Made available in DSpace on 2014-12-17T15:41:46Z (GMT). No. of bitstreams: 1 MoisesRCpdf.pdf: 4615723 bytes, checksum: 8e0d75d3465b34a6f59e81df4ba5830e (MD5) Previous issue date: 2009-02-04 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / The present work aims the preparation of filmes of strontium-doped lanthanum manganite (perovskita) yttria-stabilized zirconia (LSM-SDC) films deposited on substrate of YSZ by means of spin coating technique having as principal objective their application to solid oxide fuel cells of intermediate temperature. La0,8Sr0,2MnO3 and Ce0,8Sm0,2O1,9 were obtained by modified Pechini method by use of gelatin which act as polymerization agent. The powders obtained were characterized by Xray fluorescence, X ray diffraction, electronic scanning microscopy and the superficial area by BET method. The results obtained by X-ray fluorescence showed that the route adopted for obtention of powders was effective in the obtention of the compositions with close values to the stoichiometrics. Ethyl cellulose was used as pore-forming agent and mixed with the LSM-SDC powders in weight proportions of 1:24, 2:23 and 1:9. The films were sintered at 1150 ?C for 4 h and characterized by X-ray diffraction and scanning electron microscopy technique (SEM) and atomic force. The phases quantification of the precursory powders and of the obtained films was carried through Rietveld method. According with the analysis of SEM, as the content of ethyl cellulose was increased, the pore distribution in films become more uniform and the pore size reduced. The methodology used for the obtention of the films was very efficient, considering a material was obtained with characteristics that were proper to the application as electrolyte/cathode system to solid oxide fuel cells / O trabalho trata da prepara??o de filmes de manganita de lant?nio dopado com estr?ncio (perovskita) c?ria dopada com sam?rio (LSM-SDC) sobre substrato de zirc?nia estabilizada com ?tria (YSZ) pela t?cnica spin coating, para utiliza??o em c?lulas a combust?vel de ?xido s?lido de temperatura intermedi?ria. Neste trabalho, La0,8Sr0,2MnO3 e Ce0,8Sm0,2O1,9 foram obtidos pelo m?todo Pechini modificado pelo uso de gelatina que atua como agente polimerizante e quelante. Os p?s obtidos foram caracterizados por fluoresc?ncia de raios-X, difra??o de raios-X, microscopia eletr?nica de varredura e determina??o da ?rea superficial pelo m?todo BET. Os resultados obtidos por fluoresc?ncia de raios-X mostraram que a rota adotada para obten??o dos p?s foi eficaz na obten??o da composi??o com valores pr?ximos ao estequiom?trico. A etilcelulose foi usada como agente formador de poros e foi misturada ao p?s de LSM-SDC em propor??es m?ssicas de 1:24, 2:23 e 1:9. Os filmes foram tratados termicamente a 1150 ?C por quatro horas e caracterizados estruturalmente pela t?cnica de difra??o de raios X e morfologicamente pelas t?cnicas de microscopia eletr?nica de varredura e for?a at?mica. A quantifica??o das fases dos p?s precursores e dos filmes obtidos foi realizada atrav?s do refinamento Rietveld. De acordo com a an?lise de MEV, quando a quantidade de etilcelulose foi aumentada, a distribui??o dos poros nos filmes tornou-se mais uniformes e o tamanho de poros reduzidos. A metodologia empregada para a obten??o dos filmes mostrou-se satisfat?ria, considerando que foi obtido um material com caracter?sticas apropriadas para a aplica??o como sistema eletrodo/eletr?lito em c?lulas a combust?vel de ?xido s?lido (SOFC)

Made available in DSpace on 2014-12-17T15:42:16Z (GMT). No. of bitstreams: 1 IzangelaMA_TESE.pdf: 6002351 bytes, checksum: 61a1b03824f174ac0458b386d74608e7 (MD5) Previous issue date: 2012-03-21 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / In this study five compositions were synthesized zirconia doped with cerium and neodymium ions in the system Ce10-xNdx Zr90O2 with 0,5 ≤ x ≤ 4,0 using the Pechini method. The powders were characterized by thermogravimetric analysis, differential thermal analysis, infrared spectroscopy and X-ray diffraction, with application of Rietveld refinement of the calcination temperatures of 350?C/3h and 30 minutes at 900?C/3h. All compositions stabilized with a mixture of cubic and tetragonal phase zirconia. The samples were pressed into bars and sintered at 1500?C/3h and 1500?C/6h, being characterized by Xray diffraction, with application of the Rietveld refinement, density and porosity using Archimedes method, scanning electron microscopy and resistance the three point bending. It has been observed the increase in strength with increasing sintering temperature for the compositions x = 2,0 and x = 4,0. For x = 2,0 the main phase was the cubic with 92,56% with crystallite size of 0,56 μm, density and porosity of 96,82% from 1,36%. For x = 4,0 was a mixture of cubic and tetragonal phase with 21% and 37,98%, respectively. The crystallite size was 54,21 nm and 49,64 nm with a density porosity of 97,45% and 1,32% respectively. In the analysis of the fracture surface was observed a greater amount of grain fracture intragranular type, which contribute to increase the mechanical strength of the ceramic. Increased addition of the neodymium ion in the crystal lattice of the zirconium showed a nearly linear behavior with increasing mechanical strength of the zirconia ceramic. Was obtained a bending resistance of 537 ? 38 MPa for the composition x = 2,0 predominantly attributed to cubic phase with 92,56% / No presente trabalho foram sintetizadas cinco composi??es de zirc?nia dopada com ?ons c?rio e neod?mio no sistema Ce10-x.Ndx Zr90O2 com 0,5 ≤ x ≤ 4,0 com o uso do m?todo Pechini. Os p?s foram caracterizados por an?lise termogravim?trica, an?lise t?rmica diferencial, espectroscopia na regi?o do infravermelho e difra??o de raios X, com a aplica??o do refinamento de Rietveld nas temperaturas de calcina??o de 350?C/3h e 30 minutos a 900?C/3h. Todas as composi??es estabilizaram com mistura de fase tetragonal e c?bica da zirc?nia. As amostras foram prensadas em forma de barras e sinterizadas a 1500?C/3h e 1500?C/6h, sendo caracterizadas por difra??o de raios X, com a aplica??o do refinamento de Rietveld, densidade e porosidade usando o m?todo de Arquimedes, microscopia eletr?nica de varredura e resist?ncia a flex?o em tr?s pontos. Foi observado o aumento da resist?ncia mec?nica com o aumento da temperatura de sinteriza??o para as composi??es x=2,0 e x=4,0. Para x=2,0 a fase principal foi ? c?bica com 92,56 % com tamanho de cristalito de 0,56 μm, densidade de 96,82 % e porosidade de 1,36 %. Para x=4,0 ocorreu uma mistura da fase tetragonal e c?bica com 21 % e 37,98 %, repectivamente. O tamanho de cristalitos foi de 54,21 nm e 49,64 nm, com densidade de 97,45 % e porosidade de 1,32 %, respectivamente. Nas an?lises da superf?cie de fratura foi observado uma maior quantidade de gr?os com fratura do tipo intragranular, na qual contribuiu para o aumento da resist?ncia mec?nica da cer?mica. O aumento da adi??o do ?on neod?mio na rede cristalina da zirc?nia apresentou um comportamento quase linear com o aumento da resist?ncia mec?nica da cer?mica de zirc?nia. Foi obtida uma resist?ncia a flex?o de 537 ? 38 MPa para a composi??o x=2,0 atribu?da a predomin?ncia da fase c?bica com 92,56 %

Made available in DSpace on 2014-12-17T15:42:14Z (GMT). No. of bitstreams: 1 AndreiaCL_TESE.pdf: 5308625 bytes, checksum: 13df680734f410713c3992d8e7be1c8f (MD5) Previous issue date: 2010-12-27 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Orthoferrites AFeO3 (A = rare earth) are an important class of perovskite oxides that exhibit weak ferromagnetism. These materials find numerous applications as chemical sensors, cathodes for fuel cells and catalysis, which make them interesting from the standpoint of science and technology. Their structural, electrical and magnetic properties are dependent on many factors such as the preparation method, heat treatment conditions, chemical composition and replacement of cations in sites A and/or B. In this paper, LaFe1-xMnxO3 (0 ≤ x ≤ 1) orthoferrites-type was prepared by Pechini method and Microwave-assisted combustion reaction in order to evaluate the influence of synthesis route on the formation of oxide, as well as the effect of parcial replacement of iron by manganese and heat treatment on the magnetic properties. The precursor powders were calcined at 700?C, 900?C, 1100?C and 1300?C for 4 hours and they were characterized by the techniques: Thermogravimetric analysis (TGA), X ray diffraction (XRD), Refinement by Rietveld method, Scanning electron microscopy (SEM), Reduction temperature programmed (RTP) and Magnetic hysteresis measurements performed at room temperature. According to the XRD patterns, the formation of perovskite phase with orthorhombic structure was observed for the systems where 0 ≤ x ≤ 0.5 and rhombohedral for x = 1. The results also showed a decrease of lattice parameters with the parcial replacement of iron by manganese and consequently a reduction in cell volume. The hysteresis curves exhibited weak ferromagnetism for the systems prepared by both synthesis methods. However, a dependence of magnetization as a function of dopant content was observed for samples produced by Pechini method. As for the systems prepared by combustion reaction, it was found that the secondary phases exert a strong influence on the magnetic behavior / Ortoferritas AFeO3 (A = terra rara) constituem uma importante classe de ?xidos perovskita que exibem ferromagnetismo fraco. Estes materiais encontram in?meras aplica??es como sensores qu?micos, catodos para c?lulas a combust?veis e na ?rea de cat?lise, o que os fazem interessantes do ponto de vista cient?fico e tecnol?gico. Suas propriedades estruturais, el?tricas e magn?ticas s?o dependentes de v?rios fatores tais como: o m?todo de prepara??o, condi??es do tratamento t?rmico, composi??o qu?mica e substitui??o de c?tions nos s?tios A e/ou B. Neste trabalho, ortoferritas do tipo LaFe1-xMnxO3 (0 ≤ x ≤ 1) foram preparadas pelo m?todo Pechini e pela rea??o de combust?o assistida por microondas com a finalidade de avaliar a influ?ncia da rota de s?ntese na forma??o do ?xido, assim como o efeito da substitui??o parcial do ferro por mangan?s e do tratamento t?rmico nas propriedades magn?ticas. Os p?s precursores foram calcinados a 700?C, 900?C, 1100?C e 1300?C por 4 horas e caracterizados atrav?s das t?cnicas: An?lise termogravim?trica (TG), Difra??o de raios X (DRX), Refinamento pelo m?todo de Rietveld, Microscopia eletr?nica de varredura (MEV), Redu??o a temperatura programada (RTP) e Medidas de histerese magn?ticas realizadas ? temperatura ambiente. De acordo com os difratogramas, a forma??o da fase perovskita com estrutura ortorr?mbica foi observada para os sistemas onde 0 ≤ x ≤ 0,5 e, rombo?drica para x = 1. Os resultados tamb?m mostraram uma diminui??o dos par?metros de rede com a substitui??o parcial do ferro por mangan?s e, conseq?entemente uma redu??o do volume da c?lula unit?ria. As curvas de histerese exibiram ferromagnetismo fraco para os sistemas preparados por ambos os m?todos de s?ntese. Entretanto, uma depend?ncia da magnetiza??o em fun??o do teor de dopante foi observada para as amostras produzidas pelo m?todo Pechini. J? para os sistemas preparados por rea??o de combust?o, verificou-se que as fases secund?rias exercem forte influ?ncia no comportamento magn?tico