AgÃncia Nacional do PetrÃleo / FundaÃÃo Cearense de Apoio ao Desenvolvimento Cientifico e TecnolÃgico / A soldagem de revestimento com aÃos inoxidÃveis duplex (AID) e superduplex (AISD) à uma boa opÃÃo que pode ser utilizada no setor de petrÃleo e gÃs natural, permitindo alcanÃar caracterÃsticas desejadas, como resistÃncia à corrosÃo e boas propriedades mecÃnicas. O objetivo do presente trabalho foi desenvolver e avaliar as caracterÃsticas operacionais e metalÃrgicas em soldagens de revestimento de dutos com deposiÃÃo de AID/AISD pelo processo Plasma pÃ. Inicialmente, as soldagens foram realizadas em simples depÃsito para avaliaÃÃo das caracterÃsticas geomÃtricas e reduÃÃo de custos e, posteriormente, aplicados os revestimentos, variando diversos parÃmetros do processo Plasma pà com deposiÃÃo de AID DIN 1.4462 e AISD UNS S32760. A caracterizaÃÃo microestrutural consistiu de anÃlises de microscopia Ãtica, microscopia eletrÃnica de varredura (MEV), espectroscopia de raio-x dispersivo em energia (EDS) e difraÃÃo de raios-X (DRX). Ensaios de Temperatura CrÃtica de Pites (ASTM G 150) e ensaios de microdureza foram realizados para avaliar a resistÃncia à corrosÃo do metal de solda e determinaÃÃo da microdureza ao longo do revestimento. Os resultados mostraram que a deposiÃÃo de AID/AISD pode ser uma boa opÃÃo para soldagem de revestimento, com deposiÃÃo em apenas uma camada, com baixos nÃveis de diluiÃÃo e com caracterÃsticas favorÃveis para garantir boas propriedades aos revestimentos. Em relaÃÃo à microestrutura, os revestimentos depositados com a liga AISD UNS S32760 proporcionou uma quantidade considerÃvel de nitretos no metal de solda, porÃm os revestimentos com deposiÃÃo de AID DIN 1.4462 obtiveram maior quantidade de austenita secundÃria em relaÃÃo aos nitretos, ambos com bom balanÃo de fases ferrita e austenita. Os resultados de microdureza dos revestimentos mostraram maior resistÃncia do metal de solda em relaÃÃo ao API 5L X65 com ausÃncia de elevados picos de microdureza na interface. O ensaio de TCP mostrou que o primeiro cordÃo de solda à menos resistente em relaÃÃo ao Ãltimo cordÃo depositado e que a liga AID mostrou ter maior resistÃncia à corrosÃo por pites em relaÃÃo à liga AISD. / The weld overlay of duplex (DSS) and superduplex (SDSS) stainless steels is an interesting alternative used in oil and gas industry, allowing to reach the desirable characteristics, such as corrosion resistance and good mechanical properties. The main objective of the present work was to develop and evaluate the operational and metallurgical characteristics of DSS/SDSS alloys weld overlays deposited by PTA-P on pipes. Initially, the welds were performed in single weld bead for evaluation of geometric characteristics and cost reduction and later in multipass to produce the coating, changing several operational parameters with deposition of DSS DIN 1.4462 and SSS UNS S32760. The microstructure was investigated using light microscopy, scanning electron microscopy (SEM), energy dispersive of X-ray spectroscopy (EDS) and X-ray diffraction (XRD). Critical Pitting Temperature (CPT) - ASTM G 150 and microhardness tests were carried out to evaluate the corrosion resistance and determining the microhardness over coating. The results showed that deposition of DSS and SSS demonstrated to be an interesting option for the weld overlay. It could to deposited in just one layer, coatings with low levels of dilution, important characteristics to assure a good performance of the coatings. The microstructure in weld metal of the coatings deposited with SDSS alloy was constituted by nitrides, however the DSS alloy was constituted by secondary austenite precipitation and a good balance between ferrite and austenite. The results of microhardness test showed that the coating is more resistance than the API 5L X65 and it was not observed higher levels in the coating near the interface coating/substrate. The CPT test showed that the first weld bead is less resistant in relation to the last bead deposited and the DSS alloy showed greater pitting corrosion resistance in relation to the SdSS alloy.

Este trabalho investigou a deposição de filmes finos de ferrita de bismuto (BFO) através da técnica spray pirólise utilizando sais inorgânicos como precursores em diferentes solventes e silício como substrato, visando a deposição em menor temperatura e a obtenção de diferentes morfologias de superfície. Para tanto, foram utilizados água, etilenoglicol e etanol/butil carbitol (1:1) como solventes na preparação da solução a ser aspergida. Foram realizadas deposições com diferentes temperaturas do substrato: 200, 250, 300 e 350ºC para cada solvente utilizado. A deposição de filmes BFO em baixas temperaturas (200ºC) favoreceu a formação de filme. Para o solvente etilenoglicol (maior ponto de ebulição), verifica-se a formação de filmes porosos, já para o solvente etanol/butil carbitol (1:1) foi verificada a formação de filmes densos com a presença de trincas. As análises termogravimétricas (ATG) e termodiferenciais (ATD) foram realizadas para os filmes como-depositados a 200ºC com diferentes solventes. Após a deposição, as amostras foram tratadas termicamente a 550ºC por 1h, visando a formação da fase cristalina BiFeO3 com estrutura romboédrica. Os filmes foram analisados por difração de raios X (DRX) e microscopia eletrônica de varredura (MEV). Os resultados mostraram a obtenção da fase cristalina do BiFeO3 após o tratamento térmico a 550ºC/1h com a presença de fase secundária. As imagens de MEV evidenciaram a formação de filmes independente do solvente utilizado para a temperatura de 200ºC. Contudo, o aumento da temperatura promoveu a formação de partículas sobre o substrato e não uma formação contínua de filme, evidenciada pela composição elementar medida através de espectroscopia por energia dispersiva de raios X (EDX). A caracterização elétrica dos filmes foi realizada utilizando espectroscopia de impedância (EI) em função da temperatura, sendo observada maior condutividade para o filme depositado com etilenoglicol. A fase BFO não estequiométrica evidenciada por DRX pode explicar as diferentes condutividades elétricas mensuradas por EI quando utilizado diferentes solventes. As propriedades ópticas foram medidas utilizando-se espectroscopia de reflectância difusa, encontrando-se um band gap entre 2,23 – 2,26 eV. / This research investigated the deposition of thin films of bismuth ferrite (BFO) on silicon substrate using the spray pyrolysis technique based on inorganic salts as precursors. For this purpose water, ethylene glycol and ethanol/butyl carbytol (1:1) were used as solvents to prepare the solution for spraying. The depositions were carried out with different substrate temperatures for each solvent used: 200, 250, 300 and 350ºC. The film deposition at low temperatures (200°C) promotes the formation of cracks due to the arrival of the liquid state from droplets sprayed by the atomizer. When using solvent ethanol/butyl carbytol (1:1) the formation of dense films was verified for the different depositions. The thermal gravimetric (TGA) and differential thermal analysis (DTA) were performed for the as-deposited films at 200°C with different solvents for the study of possible reactions of thermal decomposition. The BFO films were heated at 550°C for one hour aiming to the formation of the crystalline state BiFeO3 with rhombohedral structure. The films were analyzed by Xray diffraction (XRD) and scanning electron microscopy (SEM) before and after treatment. The XRD showed the crystalline state obtained after the heat treatment at 550°C/1h. It was observed the formation of non-stoichiometric composition on the film. The SEM images showed formation of films regardless of the solvent used for the temperature to 200°C. However, the increase temperature promotes the formation of particles on the substrate. Applying the ethylene glycol solvent the formation of porous films appeared, since for ethanol/butyl carbytol (1:1) was observed the formation of dense films with the presence of cracks. The electrical characterization of the films will be performed using impedance spectroscopy (IS) coupled to a furnace in order to vary the temperature of the measures. The film deposited with ethylene glycol presents a major electrical conductivity than films deposited using ethanol/butyl carbytol or water. This behavior can be associated with a non-stoichiometric composition of BFO. Moreover, the optical properties were obtained by diffuse reflectance spectroscopy. The films present a band gap between 2.23 and 2.26 eV, approximately.

Made available in DSpace on 2014-10-09T12:51:54Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:06:44Z (GMT). No. of bitstreams: 0 / Atualmente com o advento da nanociência e nanotecnologia, as nanopartículas magnéticas têm encontrado inúmeras aplicações nos campos da biomedicina, diagnóstico, biologia molecular, bioquímica, catálise, etc. As nanopartículas magnéticas funcionalizadas são constituídas de um núcleo magnético, envolvido por uma camada polimérica com sítios ativos, que podem ancorar metais ou compostos orgânicos seletivos. Estas nanopartículas são consideradas materiais híbridos orgânico-inorgânicos de grande interesse em aplicações comerciais devido à particularidade das propriedades obtidas. Entre as aplicações importantes podemos citar: tratamento por magnetohipertermia, carregadores de fármacos para áreas específicas do corpo, seleção de moléculas específicas, biossensores, melhoria da qualidade de imagens por RMN, etc. O trabalho foi desenvolvido em duas partes: 1) a síntese do núcleo constituído de nanopartículas superparamagnéticas de ferrita de cobalto e, 2) o recobrimento do núcleo por um polímero bifuncional o 3-aminopropiltrietoxissilano. Os parâmetros estudados na primeira parte da pesquisa foram: pH, concentração molar da base, tipo de base, ordem de adição dos reagentes, modo de adição dos reagentes, velocidade de agitação, concentração inicial dos metais, fração molar de cobalto e tratamento térmico. Na segunda parte estudou-se: o pH, a temperatura, o catalisador, a concentração do catalisador, o tempo de reação, a relação H2O/silano, o tipo de meio, o agente umectante e a eficiência do recobrimento em relação ao pH. Os produtos obtidos foram caracterizados pelas técnicas de difratometria de raios-X (DRX), microscopia eletrônica de transmissão (MET), microscopia eletrônica de varredura (MEV), espectroscopia de energia dispersiva (EDS), espectroscopia de emissão atômica (ICP-AES), espectroscopia por infravermelho (FTIR), análises termogravimétricas (TGA/DTGA), calorimetria exploratória diferencial (DSC) e curvas de magnetização (MAV) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Orientador: Oswaldo Luiz Alves / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Quimica / Made available in DSpace on 2018-08-13T13:21:45Z (GMT). No. of bitstreams: 1 Oliveira_FlavioHenrique_M.pdf: 1865644 bytes, checksum: f0716bfd25ded49ec69dd8796c111a00 (MD5) Previous issue date: 2009 / Resumo: Sistemas ternários tipo hidrotalcita contendo metais de transição Ni, Fe e Cu tendo o ânion interlamelar o carbonato foram preparados através de um estudo sistemático de composição e parâmetros de síntese. Diferentes quantidades de Cu foram introduzidas na camada tipo brucita da hidrotalcita, sendo estas quantidades de 10, 20, 30, 40 e 50 % em relação a quantidade de Níquel. De acordo com difratogramas para baixas quantidades de cobre (10 e 20 %) a fase hidrotalcita apresentou-se pura, para maiores quantidades de cobre ocorreu segregação de fase a qual foi identificada como CuO. A preparação dos compostos ternários foi feita tendo como razão de metal II para metal III 2:1, essa razão entre os metais foi confirmada através de análises de ICP a qual demonstrou exata proporção entre os metais nas amostras. Análise térmica apresentaram um comportamento típico para hidrotalcitas, apresentando duas transições características a 170 °C e a 280 ºC. Devido à ocorrência de alta segregação de fases que ocorre na precipitação com estes metais, foram realizados experimentos com diferentes temperaturas de precipitação e os resultados preliminares indicam a formação de uma fase pura em baixas temperaturas. Compostos preparados com 30 % de Cu a temperatura ambiente apresenta segregação de fase o que não ocorre a temperaturas próximas a 0 ºC, temperaturas elevadas (60 °C) favorecem a formação de óxidos durante a precipitação. Portanto baixas temperaturas de precipitação resultam em fases puras de hidrotalcitas para concentrações de cobre intermediarias, como conseqüência é possível preparar amostras com altas concentrações de cobre na estrutura lamelar com a fase da hidrotalcita pura. Com estes metais de transição na estrutura lamelar este sistema pode vir a ser um bom precursor na formação de óxidos dos respectivos metais que constituem o composto, com a finalidade de ser utilizada em catálise / Abstract: Ternary systems of hydrotalcite-like compouds containing transition metals Ni, Fe and Cu and the interlayer anion the carbonate were prepared through a systematic study of composition and synthesis parameters. Different amounts of Cu were introduced into the layer hydrotalcite, and the figure of 10, 20, 30, 40 and 50% on the amount of Nickel. According to difratograms, for low quantities of copper (10 and 20%) the phase is pure hydrotalcite and for larger quantities of copper segregation occurred, which was identified as CuO. The preparation of ternary compound was made with the ratio of metal II to metal III 2:1, the ratio between the metals was confirmed through analysis of ICP which showed exact proportion between the metals in the samples. Thermal analysis showed a typical behavior for hydrotalcite, presenting features two transitions to 170 ° C and 280 C. Due to the high occurrence of segregation of phases in the precipitation that occurs with these metals, experiments were performed with different temperatures and precipitation and the preliminary results indicate the formation of a pure phase at low temperatures. Compounds prepared with 30% of Cu at room temperature shows segregation of the stage that does not occur at temperatures close to 0 º C, high temperature (60 C) favor the formation of oxides during the precipitation. In conclusion, low temperatures of precipitation result in phases of pure hydrotalcite for an intermediary concentration of copper, as a result, is possible to prepare samples with high concentrations of copper in the lamellar structure with pure phase of hydrotalcite. With these transitions metals in the lamellar structure this systems might be a good precursor in the formation of oxides of the metals that constitute the compound in order to be used in catalysis / Mestrado / Quimica Inorganica / Mestre em Química

Les nanoparticules magnétiques de structure spinelle MFe2O4 (M = Fe, Co, Mn, Zn, Ni...) ont été largement étudiées pour leurs applications variées allant du stockage de l'information aux applications biomédicales. Parmi ces applications, les plus récentes basées sur les propriétés magnétiques dynamiques des nanoparticules sont en pleine expansion et nécessitent des particules magnétiques avec une énergie d'anisotropie contrôlée. L'objectif de cette thèse était de synthétiser des nanoparticules magnétiques avec une énergie d'anisotropie modulable, en associant des matériaux présentant des propriétés magnétiques intrinsèques différentes. Nous avons choisis la synthèse par décomposition thermique à haute température, qui présente l'avantage de former des nanoparticules monodisperses avec une morphologie contrôlée. Afin de développer des propriétés magnétiques originales et moduler l'énergie d'anisotropie des particules, nous avons synthétisé des nanoparticules multicoquilles magnétiques constituées d'un coeur doux (Fe3O4, MnFe2O4, NiFe2O4), d'une coquille dure (CoFe2O4) et d'une deuxième coquille douce pour les particules trimagnétiques. Nous avons montré que le champ coercitif augmente lorsqu'un cœur d'un matériau doux est recouvert avec une coquille d'un matériau dur. Pour les particules MnFe2O4@CoFe2O4@NiFe2O4, l'ajout d'une seconde coquille douce diminue le champ coercitif. La constante d'anisotropie évolue dans le même sens. Deux autres systèmes ont également été synthétisés et comparés à ces multicoquilles. Les ferrites mixtes Co1?xMnxFe2O4, avec x compris entre 0 et 1, et les ferrofluides binaires composés d'un mélange de ferrites MFe2O4 (M = Mn ou Ni) et CoFe2O4. / Magnetic nanoparticles with spinel structure MFe2O4 (M = Fe, Co, Mn, Zn, Ni...) have been extensively studied for their various applications ranging from magnetic recording to biomeical applications(...)...

Typical microwave components such as antennas are large in size and occupy considerable space. Since multiple standards are utilized in modern day systems and thus multiple antennas are required, it is best if a single component can be reconfigured or tuned to various bands. Similarly phase shifters to provide beam scanning and polarization reconfigurable antennas are important for modern day congested wireless systems. Tunability of antennas or phase shifting between antenna elements has been demonstrated using various techniques which include magnetically tunable components on ferrite based substrates. Although this method has shown promising results it also has several issues due to the use of large external electromagnets and operation in the magnetically saturated state. These issues include the device being bulky, inefficient, non-integrable and expensive. In this thesis, we have tried to resolve the above mentioned issues of large size and large power requirement by replacing the large electromagnets with embedded bias windings and also by operating the ferrites in the partially magnetized state. New theoretical models and simulation methodology have been used to evaluate the performance of the microwave passive components in the partially magnetized state. A multilayer ferrite Low Temperature Cofired Ceramic (LTCC) tape system has been used to verify the performance experimentally. There exists a good agreement between the theoretical, simulation and measurement results. Tunable antennas with tuning range of almost 10 % and phase shifter with an FoM of 83.2/dB have been demonstrated in this work, however the major contribution is that this has been achieved with bias fields that are 90 % less than the typically reported values in the literature. Finally, polarization reconfigurability has also been demonstrated for a circular patch antenna using a low cost additive manufacturing technique. The results are promising and indicate that highly integrated ferrite based tunable components are feasible in small form factor, without the need of the large electromagnets and coils, and thus can be operated at very low bias levels as compared to the ones which are operated in the saturated state with external bias mechanisms.

Phased array antennas, capable of controlling the direction of their radiated beam, are demanded by many conventional as well as modern systems. Applications such as automotive collision avoidance radar, inter-satellite communication links and future man-portable satellite communication on move services require reconfigurable beam systems with stress on mobility and cost effectiveness. Microwave phase shifters are key components of phased antenna arrays. A phase shifter is a device that controls the phase of the signal passing through it. Among the technologies used to realize this device, traditional ferrite waveguide phase shifters offer the best performance. However, they are bulky and difficult to integrate with other system components. Recently, ferrite material has been introduced in Low Temperature Co-fired Ceramic (LTCC) multilayer packaging technology. This enables the integration of ferrite based components with other microwave circuitry in a compact, light-weight and mass producible package. Additionally, the recent concept of Substrate Integrated Waveguide (SIW) allowed realization of synthesized rectangular waveguide-like structures in planar and multilayer substrates. These SIW structures have been shown to maintain the merits of conventional rectangular waveguides such as low loss and high power handling capabilities while being planar and easily integrable with other components. Implementing SIW structures inside a multilayer ferrite LTCC package enables monolithic integration of phase shifters and phased arrays representing a true System on Package (SoP) solution. It is the objective of this thesis to pursue realizing efficient integrated phase shifters and phased arrays combining the above mentioned technologies, namely Ferrite LTCC and SIW. In this work, a novel SIW phase shifter in ferrite LTCC package is designed, fabricated and tested. The device is able to operate reciprocally as well as non-reciprocally. Demonstrating a measured maximum reciprocal phase shift of 132o and maximum non-reciprocal shift of 118o at 12 GHz. Additionally a slotted SIW antenna is designed and integrated with the phase shifter in an array format, demonstrating a beam scanning of ± 15o. The design is highly suitable for mobile automotive radars and satellite communications systems.

Specimens of steel 42CrMoS4 were quenched from the austenite (γ) and the ferrite (α) + austenite + cementite phase fields to produce fully martensitic matrices with 0 – 14 % ferrite dispersed in the matrix. After tempering at 300°C or 600°C mechanical and fatigue properties were determined. As expected yield strength, tensile strength and hardness decreased with increased tempering temperature and ferrite content. Quite unexpected, the fatigue properties were mildly affected. A small amount of ferrite, approximately 3% even appears to improve the fatigue strength. Then, at even higher ferrite amounts, slightly below 20% the fatigue strength appears to decrease again.

Within this thesis, a comprehensive study of the initial growth process of pure Fe3O4 films and Fe3O4/NiO bilayers on Nb:SrTiO3(001) substrates including the thermal interdiffusion behavior of these bilayers is presented. The sensitive interplay between magnetic, electronic and structural properties of these materials has been investigated in detail. In the first study, the initial growth behavior of high-quality ultrathin magnetite films on SrTiO3(001) deposited by reactive molecular beam epitaxy depending on the deposition temperature has been analyzed. For this purpose, the growth process has been monitored in situ and during the deposition by grazing incidence x-ray diffraction (GIXRD). The second part provides a comparative study of Fe3O4/NiO bilayers grown on both MgO(001) and Nb:SrTiO3(001) substrates exploring morphological, structural and magnetic properties. These structures have been investigated by means of x-ray photoelectron spectroscopy (XPS), low-energy electron diffraction (LEED), x-ray reflectivity (XRR) and diffraction (XRD), as well as vibrating sample magnetometry (VSM). Subsequently, thermal stability of these bilayers and the thermally induced interdiffusion process have been studied successively accompanied by a comprehensive characterization of the fundamental electronic, structural and magnetic properties using additional techniques such as angle resolved hard x-ray photoelectron spectroscopy (AR-HAXPES) and x-ray magnetic circular dichroism (XMCD). Finally, an alternative pathway for the preparation of ultrathin nickel ferrite films through interdiffusion is provided.

[pt] Consideramos neste trabalho a propagação de ondas magnetostáticas em cilindros de ferrite axialmente magnetizados, levando em conta a variação radial do campo interno de magnetização. O problema foi resolvido exatamente para campos não variáveis angularmente. Verificamos que as relações de disperção para o caso do campo de magnetização uniforme e o variável radialmente (foi considerada uma variação parabólica) somente coincidem para valores de freqüência bastante afastados da freqüência de ressonância. O fato de se considerar um campo de magnetização uniforme leva a resultados incorretos quando se consideram atrasos de pulsos de onda relativamente grandes. / [en] This work treats the propagation of magnetostatic waves in axially magnetized ferrite rods, taking into account the radial variation of the static magnetic field. An exact solution is found for no angular variation of the field. It is shown that only for frequencies sufficiently distant from resonance can the dispersion relation be the same for the cases of uniform magnetizing field and that of radially varying field (We considered a parabolic variation). The uniform magnetic field approximation leads to incorrect results when in the case of relatively large time delays.