Made available in DSpace on 2014-12-17T14:07:12Z (GMT). No. of bitstreams: 1 RaimisonBA_DISSERT.pdf: 2147079 bytes, checksum: db6881c15458f1e487de74465b7088a0 (MD5) Previous issue date: 2013-07-04 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Magnetic ceramics have been widely investigated, especially with respect to intrinsic and extrinsic characteristics of these materials. Among the magnetic ceramic materials of technological interest, there are the ferrites. On the other hand, the thermal treatment of ceramic materials by microwave energy has offered various advantages such as: optimization of production processes, high heat control, low consumption of time and energy among others. In this work were synthesized powders of Ni-Zn ferrite with compositions Ni1- xZnxFe2O4 (0.25 ≤ x ≤ 0.75 mols) by the polymeric precursor route in two heat treatment conditions, conventional oven and microwave energy at 500, 650, 800 and 950?C and its structural, and morphological imaging. The materials were characterized by thermal analysis (TG/ DSC), X-ray diffraction (XRD), absorption spectroscopy in the infrared (FTIR), scanning electron microscopy (SEM), X-ray spectroscopy and energy dispersive (EDS) and vibrating sample magnetometry (VSM). The results of X-ray diffraction confirmed the formation of ferrite with spinel-type cubic structure. The extrinsic characteristics of the powders obtained by microwave calcination and influence significantly the magnetic behavior of ferrites, showing particles ferrimagn?ticas characterized as soft magnetic materials (soft), is of great technological interest. The results obtained led the potential application of microwave energy for calcining powders of Ni-Zn ferrite / Cer?micas magn?ticas t?m sido amplamente investigadas, principalmente com rela??o as caracter?sticas intr?nsecas e extr?nsecas destes materiais. Dentre os materiais cer?micos magn?ticos de interesse tecnol?gico, destacam-se as ferritas. Por outro lado, o tratamento t?rmico de materiais cer?micos por energia de microondas tem oferecido diversas vantagens, tais como: otimiza??o dos processos de obten??o, alto controle de aquecimento, menor consumo de tempo e energia entre outras. Neste trabalho, foram sintetizados p?s de ferritas Ni-Zn com composi??es Ni1-xZnxFe2O4 (0,25 ≤ x ≤ 0,75 mols) pela rota dos precursores polim?ricos em duas condi??es de tratamento t?rmico, em forno convencional e por energia de microondas a 500, 650, 800 e 950?C, e sua caracteriza??o estrutural, morfol?gica e magn?tica. Os materiais obtidos foram caracterizados por an?lises t?rmicas (TG/DSC), difra??o de raios x (DRX), espectroscopia de absor??o na regi?o do infravermelho (FTIR), microscopia eletr?nica de varredura (MEV), espectroscopia de raios X por dispers?o de energia (EDS) e magnetometria de amostra vibrante (VSM). Os resultados da difra??o de raios X confirmaram a forma??o da ferrita com estrutura c?bica do tipo espin?lio. As caracter?sticas extr?nsecas dos p?s obtidos e a calcina??o por microondas influenciaram de forma significativa o comportamento magn?tico das ferritas, apresentando part?culas ferrimagn?ticas, caracterizadas como materiais magn?ticos moles (macias), sendo de grande interesse tecnol?gico. Os resultados obtidos induziram o potencial de aplica??o de energia de microondas para a calcina??o de p?s de ferritas Ni-Zn

Made available in DSpace on 2014-12-17T15:42:20Z (GMT). No. of bitstreams: 1 AdilaPGR_DISSERT.pdf: 1981953 bytes, checksum: be68a9256a00a195734cb22cb0bdc5b2 (MD5) Previous issue date: 2014-12-11 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / The ferrite composition Ni1 - xCoxFe2O4 (0 ≤ x ≤ 0.75) were obtained by the method of microwave assisted synthesis and had their structural and magnetic properties evaluated due to the effect of the substitution of Ni by Co. The compounds were prepared: according to the concept of chemical propellants and heated in the microwave oven with power 7000kw. The synthesized material was characterized by absorption spectroscopy in the infrared (FTIR), Xray diffraction (XRD) using the Rietveld refinement, specific surface area (BET) , scanning electron microscopy (SEM) with aid of energy dispersive analysis (EDS) and magnetic measurements (MAV). The results obtained from these techniques confirmed the feasibility of the method of synthesis employed to obtain the desired spinel structure, the ferrite, nickel ferrite as for nickel doped with cobalt. The results from XRD refinement ally showed the formation of secondary phases concerning stages α - Fe2O3, FeO, (FeCo)O e Ni0. On the other hand, there is an increase in crystallite size with the increase of cobalt in systems, resulting in an increased crystallinity. The results showed that the BET systems showed a reduction in specific surface area with the increase of cobalt and from the SEM, the formation of irregular porous blocks and that the concentration of cobalt decreased the agglomerative state of the system. The magnetic ferrites studied showed different characteristics according to the amount of dopant used, ranging from a very soft magnetic material (easy magnetization and demagnetization ) - for the system without cobalt - a magnetic material with a little stiffer behavior - for systems containing cobalt. The values of the coercive field increased with the increasing growth of cobalt, and the values of saturation magnetization and remanence increased up to x = 0,25 and then reduced. The different magnetic characteristics presented by the systems according to the amount of dopant used, allows the use of these materials as intermediates magnetic / As ferritas de composi??o Ni1−xCoxFe2O4 (0≤x≤0,75) foram obtidas atrav?s do m?todo de s?ntese assistida por microondas e tiveram suas propriedades estruturais e magn?ticas avaliadas em fun??o do efeito da substitui??o do Ni pelo Co. Os compostos foram preparados de acordo com o conceito da qu?mica dos propelentes e aquecidos em forno micro-ondas com pot?ncia 7000kw. O material sintetizado foi caracterizado por espectroscopia de absor??o na regi?o do infravermelho (FTIR), difra??o de raios X (DRX), com o uso do refinamento pelo m?todo de Rietveld, ?rea superficial espec?fica (BET), microscopia eletr?nica de varredura (MEV) com aux?lio de an?lise por dispers?o de energia (EDS) e medidas magn?ticas (MAV). Os resultados obtidos, a partir destas t?cnicas confirmaram a viabilidade do m?todo de s?ntese empregado para a obten??o da estrutura espin?lio desejada, tanto para a ferrita de n?quel quanto para as ferritas de n?quel dopadas com cobalto. Os resultados do DRX, aliado ao refinamento, mostraram a forma??o de fases secund?rias tais como as fases α - Fe2O3, FeO, (FeCo)O e Ni0. Por outro lado, observou-se um aumento no tamanho do cristalito com o incremento do cobalto nos sistemas, implicando em um aumento da cristalinidade. Os resultados do BET mostraram que os sistemas apresentaram uma redu??o da ?rea superficial espec?fica com o incremento do cobalto e a partir do MEV observou-se a forma??o de blocos porosos irregulares e que o aumento da concentra??o de cobalto dimunuiu o estado de aglomera??o dos sistemas. As ferritas estudadas apresentaram caracter?sticas magn?ticas diferenciadas de acordo com a quantidade do dopante utilizado, variando de um material magn?tico bastante mole (f?cil magnetiza??o e desmagnetiza??o) - para o sistema sem cobalto - a um material magn?tico com comportamento um pouco mais duro - para os sistemas contendo cobalto. Os valores do campo coercitivo aumentaram com o crescente incremento do cobalto, e os valores de magnetiza??o de satura??o e reman?ncia aumentaram at? x=0,25 e depois reduziram. As caracter?sticas magn?ticas diferenciadas apresentadas pelos sistemas, de acordo com a quantidade de dopante utilizado, permite o uso desses materiais como magn?ticos intermedi?rios

Made available in DSpace on 2014-12-17T15:42:21Z (GMT). No. of bitstreams: 1 JoseEMS_TESE.pdf: 5374821 bytes, checksum: 56fe60cd3bbf0a42f7512c62fe5b976e (MD5) Previous issue date: 2013-03-08 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Were synthesized spinel-type ferrites with general formula Ni0,8Mg0.2-xMxFe2O4, where M represents the doping Mn, Co or Mn + Co simultaneously, x ranges for the values 0.02, 0.05 and 0.1. The value of x was divided by 2 in cases where M equals Mn and Co conjugates. We used the citrate precursor method and heat treatment to obtain the phases at 1100?C. The materials were characterized by XRD, TGA/ DTGA, SEM, MAV and reflectivity measurements by the method of waveguide. Powders to 350?C/3.5 h were crystalline and nanosized. According to the results this temperature all powders have a percentage of ferrite phase over 90%. The composition had the addition of Mn and Co simultaneously showed a higher percentage of secondary phase NiO, 5.8%. The TGA/DTGA curves indicate that this sample reached phase (s) crystalline (s) at lowest temperatures. The X-ray diffractograms of the samples calcined at 350?C and 1100?C were treated with the Rietveld refinament technique. The powders calcined at 1100 ?C/3h in air show to be 100% except spinel phase composition with 0.02 doping. The micrographs show clusters of particles with sizes smaller than 1 μm in calcination temperature of 1100?C which agreed with the result of Rietveld refinement. In the compositions doped with Mn were higher values of magnetization (45.90 and 53.20 Am2/kg), which did not cause high microwave absorption. The theoretical calculation of magnetization (MT) was consistent with the results, considering that there was agreement between the increase of magnetization experimental and theoretical. It was observed that there was the interrelation of the final effect of absorption with the thickness of MARE, the composition of ferrimagnetic materials and in particular the specific values of frequency. The analysis shows that the reflectivity increases in the concentration of cobalt increased the frequency range and also for absorption 10.17 GHz and 84%, respectively. The best result of chemical homogeneity and the value of 2.96 x 10-2 tesla coercive field were crucial for high performance ferrite absorber with 0.1 cobalt. The Cobalt has high magnetocrystalline anisotropy, it is associated with an increased coercive field, Hc. Therefore, this property improves the results of reflectivity of spinel ferrites / Foram sintetizadas ferritas do tipo espin?lio com f?rmula geral Ni0,8Mg0,2-xMxFe2O4, onde M representa os dopantes Mn, Co ou Mn + Co simultaneamente, x varia para os valores 0,02; 0,05 e 0,1. O valor de x foi dividido por 2 nos casos em que M equivale a Mn com Co conjugados. Foi utilizado o m?todo dos citratos precursores e tratamento t?rmico na obten??o das fases a 1100?C. Os materiais foram caracterizados por DRX, TGA/DTGA, MEV, MAV e medidas de refletividade pelo m?todo de guia de ondas. Os p?s a 350?C/3,5h foram cristalinos e nanom?tricos. De acordo com os resultados nesta temperatura todos os p?s apresentam um percentual de fase ferrita superior a 90%. A composi??o que teve a adi??o de Mn e Co simultaneamente apresentou maior percentual de fase secund?ria NiO, 5,8%. As curvas TGA/DTGA indicam que essa amostra alcan?ou fase(s) cristalina(s) em temperaturas mais baixas. Os difratogramas de raios X das amostras calcinadas a 350?C e 1100?C foram tratados pela t?cnica de refinamento Rietveld. Os p?s calcinados a 1100?C/3h em atmosfera ambiente mostram ser 100% de fase espin?lio exceto a composi??o com 0,02 de dopantes. As micrografias apresentam aglomerados de part?culas com tamanhos menores que 1 μm na temperatura de calcina??o de 1100?C, o que concordou com o resultado de refinamento Rietveld. Nas composi??es dopadas com Mn ocorreram os maiores valores de magnetiza??o (45,90 e 53,20 Am2/kg), o que n?o acarretou alta absor??o de microondas. O c?lculo te?rico da magnetiza??o (MT) foi coerente com os resultados, considerando-se que houve concord?ncia entre o aumento das magnetiza??es experimental e te?rica. Observa-se que houve interrela??o do efeito final de absor??o com a espessura do MARE, a composi??o do material ferrimagn?tico em particular e os valores espec?ficos de freq??ncia. A an?lise de refletividade indica que o aumento na concentra??o de cobalto aumentou a faixa de freq??ncia e a absor??o para 10,17 GHz e 84%, respectivamente. O resultado indica que a melhor homogeneidade qu?mica e o valor 2,96 x 10-2 tesla de campo coercitivo foram determinantes para o alto desempenho absorvedor da ferrita com 0,1 de cobalto. O Cobalto tem alta anisotropia magnetocristalina, isto est? associado ao aumento do campo coercitivo, Hc. Portanto, essa propriedade melhora os resultados de refletividade das ferritas espin?lio