Made available in DSpace on 2014-12-17T15:41:43Z (GMT). No. of bitstreams: 1 JoseEMS.pdf: 2230919 bytes, checksum: f0f4e57c89f3eae4282c6daae0fe0aba (MD5) Previous issue date: 2008-04-18 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / It was synthesized different Ni1-xMgxFe2O4 (0,2 ≤ x ≤ 0,7) compositions by use of citrate precursor method. Initially, the precursory citrates of iron, nickel and magnesium were mixed and homogenized. The stoichiometric compositions were calcined from 350?C to 1200?C at ambient atmosphere or in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, magnetic measures and reflectivity using the wave guide method. I was observed pure magnetic phase formation between 350?C and 500?C, with formation of ferrite and hematite after 600?C at ambient atmosphere. The calcined powder at argon atmosphere formed pure ferromagnetic phase at 1100?C and 1200?C. The Rietveld analyses calculated the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (11-66 nm), that at 900?C/3h presents micrometric sizes (0,45 - 0,70 Om). The better magnetization results were 54 Am2/Kg for x= 0,2 composition, calcined at 350?C/3h and 30 min, and 55,6 Am2/Kg for x= 0,2 1200?C, calcined in argon. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The materials presented absorption less or equal the 50 % in ranges specific frequency. As for the 2,0 and 3,0 thickness (in 11,0 - 11,8 GHz), the reflectivity of the x= 0,3, 0,5 and 0,4 compositions, all calcined at 900?C/3h showed agreement with MS and O. Various factors contribute for the final radiation absortion effect, such as, the particle size, the magnetization and the polymer characteristics in the MARE composition. The samples that presented better magnetization does not obtaining high radiation absorption. It is not clear the interrelaction between the magnetization and the radiation absorption in the strip of frequencies studied (8,2 - 12,4 GHz) / Foram sintetizadas diferentes composi??es da ferrita Ni1-xMgxFe2O4 com (0,2 ≤ x ≤ 0,7) pelo uso do m?todo dos citratos precursores. Para se obter a fase estequiom?trica Ni1-xMgxFe2O4, inicialmente foram misturados e homogeneizados os citratos precursores de ferro, n?quel e magn?sio. As composi??es estequiom?tricas foram calcinadas entre as temperaturas de 350?C e 1200?C, em atmosfera ambiente ou de arg?nio. Os p?s calcinados foram caracterizados por DRX, TGA/DTG, FTIR, medidas magn?ticas e refletividade pelo m?todo de guia de ondas. Foi observada a forma??o de fase pura ferrimagn?tica entre 350?C e 500?C, formando ferrita e hematita ap?s 600?C, em atmosfera ambiente. O p? calcinado em atmosfera de arg?nio formou fase ferrimagn?tica pura em 1100?C e 1200?C. A an?lise pelo m?todo de Rietveld calculou o n?vel de ocupa??o dos c?tions e o tamanho de cristalito. A an?lise obteve tamanhos de cristais nanom?tricos, (11 - 66 nm), que a 900?C/3h apresentam tamanhos microm?tricos (0,45 0,70 Om). Os melhores resultados de magnetiza??o foram 54 Am2/Kg para a composi??o x= 0,2, calcinada a 350?C/3h e 30 min, e 55,6 Am2/Kg para x= 0,2 a 1200?C, calcinada em arg?nio. As histereses mostraram um perfil de materiais magn?ticos moles. Dois processos de magnetiza??o foram considerados, o superparamagnetismo a baixa temperatura e a forma??o de dom?nios magn?ticos em altas temperaturas. Os materiais apresentaram absor??o igual ou inferior a 50 % em faixas de freq??ncias espec?ficas. Para as espessuras 3,0 e 2,0 mm (em 11-11,8 GHz), as refletividades das composi??es x= 0,3, x= 0,5 e x= 0,4, todas a 900?C/3h demonstraram concord?ncia com MS e O. V?rios fatores contribuem para o efeito final de absor??o de radia??o, tais como, o tamanho de part?culas, a magnetiza??o, e as caracter?sticas do pol?mero na composi??o do MARE. As amostras que apresentaram maiores magnetiza??es n?o atingiram alta absor??o de radia??o. N?o ficou esclarecido a interrela??o entre a magnetiza??o e a absor??o de radia??o na faixa de freq??ncia estudada (8,2 12,4 GHz)

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 2014-12-17T15:41:43Z (GMT). No. of bitstreams: 1 AlyssonEGM.pdf: 4274696 bytes, checksum: 0f940193275b15ce59b4b1f45e3dc11c (MD5) Previous issue date: 2008-09-24 / Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico / Were synthesized different ferrites NixZn1-xFe2O4 (0,4 ≤ x ≤ 0,6) compositions by using citrate precursor method. Initially, the precursors citrates of iron, nickel and zinc were mixed and homogenized. The stoichiometric compositions were calcined at 350?C without atmosphere control and the calcined powders were pressed in pellets and toroids. The pressed material was sintered from 1100? up to 1200?C in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, SEM and vibrating sample magnetometer (VSM). All sintered samples were characterized using XRD, SEM, VSM and measurements of magnetic permeability and loss factor were obtained. It was formed pure ferromagnetic phase at all used temperatures. The Rietveld analyses allowed to calculate the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (12-20 nm) to the calcined powder. By SEM, the sintered samples shows grains sizes from 1 to 10 μm. Sintered densities (ρ) were measured by the Archimedes method and with increasing Zn content, the bulk density decrease. The better magnetization results (105-110 emu/g) were obtained for x=0,6 at all sintering temperatures. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The sintered toroids presents relative magnetic permeability (μr) from 7 to 32 and loss factor (tanδ) of about 1. The frequency response of toroids range from 0,3 kHz to 0,2 GHz. The composition x=0,5 presents both greater μr and tanδ values and x=0,6 the most broad range of frequency response. Various microstructural factors show influence on the behavior of μr and tanδ, such as: grain size, porosity across grain boundary and inside the grain, grain boundary content and domain walls movement during the process of magnetization at high frequency studies (0,3kKz 0,2 GHz) / Foram sintetizadas diferentes composi??es da ferrita Ni1-xZnxFe2O4 com 0,4 ≤ x ≤ 0,6 pelo uso do m?todo dos citratos precursores. Para se obter a fase estequiom?trica do sistema Ni1-xZnxFe2O4 foram misturados e homogeneizados os citratos precursores de ferro, n?quel e zinco. As composi??es estequiom?tricas foram calcinadas em atmosfera ambiente na temperatura de 350?C e depois prensadas em pastilhas e tor?ides. As amostras prensadas foram sinterizadas nas temperaturas de 1100?, 1150? e 1200?C em atmosfera de arg?nio. Os p?s calcinados foram caracterizados por DRX, TGA/DTG, FTIR, MEV e magnetometria de amostra vibrante (MAV) e as amostras sinterizadas por DRX, MEV, MAV, massa espec?fica e medidas de permeabilidade e perdas magn?ticas. Observou-se a forma??o de fase pura ferrimagn?tica em todas as temperaturas aplicadas. A an?lise pelo m?todo de Rietveld calculou o n?vel de ocupa??o dos c?tions e o tamanho de cristalito. Foram obtidos tamanhos de cristais nanom?tricos, de 12 a 20 nm para os p?s calcinados. Por MEV, as amostras sinterizadas apresentam tamanhos de gr?os na faixa de 1 a 10 μm. A massa espec?fica (ρ) do material sinterizado apresenta uma tend?ncia de diminui??o com a adi??o de Zn. Os melhores resultados de magnetiza??o foram obtidos para x=0,6 nas tr?s temperaturas de sinteriza??o, variando de 105 a 110 emu/g. As histereses mostram um perfil de materiais magn?ticos moles. Dois processos de magnetiza??o foram considerados, o superparamagnetismo a baixa temperatura (350?C) e a forma??o de dom?nios magn?ticos em altas temperaturas. Os materiais sinterizados apresentam permeabilidade (μ) de algumas unidades, de 7 a 30, e perdas magn?ticas (tanδ) por volta de 1. A resposta em freq??ncia dos n?cleos toroidais est? na faixa de 0,3 kHz a 0,2 GHz. Os maiores valores de μ e tanδ s?o para x=0,5 e a maior faixa de resposta em freq??ncia ? para x=0,6. V?rios fatores da microestrutura contribuem para o comportamento das grandezas μ e tanδ, tais como: os tamanhos dos gr?os, porosidade inter e intragranular, quantidade de contornos de gr?os e os aspectos da din?mica das paredes de dom?nios quando excitadas magneticamente sob alta freq??ncia

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