonium species, respectively. Liquidsolutions were prepared by sol-gel and photochemistry methods, in association or not. Physicochemical,morphological and structural characterizations have first been realized to optimize the solutionformulations and the characteristics of active species in solutions towards various industrialspecifications. This optimization study has in particular led to stable solutions allowing their use inreproducible conditions over time. The optimized solutions were then imparted to textile samples, using asimplified "pad-coating device implemented during the thesis, in order to test the anti-bacterial functionof treated textiles. Depending on the nature of the species present on textiles, the optimized solutions ledto a passive or active anti-bacterial function while keeping the visual aspect and hand feeling of textiles.Laboratory washing tests or laundering washings in real conditions also showed a significant attachmentof impregnated species on textiles. Different options have finally been proposed to enhance thisattachment in order to fulfill industrial washing criteria. In conclusion, this thesis work highlights thepotential of soft chemistry approaches to functionalize textiles supports and enable us to propose originaland simplified methodologies in adequacy with industrial requirements.
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