Diagnóstico das espécies ativas do plasma usado em tratamentos termoquímicos do titânio

Plasma diagnostics by Optical Emission Spectroscopy were performed for electrical discharge in three gas mixture respecting the combinations z N2 y Ar x H2, z N2 y Ar x O2 e z N2 y Ar x CH4, in which the indexes z and y systematically vary from 1 to 4 and x varies from 0 to 4, every one has dimension SCCM, resulting in 80 combinations. From the all obtained spectrums, the species CH (387,1 nm), N2+ (391,4 nm), Hβ (486,1 nm), Hα (656,3 nm), Ar (750,4 nm), O (777,4 nm) e O (842,6 nm) were analyzed because of their abundance and importance on the kinetic of reaction from the plasma to surface, besides their high dependences on the gases flows. Particularly interesting z, y and x combinations were chosen in order to study the influence of active species on the surface modification during the thermochemical treatment. From the mixtures N2 Ar O2 e N2 Ar CH4 were chosen three peculiar proportions which presented luminous intensity profile with unexpected maximum or minimum values, denominated as plasma anomaly. Those plasma concentrations were utilized as atmosphere of titanium treatment maintaining constant the control parameters pressure and temperature. It has been verified a relation among luminous intensity associated to N2+ and roughness, nanohardness and O atoms diffusion into the crystalline lattice of treated titanium and it has been seen which those properties becomes more intense precisely in the higher points found in the optical profile associated to the N2+ specie. Those parameters were verified for the mixture which involved O2 gas. For the mixture which involves CH4 gas, the relation was determinate by roughness, number of nitrogen and carbon atoms diffused into the titanium structure which presented direct proportionality with the luminous intensity referent to the N2+ and CH. It has been yet studied the formation of TiCN phases on the surface which presented to be essentially directly proportional to the increasing of the CH specie and inversely proportional to the increasing of the specie N2+

Estudo sobre a redução aluminotérmica de Ta2O5 e TiO2 usando descarga de cátodo oco

In this study it was used two metallic oxides, Ta2O5 and TiO2, in order to obtain metallic powders of Ta and Ti through aluminothermic reduction ignited by plasma. Ta2O5 and TiO2 powders were mixed with Al in a planetary mill, using different milling times. A thermal analysis study (DTA and TG) was carried out, in order to know the temperature to react both the mixtures. Then, these mixtures were submitted to a hollow cathode discharge, where they were reacted using aluminothermic reduction ignited by plasma. The product obtained was characterized by XRD and SEM, where it was proven the possibility of producing these metallic particles, different from the conventional process, where metallic ingots are obtained. It was verified that the aluminothermic reduction ignited by plasma is able to produce metallic powders of Ta and Ti, and a higher efficiency was observed to the process with Ta2O5-Al mixtures. Among different microstructural aspects observed, it can be noted the presence of metallic nanoparticles trapped into an Al2O3 matrix, besides acicular structures (titanium) and dendritic structures (tantalum), which are a product characteristic from a fast cooling

Síntese, aplicação e avaliação do efeito do teor de fósforo da celulose fosfatada em argamassa de alvenaria com aditivo comercial a base de hidroxi-etil-metil celulose (HEMC)

Generally, cellulose ethers improves mortar properties such as water retention, workability and setting time, along with adherence to the substrate. However, a major disadvantage of the addition of cellulose ethers in mortars is the delay in hydration of the cement. In this paper a cellulose phosphate (Cp) was synthesized water soluble and has been evaluated the effect of their incorporation into mortar based on Portland cement. Cellulose phosphate obtained was characterized by spectrophotometry Fourier transform infrared (FTIR), X-ray diffraction (XRD), elemental analysis and scanning electron microscopy (SEM). Mortar compositions were formulated with varying phosphorus content in cellulose and cellulose phosphate concentrations, when used in partial or total replacement of the commercial additive based hydroxyethyl methyl cellulose (HEMC). The mortars formulated with additives were prepared and characterized by: testing in the fresh state (consistency index, water retention, bulk density and air content incorporated) and in the hardened state (absorption by capillarity, density, flexural and compression strength). In mixtures the proportion of sand:cement of 1:5 (v / v) and factor a / c = 1.31 and water were held constant. Overall, the results showed that the celluloses phosphates employed in mortars added acted significantly when partially substituting the commercial additive. With regard to consistency index, water retention and bulk density in the fresh state and absorption by capillarity and bulk density apparent in the hardened state, showed no appreciable differences as compared to the commercial additive. The incorporated air content in the fresh state reduced markedly, but did not affect other properties. The mortars with cellulose phosphate, partially replacing the commercial additive showed an improvement of the properties of flexural strength and compressive strength

Desenvolvimento de um sistema misto de pasta à base de geopolímero e cimento portland para correção de perda de circulação

The materials engineering includes processes and products involving several areas of engineering, allowing them to prepare materials that fulfill the needs of various new products. In this case, this work aims to study a system composed of cement paste and geopolymers, which can contribute to solving an engineering problem that directly involves the exploitation of oil wells subject to loss of circulation. To correct it, has been already proposed the use of granular materials, fibers, reducing the drilling fluid or cement paste density and even surface and downhole mixed systems. In this work, we proposed the development of a slurry mixed system, the first was a cement-based slurry and the second a geopolymer-based slurry. The cement-based slurry was formulated with low density and extenders, 12.0 ppg (1.438 g/cm ³), showing great thixotropic characteristics. It was added nano silica at concentrations of 0.5, 1.0 and 1.5 gps (66.88, 133.76 and 200.64 L/m3) and CaCl2 at concentrations of 0.5, 1, 0 and 1.5%. The second system is a geopolymer-based paste formulated from molar ratios of 3.5 (nSiO2/nAl2O3), 0.27 (nK2O/nSiO2), 1.07 (nK2O/nAl2O3) and 13.99 (nH2O/nK2O). Finally, we performed a mixture of these two systems, for their application for correction of circulation lost. To characterize the raw materials, XRD, XRF, FTIR analysis and titration were performed. The both systems were characterized in tests based on API RP10B. Compressive strength tests were conducted after curing for 24 hours, 7 and 28 days at 58 °C on the cement-based system and the geopolymer-based system. From the mixtures have been performed mixability tests and micro structural characterizations (XRD, SEM and TG). The results showed that the nano silica, when combined with CaCl2 modified the rheological properties of the cement slurry and from the concentration of 1.5 gpc (200.64 L / m³) it was possible to obtain stable systems. The system mixture caused a change in the microstructure of the material by favoring the rate of geopolymer formation to hinder the C3S phase hydration, thus, the production of CSH phases and Portlandite were harmed. Through the mixability tests it can be concluded that the system, due to reduced setting time of the mixture, can be applied to plug lost circulation zones when mixed downhole

Avaliação da atividade fungicida de óleos essenciais e suas substâncias ativas no controlo de fungos de armazenamento

Mestrado em Engenharia Agronómica - Proteção da Plantas - Instituto Superior de Agronomia - UL

Produção de hortaliças de folha para processamento minimo. Estágio curricular na unidade fabril de processamento minimo de hortofrutícolas CAMPOTEC

Mestrado em Engenharia Alimentar - Instituto Superior de Agronomia - UL

Efeito da adição do poli(etileno acrilato de metila) (ema) e da fibra de linter de algodão nas propriedades do poli(tereftalato de etileno) reciclado (petrec)

The development of new materials to fill the demand of technological advances is a challenge for many researchers around the world. Strategies such as making blends and composites are promising alternatives to produce materials with different properties from those found in conventional polymers. The objective of this study is to evaluate the effect of adding the copolymer poly(ethylene methyl acrylate) (EMA) and cotton linter fibers (LB) on the properties of recycled poly(ethylene terephthalate) (PETrec) by the development of PETrec/EMA blend and PETrec/EMA/LB blend composite. In order to improve the properties of these materials were added as compatibilizers: Ethylene - methyl acrylate - glycidyl methacrylate terpolymer (EMA-GMA) and maleic anhydride grafted polyethylene (PE-g-MA). The samples were produced using a single screw extruder and then injection molded. The obtained materials were characterized by thermogravimetry (TG), melt flow index (MFI) mensurements, torque rheometry, pycnometry to determinate the density, tensile testing and scanning electron microscopy (SEM). The rheological results showed that the addition of the EMA copolymer increased the viscosity of the blend and LB reduces the viscosity of the blend composite. SEM analysis of the binary blend showed poor interfacial adhesion between the PETrec matrix and the EMA dispersed phase, as well as the blend composite of PETrec/EMA/LB also observed low adhesion with the LB fiber. The tensile tests showed that the increase of EMA percentage decreased the tensile strength and the Young s modulus, also lower EMA percentage samples had increased the elongation at break. The blend composite showed an increase in the tensile strength and in the Young`s modulus, and a decrease in the elongation at break. The blend formulations with lower EMA percentages showed better mechanical properties that agree with the particle size analysis which showed that these formulations presented a smaller diameter of the dispersed phase. The blend composite mechanical tests showed that this material is stronger and stiffer than the blend PETrec/EMA, whose properties have been reduced due to the presence of EMA rubbery phase. The use of EMA-GMA was effective in reducing the particle size of the EMA dispersed phase in the PETrec/EMA blend and PE-g-MA showed evidences of reaction with LB and physical mixture with the EMA

Development of a novel platform for high-throughput gene design and artificial gene synthesis to produce large libraries of recombinant venom peptides for drug discovery

Tese de Doutoramento em Ciências Veterinárias na Especialidade de Ciências Biológicas e Biomédicas

Comportamento ao corte e à flexão de vigas com betões incorporando nanopartículas

Existe uma crescente preocupação com a sustentabilidade e com o impacto ambiental da atividade da construção que, desde o início do séc. XXI, com o avanço exponencial da nanotecnologia e do estudo das nanopartículas (para incorporação em argamassas e betões), tem vindo a ser atendida de uma forma inovadora. As nanopartículas, quando substituindo pequenas percentagens da massa de cimento, conferem características melhoradas às misturas: resistência, durabilidade, entre outras. Os potenciais benefícios no betão são variados e estão, genericamente, identificados. Todavia, existem ainda algumas lacunas (e.g. estudos que incluam ensaios estruturais). Tendo este aspeto em conta, foi formado um consórcio entre a empresa Smart Inovation, Lda e o Instituto Superior de Engenharia de Coimbra por forma a conduzir uma investigação com o intuito de estudar o efeito da incorporação das nanopartículas em argamassas e betões. Inserindo-se a presente dissertação no âmbito desse projeto de investigação, decidiu-se estudar o comportamento de vigas de betão incorporando nanopartículas (ou nanobetão) quando sujeitas a esforços de corte e de flexão, comparando-o com o de betões de referência. Foram, então, realizados dois tipos de ensaios, para as mesmas misturas (que incluem betões simples, com nanopartículas, com fibras e com nanopartículas e fibras em conjunto): (i) ao corte – em que se submeteram oito vigas, simplesmente apoiadas, à aplicação de uma carga concentrada a 0,85 m do apoio mais afastado; (ii) à flexão – em que se submeteram também oito vigas, simplesmente apoiadas, à aplicação de uma carga concentrada a meio vão. Com base nos dados recolhidos durante os ensaios experimentais, estudou-se: a relação carga-deslocamento, os valores teóricos e experimentais do esforço transverso e do momento, a curvatura, a rigidez, a fendilhação e o tipo de rotura. Da análise de resultados, foi possível observar que o comportamento estrutural de vigas de betão incorporando nanopartículas não evidencia, de forma clara, as previsões dos ensaios de caracterização dos betões. Porém, verificou-se que existe alguma potencialidade da incorporação das nanopartículas (principalmente as nanopartículas de Al2O3) beneficiarem a resistência ao corte e à flexão. Foi ainda possível observar que a interação entre nanopartículas e fibras de aço induz efeitos negativos na resistência ao corte e a resistência à flexão

Betão betuminoso temperado com betume aditivado em refinaria

Ao longo dos tempos, tem-se vindo a verificar maior preocupação e consciência ambientais, pelo que os organismos e associações independentes têm procurado sensibilizar as empresas e os governos a nível mundial para um consumo mais racional da energia, tendo em vista uma menor emissão de dióxido de carbono para a atmosfera. Neste contexto, as tecnologias de pavimentação têm evoluído no sentido ecológico, isto é, de modo a terem menos impactes ambientais e a serem economicamente viáveis. As misturas betuminosas não são exceção desses avanços tecnológicos, tendo surgido as misturas betuminosas temperadas com o objetivo de contribuírem para a redução do consumo de energia e de emissões face às misturas convencionais. A sustentabilidade ambiental só pode consolidar-se através do desenvolvimento de tecnologias de produção ambientalmente mais adequadas, evitando desta forma comprometer o bem-estar das futuras gerações. Atualmente, as misturas betuminosas temperadas não conseguiram ainda uma posição de destaque face às misturas convencionais, dado que os agentes que as utilizam mantem ainda alguma desconfiança relativamente à performance desta tecnologia comparativamente às convencionais, pelo que é primordial demonstrar que o seu desempenho mecânico é adequado e semelhante ao das misturas produzidas a quente. Assim, o objetivo deste trabalho é realizar um estudo exploratório de algumas características de uma mistura betuminosa temperada produzida com um betume aditivado em refinaria e que, portanto, dispensa o uso de outros aditivos para baixar a temperatura de manipulação. Neste documento faz-se um breve enquadramento e uma abordagem histórica da evolução das misturas betuminosas temperadas e descrevem-se as diferentes tecnologias e técnicas de produção, abordando os seus benefícios e desvantagens, e indicando as propriedades típicas das mesmas. Em seguida apresentam-se os estudos laboratoriais para avaliação das diferentes propriedades volumétricas e o comportamento mecânico da mistura. Inclui-se também, sempre que possível, uma comparação das propriedades obtidas com resultados obtidos em misturas betuminosas a quente semelhantes, de forma a mostrar a aplicabilidade das MBT.

Compósitos de matriz metálica à base níquel com adição de TaC e NbC produzidos via metalurgia do pó

Carbide reinforced metallic alloys potentially improve some important mechanical properties required for the overall use of important engineering materials such as steel and nickel. Nevertheless, improved performance is achieved not only by composition enhancement but also by adequate processing techniques, such as novel sintering methods in the case of powder metallurgy. The method minimizes energy losses in addition to providing uniform heating during sintering. Thus, the general objective of this study was to evaluate the density, hardness, flexural strength, dilatometric behavior and to analyze the microstructure of metal matrix composites based nickel with addition of carbides of tantalum and / or niobium when sintered in a conventional furnace and Plasma assisted debinding and sintering (PADS). Initially, were defineds best parameters of granulation, screening and mixing procedure. After, mixtures of carbonyl Ni and 5%, 10% and 15 wt.% NbC and TaC were prepared in a Y-type mixer under wet conditions during 60 minutes. The mixtures were then dried and granulated using 1.5 wt. % paraffin diluted in hexane. Granulates were cold pressed under 600 MPa. Paraffin was then removed from the pressed pellets during a pre-sintering process carried out in a tubular furnace at 500 °C during 30 min. The heating rate was 3 ºC/min. The pellets were then sintered using either a plasma assisted reactor or a conventional resistive tubular furnace. For both methods, the heating rate was set to 8 ºC/min up to 1150 °C. The holding time was 60 minutes. The microstructure of the sintered samples was evaluated by SEM. Brinell hardness tests were also carried out. The results revealed that higher density and higher hardness values were observed in the plasma-assisted sintered samples. Hardness increased with the concentration of carbides in the Ni-matrix. The flexural strength also increased by adding the carbides. The decline was larger for the sample with addition of 5% 5% TaC and NbC. In general, compositions containing added carbide 10% showed less porous and more uniform distribution of carbides in the nickel matrix microstructural appearance. Thus, both added carbide and plasma sintering improved density, hardness, flexural strength and microstructural appearance of the composites

Estudo da aderência e fendilhação em elementos de betão incorporando nanopartículas

Com o crescimento progressivo da preocupação quanto ao consumo energético a nível global e a sua redução, por consequência das alterações climáticas, tem havido uma tentativa de adaptação do setor da construção para dar um contributo neste campo. O betão armado, pelas suas características e pela facilidade com que é moldado, estabeleceu com o Homem uma “amizade” duradoura. Atualmente é o material mais consumido a nível mundial, com uma produção de, aproximadamente, 10km3/ano, prevendo-se que este número venha a aumentar nos próximos anos. A sua produção necessita de um elevado consumo energético, principalmente na produção de um dos seus constituintes, o cimento. Mantendo-se a utilização generalizada do betão, uma potencial solução para este problema passa então pela redução do consumo deste elemento. Uma alternativa possível e que, nos últimos anos, ganhou relevo, prende-se com a introdução de nanotecnologia na produção do betão. A progressiva substituição do cimento Portland, por outro elemento capaz de fornecer as mesmas características às peças de betão, é uma necessidade, surgindo a introdução de nanopartículas como um caminho possível para esse objetivo. A alteração da composição do betão com a introdução de nanopartículas, acarreta consigo uma possível alteração do comportamento estrutural de elementos de betão armado, devido às alterações das propriedades do próprio betão. Este trabalho teve como motivação principal o estudo da influência deste “novo” betão na aderência aço-betão. Para a análise deste fenómeno, foram definidas duas etapas de estudo, sendo a primeira a produção de ensaios de arrancamento (Pull Out) para medir a tensão de aderência máxima e a segunda a realização de testes em tirantes com o objetivo de medir o padrão de fendilhação nestes elementos. Foram produzidas várias misturas de betão contendo dois tipos de nanopartículas (nano-sílica e nano-alumínio), incorporando também fibras metálicas. O estudo da aderência através do programa experimental apresentado, teve ainda como variáveis o uso de varões lisos e nervurados. No total foram realizados trinta e dois ensaios de arrancamento e dezasseis ensaios de tração com tirantes de betão armado. Os resultados obtidos demonstraram que a introdução de nanopartículas na composição do betão origina algumas diferenças de comportamento, relativamente ao betão normal. Nalguns casos os resultados foram algo inesperados. O trabalho desenvolvido no âmbito desta tese estava enquadrado num projeto mais amplo, designado por Nanobetão, promovido por um consórcio estabelecido entre o Instituto Superior de Engenharia de Coimbra e a empresa Smart Inovation.

Formulação e análise de desempenho de UHPC reforçado com fibras não metálicas

A evolução dos betões, na procura de estruturas com um maior tempo de vida útil, melhor desempenho ou menores custos de manutenção, tem sido alvo de pesquisa por investigadores de todo o mundo. Neste sentido, o desenvolvimento dos betões de ultra-elevado desempenho (UHPC – Ultra High Performance Concrete), permitiu, desde o seu desenvolvimento inicial, uma multiplicidade de aplicações quer a nível estrutural ou arquitetónico, aportando a estes elementos, vantagens características deste material de construção. No entanto, e particularizando um dos seus constituintes, a aplicação tradicional de fibras metálicas na composição de UHPC, poderá originar alguns fenómenos indesejados de perda de durabilidade, nomeadamente por corrosão destas. Por consequência, julga-se pertinente encontrar alternativas a este componente, de forma a que se obtenha um nível de desempenho semelhante, diminuindo o risco de ocorrência dos fenómenos anteriormente referidos. Neste sentido, o estudo que aqui se apresenta, visa efetuar uma breve abordagem à aplicação de fibras em materiais alternativos tais como fibra de vidro ou fibra de polipropileno. Serão analisadas algumas propriedades em estado fresco e endurecido de várias misturas de betão, com diferentes aplicações de fibras, quer em tipo, quer em dosagem.

Estudo de inibidores de corrosão em concreto armado, visando a melhoria na sua durabilidade

This thesis has as objective presents a methodology to evaluate the behavior of the corrosion inhibitors sodium nitrite, sodium dichromate and sodium molybdate, as well as your mixture, the corrosion process for the built-in steel in the reinforced concrete, through different techniques electrochemical, as well as the mechanical properties of that concrete non conventional. The addition of the inhibitors was studied in the concrete in the proportions from 0.5 to 3.5 % regarding the cement mass, isolated or in the mixture, with concrete mixture proportions of 1.0:1.5:2.5 (cement, fine aggregate and coarse aggregate), superplasticizers 2.0 % and 0.40 water/cement ratio. In the modified concrete resistance rehearsals they were accomplished to the compression, consistence and the absorption of water, while to analyze the built-in steel in the concrete the rehearsals of polarization curves they were made. They were also execute, rehearsals of corrosion potential and polarization resistance with intention of diagnose the beginning of the corrosion of the armors inserted in body-of-proof submitted to an accelerated exhibition in immersion cycle and drying to the air. It was concluded, that among the studied inhibitors sodium nitrite , in the proportion of 2.0 % in relation to the mass of the cement, presented the best capacity of protection of the steel through all the studied techniques and that the methodology and the monitoring techniques used in this work, they were shown appropriate to evaluate the behavior and the efficiency of the inhibitors

Aplicação da metodologia de planejamento de experimentos para formulação de massas cerâmicas para telhas

Rio Grande do Norte State stands out as one great producer of structural clay of the brazilian northeastern. The Valley Assu ceramic tiles production stands out obtained from ilitics ball clays that abound in the region under study. Ceramics formulation and the design of experiments with mixture approach, has been applied for researchers, come as an important aid to decrease the number of experiments necessary to the optimization. In this context, the objective of this work is to evaluate the effects of the formulation, temperature and heating rate in the physical-mechanical properties of the red ceramic body used for roofing tile fabrication of the Valley Assu, using design of mixture experiments. Four clays samples used in two ceramics industry of the region were use as raw material and characterized by X-ray diffraction, chemical composition, differential thermal analysis (DTA), thermogravimetric analysis (TGA), particle size distribution analysis and plasticity techniques. Afterwards, they were defined initial molded bodies and made specimens were then prepared by uniaxial pressing at 25 MPa before firing at 850, 950 and 1050 ºC in a laboratory furnace, with heating rate in the proportions of 5, 10 e 15 ºC/min. The following tecnologicals properties were evaluated: linear firing shrinkage, water absorption and flexural strength. Results show that the temperature 1050 ºC and heating rate of 5 ºC/min was the best condition, therefore presented significance in all physical-mechanical properties. The model was accepted as valid based of the production of three new formulations with fractions mass diferents of the initial molded bodies and heated with temperature at 1050 ºC and heating rate of 5 ºC/min. Considering the formulation, temperature and heating rate as variables of the equations, another model was suggested, where from the aplication of design of experiments with mixtures was possible to get a best formulation, whose experimental error is the minor in relation to the too much formulations