Cobalt Ferrite has important, size-dependent magnetic properties. Consequently, an overview of particle size is important. Co-precipitation in air was the fabrication method used because it is comparatively simple and safe. The effects of three different reaction times including 1, 2, 3 hour(s) on particle size were compared. Also, the effectiveness of three different capping agents (Oleic Acid, Polyvinylpyrollidone (PVP), and Trisodium Citrate) in reducing aggregation and correspondingly particle size were examined. Using Welch’s analysis of variance (ANOVA) and the relevant post hoc tests, there was no significant difference (p=0.05) between reaction times of 1 hour and 2 hours, but there was a significant difference between reaction times of 2 hours and 3 hours. Potentially, because of increased coarsening for the 3 hour reaction time. PVP and Oleic Acid were shown to be effective in reducing aggregation; however, Citrate was not effective. Possibly, the synthesis procedure was inadequate.

The search for improved physical and mechanical properties of ceramic tiles is an increasingly urgent need, facing increasing competition from the globalization of the economy. The design of experiments has been used more and more to model, simulate and obtain characteristics of interest in several areas of science. This work aimed at the development of mathematical models for predicting the properties of water absorption, linear shrinkage and flexural strength of the ceramic tiles using the factorial design of experiments. Samples of three clay deposits were collected, whose physical, chemical and mineralogical characterizations, showed that these are clay characteristics used in the industry of ceramic tiles. Then, based on the major variables of ceramic processing that directly influence the final quality of the ceramic tiles( formulation, particle size, pressing and firing conditions), mathematical models were developed for the prediction of properties of water absorption, linear shrinkage and of the flexural strength modulus. Mathematical models obtained for the prediction of absorption and shrinkage were considered satisfactory for they were able to describe the experimental data in the evaluated range and to the desired level of trust. However, the same has not happened to the model for the flexural strength that must be associated to peculiar characteristic of mechanical behavior of ceramic materials. This work has shown that the importance of characterization of experimental errors in a design of experiments and presents a proposal of procedures for the usage of factorial planning of experiments, specially in the modeling of mechanical behavior of ceramic materials. / A busca da melhoria de propriedades físicas e mecânicas da cerâmica de revestimento é uma necessidade cada vez mais premente devido, principalmente à globalização da economia. O planejamento de experimentos tem sido cada vez mais utilizado para modelar, simular e obter características de interesses em diversas áreas da ciência. Este trabalho teve como objetivo o desenvolvimento de modelos matemáticos para predição das propriedades de absorção de água, retração linear e resistência à flexão da cerâmica de revestimento usando o planejamento fatorial de experimentos. Foram coletadas amostras de 03 depósitos argilosos, cuja caracterização física, química e mineralógica mostrou que as mesmas são características de argilas utilizadas na indústria da cerâmica de revestimento. Em seguida, com base nas principais variáveis do processamento cerâmico que influenciam diretamente a qualidade final do revestimento cerâmico (formulação, granulometria, prensagem e condições de queima), foram desenvolvidos modelos matemáticos para predição das propriedades de absorção de água, retração linear e do módulo de resistência à flexão. Os modelos matemáticos obtidos para predição da absorção e retração foram considerados satisfatórios, pois foram capazes de descrever os dados experimentais na faixa avaliada e para o nível de confiança desejado. Entretanto o mesmo não ocorreu com o modelo para resistência à flexão, que deve estar associado às características peculiares do comportamento mecânico dos materiais cerâmicos. Este trabalho demonstrou também a importância da caracterização dos erros experimentais em um planejamento de experimentos, e apresenta uma proposta de procedimentos para a utilização do planejamento fatorial de experimentos, especialmente na modelagem do comportamento mecânico de materiais cerâmicos.

No description available.

Ceramics are very important materials with many unique properties used in numerous industrial applications. Ceramics could be very hard and very strong in comparison to metals; however, they are very brittle, thus they are prone to instantaneous and catastrophic failure. Therefore, their reliability is compromised and it is very important to have advanced techniques that allow evaluating their mechanical behavior in many unusual stress states. One of such testing methods is biaxial strength method, that allows to measure properties not only unidirectional, but also in a biaxial way. The research work for this thesis will be built on design and development of ring-on-ring test jigs that will measure a biaxial strength of thin ceramic disks.

Polymeric materials have provided pathways to products that could not be manufactured otherwise. A new technology which merges the benefits of ceramics into these polymer products has created materials ideally suited to many different industries, like food packaging. Nano Scale Surface Systems, Inc. (NS3), a company which coats polymers with ceramic oxides like SiO2 through a process known as plasma enhanced chemical vapor deposition (PECVD), was interested in the feasibility of an in line measurement system for monitoring the deposited films on various polymer products. This project examined two different coated polymer products, polyethylene terephthalate (PET) beverage containers and biaxially oriented PET food packaging, commonly known as plastic wrap in an effort to determine the feasibility of an ellipsometry based measurement system for NS3’s purpose. Due to its extensive use in the semiconductor industry for monitoring films deposited on silicon, a measurement systems known as ellipsometry, adept at monitoring the thickness and refractive index of thin films deposited on various substrates, appeared to be an ideal system for the measurement of ceramic oxides deposited on various polymer substrates. This project set out to determine the feasibility of using an ellipsometry based measurement system to monitor ceramic films, specifically silicon oxides (SiOX), deposited on polymer products. A preliminary experiment determined linearly polarized light could induce a discernible change in polarized light traversing a coated beverage container relative to an uncoated container. However, the experiment lacked repeatability due to the measurement apparatus’ cheap setup, prompting the construction of a null (conventional) ellipsometer for further research. The curved surface of the beverage containers under study unnecessarily complicated the feasibility study so further research examined PECVD SiOX on biaxially oriented PET instead. Characterization of the PECVD SiOX-PET material was divided into three experiments, with the first two analyzing the SiOX film and PET substrate separately while the third analyzed them together. To assist with the characterization experiments, NS3 provided samples, both SiOX coated and uncoated, of various deposition thicknesses on silicon and biaxially oriented PET substrates. Null ellipsometry was used in conjunction with spectroscopic reflectometry to characterize the refractive index and thickness of the deposited films. The combined measurement systems found the refractive index of the deposited SiOX films to be between 1.461 and 1.465. The measured thicknesses resulting from the two measurement systems coincided well and were usually 10-20 nm thicker than the predicted thicknesses by the deposition processing parameters. Abeles’ method and monochromatic goniometry were attempted; however, the results had to be discarded due to irrecoverable errors discovered in the reflectance measurement. X-ray photoelectron spectroscopy (XPS) data provided by NS3 showed the deposited SiOX films to be homogeneous with stoichiometries between 2.15 and 2.23. Characterization of the uncoated biaxially oriented PET required numerous measurement systems. From spectroscopic transmission, trirefringent anisotropy was discovered, intertwined with thickness variations in the PET foil. Goniometry measurements displayed distinct interference curves resulting from rear interface reflections interfering with front interface reflections from the PET sample. Subsequent goniometric models produced multiple solutions due to an unknown optical phenomenon, probably scattering, which degraded the reflection measurements. However, a combined measurement technique utilizing goniometry and differential scanning calorimetry (DSC) determined the refractive indices of the polymer to be NX = 1.677, NY = 1.632 and NZ = 1.495 with a thickness of 11.343 μm and a volume fraction crystallinity of 35-41%. Utilizing the measured refractive indices, ellipsometric models produced only an adequate fit of the measured data due to the presence of depolarization caused by non-uniform PET thickness and scattering resulting from embedded microscopic crystallites. The majority of the error in the ellipsometric data was observed in the Δ measurement. XPS measurements of SiOX deposited on polypropylene (PP) provided by NS3 showed a heterogeneous interphase layer between the deposited oxide and the polymer substrate where the composition of the layer was continually changing. A similar region, which violates the homogenous assumption the ellipsometric model relied on, was anticipated for the SiOX-PET samples under investigation. The use of an effective medium approximation (EMA) to represent the interphase region was attempted, but failed to provide a decent model fit of the measured data. Depolarization and high optical anisotropy caused by the polymer substrate in combination with a heterogeneous interphase region and the effects of the deposited SiOX layer all interacted to prevent ellipsometric modelling of the null ellipsometry measurements conducted. Goniometry measurements were conducted on the thickest deposited SiOX film (approximately 100 nm) which allowed for the refractive index of the film to be approximated through Abeles’ method (n = 1.46); however the validity of this approximation was questionable given the presence of interference fringes resulting from interference between reflections at both the front and rear interfaces of the material. From the experiments conducted, it was concluded that null ellipsometry with conventional ellipsometric models could not adequately measure a SiOX film’s refractive index or thickness when deposited on biaxially oriented PET. The reasons for the failure were interactions between multiple sources of error which led to both measurement errors and inaccurate model assumptions. Use of generalized ellipsometry, possibly with spectroscopic ellipsometry, may overcome the failures of conventional ellipsometry when studying this complex optical material.

Submitted by Emanuel Varela Cardoso (emanuel.varela@ufcg.edu.br) on 2018-06-11T21:47:59Z No. of bitstreams: 1 VERALÚCIA SEVERINA DA SILVA – TESE (PPGEP) 2016.pdf: 6421802 bytes, checksum: 9b42464393ac9c935bb0b5026ad45fc2 (MD5) / Made available in DSpace on 2018-06-11T21:47:59Z (GMT). No. of bitstreams: 1 VERALÚCIA SEVERINA DA SILVA – TESE (PPGEP) 2016.pdf: 6421802 bytes, checksum: 9b42464393ac9c935bb0b5026ad45fc2 (MD5) Previous issue date: 2016-12-01 / A secagem é um processo termodinâmico, em que há transferência simultânea de calor e a remoção da umidade de um material poroso. Os produtos argilosos quando expostos a uma secagem sem controle pode sofrer fissuras e deformações, reduzindo sua qualidade póssecagem. Este trabalho tem como objetivo estudar teórico e experimentalmente a transferência de calor e massa em sólidos com forma complexa com, com ênfase a secagem de materiais cerâmicos argilosos. Neste trabalho desenvolveu-se um modelo matemático para descrever as trocas de calor e massa durante o processo de secagem, utilizando o método da capacitância global em corpos vazados. A solução analítica das equações governantes foi feita usando o método de separação de variáveis. Foram realizados experimentos de caracterização química e terrmo-hídrica da argila, e secagem de materiais cerâmicos argilosos vazados e com formas não-convencionais, em diferentes temperaturas (60, 70, 80, 90 e 100ºC). Resultados da composição química e granulometria da argila, e cinéticos de perda de massa e aquecimento das peças cerâmicas são apresentados e analisados. Verificou-se que o processo de perda de umidade ocorre a uma velocidade mais baixa do que o aquecimento do material cerâmico, que a temperatura e forma do corpo afetam fortemente os fenômenos de transporte de calor e massa, que a secagem a baixa temperatura favorece a redução de problemas no material pós secagem e melhoramento na qualidade final, e que os números de Biot de transferência de calor e de massa influenciam diretamente no tempo que o produto atinge sua condição de equilíbrio. A comparação entre o teor de umidade e temperatura preditos pelo modelo matemático proposto e os dados experimentais permitiu a estimativa dos coeficientes de transferência de massa e calor na superfície do material, com boa precisão. / Drying is a thermodynamic process, in which there is simultaneous heat transfer and moisture removal of a porous material. Clay products exposed to drying without control may suffer cracks and deformations, reducing its quality post-drying. This work aims to study theoretical and experimental the drying of solids with complex shape. It was developed a mathematical model to describe heat and mass transfer during the drying process, using the global capacitance method of hollow bodies. The analytical solution of the governing equations was made using the variable separation method. It were realized experiments of chemical and thermo-hydric characterization of clay, and drying of hollow and non-conventional clay ceramic materials at different emperatures (60, 70, 80, 90 and 100ºC). Results of the chemical composition and granulometry, and mass loss and heating of ceramic parts are presented and analyzed. It was verified that the moisture loss process occurs at a lower velocity than the heating of the ceramic material, the temperature and body shape strongly affect heat and mass transport phenomena, drying at low temperature favors the reduction of the problems in the material post-drying and improvement in the final quality, and that Biot numbers of heat and mass transfer directly affect the time to the product to reach its equilibrium condition. Comparison between predicted and experimental moisture content and temperature permitted estimative of the convective heat and mass transfer coefficients at the surface of the material, with good precision.

Nesta pesquisa foram utilizados resíduos da produção de alumínio e ferro. Resíduo de bauxita, que também é chamado de rejeitos de bauxita ou lama vermelha, e escória siderúrgica são os principais resíduos da indústria metalúrgica. Também foi utilizada areia de fundição, que é um resíduo do processo de fundição. Estes três componentes foram utilizados em conjunto para desenvolver material cerâmico de construção. A idéia principal era usar apenas resíduos industriais, sem materiais naturais tradicionais. Os residuos de vidro e as cinzas de madeira foram adicionados às composições para deminuir o ponto de fusão das amostras. Na pesquisa, 24 composições foram queimadas a 800-1225°C e suas propriedades foram estudadas. As características mecânicas das amostras foram analisadas através do teste de resistência à flexão, medindo-se a absorção de água, densidade e retração linear. As propriedades físico-quimicas foram estudadas por XRF, XRD, AAS, SEM, EDS, LAMMA, mapeamento, DTA e TGA. O principal motivo para os resultados elevados de resistência à flexão (19,78 MPa) das amostras foi identificado como o desenvolvimento de novas formações amorfas. Como resultado da pesquisa, algumas composições foram sugeridas para a produção específica de materiais de construção. Composições contendo lama vermelha (40- 100%), escória siderúrgica (0-50%), areia de fundição (0-50%), resíduo de vidro (0-20%) e cinzas de madeira (0-20%), atenderam normas e regulamentos brasileiros para materiais de construção, podem substituir materiais cerâmicos tradicionais, que envolvem a enorme exploração de recursos naturais. / In the presented research were used residues of aluminum and iron production. Bauxite residue, which is also called bauxite tailings or red mud, and blast furnace slag are the key wastes of metallurgical industry. There was also used foundry sand, which is a residue of casting process. These three components were used together to develop ceramic construction material. The main idea was to use industrial wastes only, no traditional natural materials. The waste glass and wood ash were added to the compositions in order to decrease melting point of the samples. In the research 24 compositions were sintered at 800-1225°C and their properties were studied. Their mechanical characteristics were analyzed using flexural strength test, measuring water absorption, density, and linear shrinkage. Physicochemical properties were studied by XRF, XRD, AAS, SEM, EDS, LAMMA, mapping, DTA, and TGA. The main reason for high results of flexural strength (19.78 MPa) of the samples was identified as a development of new amorphous formations. As a result of research, some compositions were suggested for specific construction materials production. Compositions containing red mud (40-100%), blast furnace slag (0-50%), foundry sand (0-50%), waste glass (0-20%), and wood ash (0-20%), according to Brazilian Norms and regulations for construction materials, may substitute traditional ceramic materials, which involve enormous exploration of natural resources.

Nesta pesquisa foram utilizados resíduos da produção de alumínio e ferro. Resíduo de bauxita, que também é chamado de rejeitos de bauxita ou lama vermelha, e escória siderúrgica são os principais resíduos da indústria metalúrgica. Também foi utilizada areia de fundição, que é um resíduo do processo de fundição. Estes três componentes foram utilizados em conjunto para desenvolver material cerâmico de construção. A idéia principal era usar apenas resíduos industriais, sem materiais naturais tradicionais. Os residuos de vidro e as cinzas de madeira foram adicionados às composições para deminuir o ponto de fusão das amostras. Na pesquisa, 24 composições foram queimadas a 800-1225°C e suas propriedades foram estudadas. As características mecânicas das amostras foram analisadas através do teste de resistência à flexão, medindo-se a absorção de água, densidade e retração linear. As propriedades físico-quimicas foram estudadas por XRF, XRD, AAS, SEM, EDS, LAMMA, mapeamento, DTA e TGA. O principal motivo para os resultados elevados de resistência à flexão (19,78 MPa) das amostras foi identificado como o desenvolvimento de novas formações amorfas. Como resultado da pesquisa, algumas composições foram sugeridas para a produção específica de materiais de construção. Composições contendo lama vermelha (40- 100%), escória siderúrgica (0-50%), areia de fundição (0-50%), resíduo de vidro (0-20%) e cinzas de madeira (0-20%), atenderam normas e regulamentos brasileiros para materiais de construção, podem substituir materiais cerâmicos tradicionais, que envolvem a enorme exploração de recursos naturais. / In the presented research were used residues of aluminum and iron production. Bauxite residue, which is also called bauxite tailings or red mud, and blast furnace slag are the key wastes of metallurgical industry. There was also used foundry sand, which is a residue of casting process. These three components were used together to develop ceramic construction material. The main idea was to use industrial wastes only, no traditional natural materials. The waste glass and wood ash were added to the compositions in order to decrease melting point of the samples. In the research 24 compositions were sintered at 800-1225°C and their properties were studied. Their mechanical characteristics were analyzed using flexural strength test, measuring water absorption, density, and linear shrinkage. Physicochemical properties were studied by XRF, XRD, AAS, SEM, EDS, LAMMA, mapping, DTA, and TGA. The main reason for high results of flexural strength (19.78 MPa) of the samples was identified as a development of new amorphous formations. As a result of research, some compositions were suggested for specific construction materials production. Compositions containing red mud (40-100%), blast furnace slag (0-50%), foundry sand (0-50%), waste glass (0-20%), and wood ash (0-20%), according to Brazilian Norms and regulations for construction materials, may substitute traditional ceramic materials, which involve enormous exploration of natural resources.

Studies on porous ceramics have a great technological and scientific interest because they are related to catalysis, control of pollutant particulates (aerosols), and powder metallurgy, among many other applications. In this context, the pursuit of new porous ceramic structures that exhibit a greater efficiency of certain properties has been very intense recently. In this work we develop alumina porous ceramic named ceramic foams that were investigated as microcavities in optical applications. Alumina nanoparticles were synthesized by a proteic sol-gel route with low level of toxicity and transformed into ceramic foams consisting of a network of pores with diameters ranging from 0.8 mm to 10 mm, depending on the processing parameters used. Fluorescence measurements in such samples with pores filled by organic dyes rhodamine B and rhodamine 6G exhibited emission characteristic of random laser. / Estudos sobre cerâmicas porosas tem um grande interesse tecnológico e científico por estarem relacionadas a controle de catálise, poluentes particulados (aerossol), e metalurgia de pó, entre várias outras aplicações. Nesse contexto, a busca de novas estruturas cerâmicas porosas que apresentem uma maior eficiência de determinadas propriedades tem sido muito intensa recentemente. Neste trabalho desenvolvemos cerâmicas porosas de alumina do tipo espuma cerâmicas que foram investigadas como microcavidades em aplicações ópticas. Nanopartículas de alumina foram sinterizadas através de uma rota de sol-gel proteico, com baixo grau de toxicidade e transformadas em espumas cerâmicas constituídas por uma rede de poros com diâmetros variando de 0,8 mm a 10 mm, a depender dos parâmetros de processamento utilizados. Medidas de fluorescência em tais amostras com os poros preenchidos pelos corantes orgânicos Rodamina B e Rodamina 6G apresentaram uma emissão característica de laser randômico.

Doctorat en philosophie et lettres / info:eu-repo/semantics/nonPublished