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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
161

Desenvolvimento de núcleos para transformadores monofásicos de baixa potência pela metalurgia do pó

Ferreira, Carlos Antônio January 2012 (has links)
O objetivo principal do projeto foi desenvolver, através da metalurgia do pó (M/P), núcleos para transformadores monofásicos de baixa potência. O processo compreende o desenvolvimento de ligas metálicas utilizando pós de ferro, níquel e resina fenólica HRJ. Essas ligas foram misturadas, compactadas e sinterizadas ou curadas, conforme o tipo de liga. Após a confecção dos protótipos, foram feitos testes relacionados às características eletromagnéticas. A partir dos resultados obtidos puderam-se fazer comparações entre um transformador convencional, construído com um núcleo de chapas laminadas de Fe-Si com os núcleos maciços confeccionados utilizando-se a metalurgia do pó. Entre os transformadores construídos a partir da metalurgia do pó, também puderam ser observados os comportamentos com núcleos formados a partir de pó de ferro, liga de ferro e níquel, que foram sinterizados e ainda uma liga de ferro com 1% de resina fenólica HRJ que foi curada para obtenção do núcleo magnético. / The main goal this design was to develop, through process of powder Metallurgy, single-phase transformer cores for low Power. The process include the development alloys using powders of iron, nickel and phenolic resin HRJ. These alloys were mixed, compacted and sintered or cured, according to the type of alloy. After the prototype creation, tests were made related to the electromagnetic characteristics. When the results were ready comparisons were made between a conventional transformer, built with a Fe-Si rolled sheet core and bulky cores made using the powder metallurgy. Between transformers built from the powder metallurgy, could also be observed behaviors with cores formed from iron powder, iron and nickel alloy that was sintered and observed too an iron alloy with 1% phenolic resin HRJ was cured to obtain the magnetic core.
162

Integrated Inductors with Micro-Patterned Magnetic Thin Films for RF and Power Applications

January 2013 (has links)
abstract: With increasing demand for System on Chip (SoC) and System in Package (SiP) design in computer and communication technologies, integrated inductor which is an essential passive component has been widely used in numerous integrated circuits (ICs) such as in voltage regulators and RF circuits. In this work, soft ferromagnetic core material, amorphous Co-Zr-Ta-B, was incorporated into on-chip and in-package inductors in order to scale down inductors and improve inductors performance in both inductance density and quality factor. With two layers of 500 nm Co-Zr-Ta-B films a 3.5X increase in inductance and a 3.9X increase in quality factor over inductors without magnetic films were measured at frequencies as high as 1 GHz. By laminating technology, up to 9.1X increase in inductance and more than 5X increase in quality factor (Q) were obtained from stripline inductors incorporated with 50 nm by 10 laminated films with a peak Q at 300 MHz. It was also demonstrated that this peak Q can be pushed towards high frequency as far as 1GHz by a combination of patterning magnetic films into fine bars and laminations. The role of magnetic vias in magnetic flux and eddy current control was investigated by both simulation and experiment using different patterning techniques and by altering the magnetic via width. Finger-shaped magnetic vias were designed and integrated into on-chip RF inductors improving the frequency of peak quality factor from 400 MHz to 800 MHz without sacrificing inductance enhancement. Eddy current and magnetic flux density in different areas of magnetic vias were analyzed by HFSS 3D EM simulation. With optimized magnetic vias, high frequency response of up to 2 GHz was achieved. Furthermore, the effect of applied magnetic field on on-chip inductors was investigated for high power applications. It was observed that as applied magnetic field along the hard axis (HA) increases, inductance maintains similar value initially at low fields, but decreases at larger fields until the magnetic films become saturated. The high frequency quality factor showed an opposite trend which is correlated to the reduction of ferromagnetic resonant absorption in the magnetic film. In addition, experiments showed that this field-dependent inductance change varied with different patterned magnetic film structures, including bars/slots and fingers structures. Magnetic properties of Co-Zr-Ta-B films on standard organic package substrates including ABF and polyimide were also characterized. Effects of substrate roughness and stress were analyzed and simulated which provide strategies for integrating Co-Zr-Ta-B into package inductors and improving inductors performance. Stripline and spiral inductors with Co-Zr-Ta-B films were fabricated on both ABF and polyimide substrates. Maximum 90% inductance increase in hundreds MHz frequency range were achieved in stripline inductors which are suitable for power delivery applications. Spiral inductors with Co-Zr-Ta-B films showed 18% inductance increase with quality factor of 4 at frequency up to 3 GHz. / Dissertation/Thesis / Ph.D. Electrical Engineering 2013
163

"Novos materiais magnéticos para imãs de alta performance" / New magnetic materials for high performance magnets

Regina Keiko Murakami 19 September 2005 (has links)
O objetivo do presente trabalho foi desenvolver novos materiais magnéticos para ímãs de alta performance. Duas classes de materiais foram estudadas: materiais a base de (Nd,Sm)5(Fe,MT)17, onde MT é um metal de transição, e materiais nanocristalinos a base de (Nd,Pr)FeB com adições de TiC. As ligas (Nd,Sm)5(Fe,MT)17 foram preparadas por fusão em forno de arco e posteriormente foram tratadas termicamente por longos períodos (no mínimo 30 dias). Tentamos melhorar as propriedades magnéticas por meio de substituições químicas (Ti, Co, Mn, etc.) e/ou por introdução intersticial de deutério ou nitrogênio. As amostras foram caracterizadas via análise termomagnética (TMA), magnetometria de baixas temperaturas, difração de raios X e de nêutrons, e espectroscopia Mössbauer. Os principais resultados foram: a) aumento de Tc de até 70 º C; b) localização dos átomos de deutério na redecristalina. Ligas de (Nd,Pr) com adição de TiC foram preparadas por fusão de arco, sendo processadas via "melt spinning" e passando por tratamentos térmicos variados. Os promissores resultados na literatura para Nd2Fe14B+TiC foram obtidos também para Pr2Fe14B + TiC, mas não para os sistemas compostos pela fase φ e Fe3B com TiC. Porém, bons resultados foram obtidos em sistemas compostos pelas fases φ e α–Fe, com aumento de até 30% nos valores de campo coercivo Hc e aumentos de até 15% de (BH)max. / The aim of the present work was to develop new improved magnetic materials suitable for permanent magnets. Two kinds of materials were studied: (Nd,Sm)5(Fe,MT)17 based materials, were MT is a transition metal and, (Nd,Pr)FeB nanocrystalline materials (exchange spring magnets) with TiC additions. The 5:17 alloys were melted in an arc melting furnace followed by a long annealing (at least 30 days). We tried to improve the magnetic properties by means of chemical substitutions (Ti, Co, Mn, etc.) and/or by addition of interstitial atoms of deuterium or nitrogen. The samples were characterized by means of thermomagnetic analysis (TMA), low temperature magnetometry, X ray and neutron diffraction, and Mössbauer spectroscopy. The main results were: a) increase of Tc temperature (up to 70 ºC) and; b) determination of interstitial sites for deuterium. (Nd,Pr)FeB alloys with TiC additions were melted in an arc melting furnace, being processed in a melt spinner system. After the samples were heat treated at different temperatures. The promissing literature results for Nd2Fe14B+TiC were also obtained for Pr2Fe14B + TiC, but not for systems composed by Pr2Fe14B and Fe3B phases with TiC additions. However, good results were obtained in systems composed by Pr2Fe14B and α-Fe with TiC additions, with 30% increase on coercive field values Hc, and 15% increase on (BH)max.
164

Desenvolvimento de núcleos para transformadores monofásicos de baixa potência pela metalurgia do pó

Ferreira, Carlos Antônio January 2012 (has links)
O objetivo principal do projeto foi desenvolver, através da metalurgia do pó (M/P), núcleos para transformadores monofásicos de baixa potência. O processo compreende o desenvolvimento de ligas metálicas utilizando pós de ferro, níquel e resina fenólica HRJ. Essas ligas foram misturadas, compactadas e sinterizadas ou curadas, conforme o tipo de liga. Após a confecção dos protótipos, foram feitos testes relacionados às características eletromagnéticas. A partir dos resultados obtidos puderam-se fazer comparações entre um transformador convencional, construído com um núcleo de chapas laminadas de Fe-Si com os núcleos maciços confeccionados utilizando-se a metalurgia do pó. Entre os transformadores construídos a partir da metalurgia do pó, também puderam ser observados os comportamentos com núcleos formados a partir de pó de ferro, liga de ferro e níquel, que foram sinterizados e ainda uma liga de ferro com 1% de resina fenólica HRJ que foi curada para obtenção do núcleo magnético. / The main goal this design was to develop, through process of powder Metallurgy, single-phase transformer cores for low Power. The process include the development alloys using powders of iron, nickel and phenolic resin HRJ. These alloys were mixed, compacted and sintered or cured, according to the type of alloy. After the prototype creation, tests were made related to the electromagnetic characteristics. When the results were ready comparisons were made between a conventional transformer, built with a Fe-Si rolled sheet core and bulky cores made using the powder metallurgy. Between transformers built from the powder metallurgy, could also be observed behaviors with cores formed from iron powder, iron and nickel alloy that was sintered and observed too an iron alloy with 1% phenolic resin HRJ was cured to obtain the magnetic core.
165

Textura cristalografica e avaliacao de dominios magneticos em imas de PrFeB

CASTRO, ANGELA R.M. de 09 October 2014 (has links)
Made available in DSpace on 2014-10-09T12:45:37Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:07:15Z (GMT). No. of bitstreams: 1 07310.pdf: 8434532 bytes, checksum: 2fffac8743bcb0d1fd0d8045952b7835 (MD5) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP
166

Estudo do campo hiperfino magnético na sonda de Ce colocada nos compostos intermetálicos do tipo Rag(R=terra rara) e do ordenamento magnético desses compostos usando cálculos de primeiros princípios

PEREIRA, LUCIANO F.D. 09 October 2014 (has links)
Made available in DSpace on 2014-10-09T12:51:59Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:07:05Z (GMT). No. of bitstreams: 0 / Nesse trabalho foram estudados os compostos intermetalicos do tipo RAg (R = Nd, Gd e Ho) por calculos teoricos desenvolvidos dentro do formalismo da Teoria do Funcional Densidade (DFT). O metodo APW+lo (Augmented Planes Waves + lo- cal orbitals) foi aplicado para resolver a equacao de Kohn-Sham e a Aproximacao do Gradiente Generalizado (GGA) usada para tratar de forma aproximada o potencial de troca-correlacao. O codigo computacional utilizado foi o WIEN2k. As atividades foram focalizadas em duas frentes. Numa delas, determinou-se a fase magnetica do estado fundamental dos compos- tos HoAg e NdAg. Para isso, simulou-se as 4 estruturas magneticas possiveis (para as celulas cristalinas cubicas) desses dois sistemas (uma ferromagnetica (0,0,0) e as antifer-romagneticas: (0,0,¼), (¼,¼,0) e (¼,¼,¼)) e com a confeccao de gra¯cos de energia das celulas cristalinas dessas estruturas magneticas pela variacao dos volumes de tais celulas, chegou-se na estrutura magnetica (¼,¼,0) como a mais provavel para o estado fundamental magnetico de ambos os compostos. Tambem observou-se que o sistema de NdAg apre- senta uma pequena diferenca entre as energias das estruturas antiferromagnetica (¼,¼,0) e ferromagnetica. Creditou-se a esse efeito a explicacao de encontrar-se na literatura re- sultados experimentais diferentes para a estrutura magnetica do composto de NdAg puro e dopado com o atomo de 140Ce (entrando no sitio do Nd). Acredita-se que a dopagem do NdAg com o atomo de 140Ce (em uma porcao reduzida), gera alteracao no sinal da integral de troca (acoplamento RKKY), mudando-o de positivo para negativo, e isso implica na modficacao da fase magnetica do estado fundamental, passando da estrutura (¼,¼,0) µa 0,0,0). Assim, com a informacao anterior da estrutura magnetica do composto de NdAg quando dopado com o atomo de 140Ce, entrou-se na segunda etapa do estudo. Nela, fez-se os calculos das estruturas eletronicas usando a aproximacao de supercelulas nos compostos de GdAg e NdAg dopados com o atomo de Ce, garantindo que esse substituisse um atomo de terra rara nas supercelulas cristalinas montadas para determinar no Ce o campo hiperfino magnetico e suas componentes geradoras. Os compostos de GdAg e NdAg (dopados com Ce), respectivamente, tiveram suas celulas cristalinas montadas ferromagnetica e antiferromagneticamente. Utilizou-se a polarizacao orbital (DFT+U) nos eletrons da camada 4f das terras raras (excluindo-se o atomo de Gd que nao apresenta momento angular). Dessa forma, em ambos os sistemas foi possivel fazer varias simulacoes, nas quais a camada 4f do atomo de Ce foi populada de maneiras diferentes, afim de se obter varios valores de momento angular e com isso diversos resultados de campo hiperfino orbital foram conseguidos; assim, automaticamente o campo magnetico hiperfino tambem assumiu diferentes valores. Escolheu-se os sub-estados da camada 4f do Ce para serem simulados por meio da regra de Hund. Como esperado o campo hiperfino magnetico orbital gerado na camada 4f e a principal componente do campo hiper¯no total no atomo de Ce e ele apresenta sinal contrario µa componente de contato. Apesar dos resultados teoricos do campo hiperfino magnetico terem consideravel discrepancia dos resultados experimentais, pode-se verificar que o unico eletron da camada 4f do atomo de Ce (nos dois compostos) possivelmente esta em um dos seguintes sub-estados da camada 4f: ml = ¡2, ml = ¡1 ou ainda uma combinacao dos dois. / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP
167

Propriedades magnéticas de filmes nanoestruturados de FeRh e FeRh/Fe / Magnetic properties of FeRh and FeRh/Fe nanostructured films

Gerson de Carli Proença de Almeida Pessotto 12 September 2014 (has links)
As ligas de FeRh apresentam um comportamento não usual quando encontradas próximas da composição equiatômica, sendo observada uma transição de fase magnetoestrutural de primeira ordem, na qual o sistema passa de um estado antiferromagnético para um estado ferromagnético com a temperatura crítica próxima da temperatura ambiente. A temperatura crítica de transição é fortemente dependente da composição da liga, das técnicas de produção e dimensionalidade da amostra, além de fatores externos como pressão e campo magnético. No presente trabalho foram depositados, via magnetron sputtering, filmes de FeRh (monocamadas) e FeRh/Fe (bicamadas) sobre substratos monocristalinos de MgO (001), sendo utilizado duas temperaturas de deposição diferentes: 798 K e 913 K. A estrutura cristalina dos filmes foi analisada através de técnicas de medidas de difração de raios X (varredura &theta - 2 &theta, varredura em &phi e rocking curves) e as composições e espessuras dos filmes foram analisadas por medidas de RBS. A principal diferença morfológica encontrada entre as amostras foi uma melhor uniformidade na distribuição de orientações dos grãos cristalinos nos filmes depositados na temperatura mais elevada. As propriedades magnéticas, medidas por meio de um VSM equipado com um criostato e um forno, evidenciaram diferenças entre as amostras depositadas nas diferentes temperaturas mencionadas, observando-se variações significativas nas temperaturas de transição de fase e diferentes larguras dos ciclos térmicos. Também foi observado, em todas as amostras, coexistência de fases antiferromagnética e ferromagnética na camada de FeRh, principalmente na região de baixas temperaturas. As amostras depositadas em 798 K foram mais favoráveis à formação da fase FeRh antiferromagnética e, no caso das bicamadas, também apresentaram um melhor acoplamento entre as camadas de FeRh e Fe que as amostras depositadas em 913 K, favorecendo um incremento do campo coercivo e da magnetização remanente relativa do sistema. / FeRh alloys, near the equiatomic composition, present an unusual magneto structural first-order phase transition in which the system changes from antiferromagnetic to ferromagnetic state at a critical temperature close to ambient temperature. The critical transition temperature is strongly dependent on the alloy composition, production techniques and dimensionality of the sample, as well as external factors such as pressure and magnetic field. In the present work, FeRh (monolayers) and FeRh/Fe (bilayers) films were deposited on monocrystalline MgO (001) substrates, via magnetron sputtering, at two different deposition temperatures: 798 K and 913 K. The crystalline structures of the films were analyzed by using different techniques of X-ray diffraction (&theta - 2 &theta scan, &phi scan and rocking curves). The compositions and thicknesses of the films were analyzed by RBS measurements. The main morphological difference between the samples was a better uniformity in the distribution of crystalline grain orientations in the films deposited at higher temperature. The magnetic properties, which were measured by a VSM equipped with a cryostat and an oven, revealed differences between the samples obtained at different temperatures. Significant variations in the critical phase transition temperatures and different widths of thermal cycles were observed. It was also observed, in all samples, coexistence of antiferromagnetic and ferromagnetic phases in the FeRh layer, mainly at low temperatures. The samples deposited at 798 K were more favorable to the formation of the antiferromagnetic FeRh phase. In addition, for the bilayers deposited at 798 K, it was observed a better coupling between the FeRh and Fe layers in comparison to samples deposited at 913 K, favoring an increase in the coercive field and the remanence magnetization.
168

Síntese e auto-organização de nanopartículas ferromagnéticas metálicas visando aplicações em gravação magnética de ultra-alta densidade e imãs permanentes de elevado desempenho / Synthesis and self-assembling of metallic ferromagnetic nanoparticles for ultrahigh density magnetic recording and high-performance permanent magnets applications

Tiago Luis da Silva 15 May 2015 (has links)
Nanomateriais de fct-FePt, SmCo e Carbeto de Cobalto têm sido bastante estudados para a aplicação em gravação magnética e imãs de elevado desempenho, devido as suas energias magnetocristalinas e coercividades elevadas. Nanopartículas de FePt unidimensionais foram propostas na tentativa de obter melhora no alinhamento magnético das estruturas auto-organizadas. Neste trabalho, a formação de nanobastão e nanofios de FePt foi estudada através da presença de oleilamina e pequena quantidade de monóxido de carbono liberado pelo pentacarbonilferro(0). Estes dois parâmetros foram estudados a fim de analisar a influência no alongamento das nanopartículas e verificou-se que ambos atuam sinergicamente. Foram obtidos tanto nanofios de FePt ramificados de comprimento de 20-100 nm quanto nanobastões de FePt de 20-60 nm de comprimento, ambos com diâmetro de 2-3 nm. Todas as nanopartículas sintetizadas foram obtidas na fase cúbica de face centrada e o processo de tratamento térmico nas temperaturas de 450 oC e 560 oC levou a conversão para a fase tetragonal de face centrada, com custo da sinterização das nanopartículas. Os nanobastões, entretanto, apresentaram maior estabilidade térmica se comparado com o nanofio ramificado, obtendo propriedade ferromagnética na amostra. Alternativamente, têm sido obtidos satisfatoriamente nanobastões de platina para posterior recobrimento com ferro para a formação da liga FePt após o processo de recozimento. Na síntese de SmCo, foi estudada a formação da liga diretamente por via química através do uso de redutores comumente utilizandos em síntese de nanopartículas, porém foi possível observar apenas uma pequena quantidade da liga Sm2Co17 quando se utiliza o boroidreto de sódio. Isto se deve, principalmente, ao alto potencial de redução de Sm3+ e a sua instabilidade química. Entretanto, foram desenvolvidos métodos promissores para a obtenção de nanopartículas de CoO e SmCoO com tamanho e forma controlada. Além destes sistemas, tem sido obtidas diretamente através de síntese química nanopartículas de carbeto de cobalto com coercividade de até 2,3 kOe e magnetização de 45 emu/g, além de desenvolver um método geral de síntese de carbetos de outros metais. / SmCo, fct-FePt and CoC nanomaterials have been studied for application in magnetic recording and permanent magnets due to theirs high coercivity and magnetocrystalline anisotropy. One-dimensional FePt nanoparticles were proposed to improve the magnetic alignment of self-assembled system. In this work, the formation of FePt nanorods and nanowires was studied by using a small amount of carbon monoxide from the precursor pentacarbonyliron(0) and oleylamine. Both parameters of synthesis were studied and was verified that they influence the one-dimensional growth of FePt. In fact, branched FePt nanowires with 20 - 100 nm of length and nanorods with 20 - 60 nm were obtained, both with 2-3 nm of diameters. The FePt nanoparticles were obtained in face centered cubic phase and the transformation to face centered tetragonal phase was carry out in the temperatures of 450 oC and 560 oC, which led the formation of sintered nanoparticles. FePt nanorods have better thermal stability than nanowires according the results obtained. The platinum nanorods covered with iron oxide also were obtained to formation of FePt by thermal treatment. In concern of SmCo syntheses, the formation of SmCo phase directly by chemical synthesis was investigated by using some reduction agent, but was obtained a small amount of smco phase only if the sodium borohydrate was used in the synthesis. This could be occurred due to high reducing potential of Sm3+ and its chemical instability. However, some methods were obtained to obtain CoO and SmCoO nanoparticles with size and shape control. Furthermore, cobalt carbide nanoparticles were well obtained with coercivity of 2,3 kOe and magnetization of 45 emu/g, and a new general method to obtain metals carbides was developed.
169

Estudo magnético e calorimétrico sobre a série TbxPr1-xAl2 / Magnetic and calorimetric study of Tb(x)Pr(1-x)Al2 serie

Tedesco, Julio Cesar Guimarães, 1973- 20 August 2018 (has links)
Orientadores: Adelino de Aguiar Coelho, Lisandro Pavie Cardoso / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Física Gleb Wataghin / Made available in DSpace on 2018-08-20T22:51:31Z (GMT). No. of bitstreams: 1 Tedesco_JulioCesarGuimaraes_D.pdf: 2714279 bytes, checksum: fa378b69872d0cd459b74a0b4da48885 (MD5) Previous issue date: 2012 / Resumo: Neste trabalho propomos o estudo de algumas propriedades magnéticas e do efeito magnetocalórico (EMC) de compostos da família TbxPr1-xAl2, onde x = 0,1; 0,2; 0,25; 0,3; 0,4; 0,5 e 0,75. É fato conhecido que dois elementos terras-raras se acoplam antiferromagneticamente quando inseridos em uma rede cristalina do tipo (R,R¿)Al2 se um deles é um elemento terra-rara leve o outro pesado. Desta forma, era esperado que as amostras desta série apresentassem um ordenamento ferrimagnético, o que foi confirmado pelos nossos dados. Comparamos nossos resultados com sistemas semelhantes e com eles fomos capazes de entender a origem de algumas características e aspectos físicos dos materiais, incluindo o EMC. Alguns compostos estudados aqui apresentaram o efeito magnetocalórico inverso, que acontece devido à competição entre as duas subredes magnéticas acopladas antiferromagneticamente. Observamos também os comportamentos da temperatura de transição magnética e dos parâmetros de rede em função da concentração de Tb, e verificamos o deslocamento dos picos do EMC associados à temperatura de transição (TC). Algumas propriedades importantes na aplicação destes materiais em refrigeração magnética foram levantadas e comparadas com a literatura. Verificamos que dois membros da série apresentaram o efeito de Exchange Bias (EB) e, em analogia com sistemas bicamadas FM-AFM em filmes finos, fomos capazes de entender e explicar este efeito. Acreditamos que o efeito de Exchange Bias está associado à forte anisotropia apresentada pelos compostos Tb0.3Pr0.7Al2 e Tb0.25Pr0.75Al2 que ocorre em temperaturas extremamente baixas e à magnetização dos elétrons polarizados de condução. Identificamos também as temperaturas de compensação (propriedades características deste tipo de sistema) nestes compostos / Abstract: In this work we studied some magnetic properties and the magnetocaloric effect (MCE) of the series of compounds TbxPr1-xAl2, where x = 0.1, 0.2, 0.25, 0.3, 0.4, 0.5 and 0.75. It is known from the literature that the moments of a light and a heavy rare earth are antiferromagnetically coupled when they are inserted in a crystal lattice and this was confirmed by our analysis of the experimental data. We compared our results with similar systems and we were able to understand the origin of some features and physical aspects of those materials, including the magnetocaloric effect (MCE). Some compounds show the inverse MCE, associated to the competition between the two magnetic sublattices antiferromagnetically coupled. We also observed the behavior of the magnetic transition temperature (TC) and lattice parameters as a function of the concentration ('x¿), with a corresponding MCE peak shift. Some important properties regarding the application of these materials in magnetic refrigeration are discussed. Two members of the family of compounds show a shifted hysteresis curve which was assigned to the Exchange Bias (EB) effect in analogy with FM-AFM bilayers systems in thin films. We believe that the EB effect is associated with strong unidirectional anisotropy of the magnetic sublattices appeared in Tb0.3Pr0.7Al2 and Tb0.25Pr0.75Al2, which occurs at low temperatures, and with the magnetization of the polarized conduction electrons. We also identified the compensation temperature (characteristic properties of this type of system) in these compounds / Doutorado / Física / Doutor em Ciências
170

Matériaux magnétiques doux Fe-Si de hautes performances obtenus par mécanosynthèse / High performance soft magnetic materials obtained by mechanosynthesis

Stanciu, Cristina Daniela 11 May 2017 (has links)
Les alliages Fe-Si sont connus pour combiner d’excellentes propriétés magnétiques avec de bonnes propriétés électriques (forte résistivité électrique). Dans ce contexte nous avons recherché à élaborer des matériaux à forte teneur en Si, souvent difficiles à obtenir et mettre en forme industriellement. Des alliages magnétiques doux de type Fe-Si avec une teneur élevée en Si (4,5%, 6,5%, 10% et 15% massique) ont été obtenus avec succès à l’état nanocristallin par broyage mécanique et recuit. La formation des alliages a été étudiée par diffraction X, spectroscopie Mössbauer et analyses thermomagnétiques. La stabilité thermique de la poudre a été analysée par DSC. Des mesures d’aimantation ont été réalisées pour caractériser les performances magnétiques. La durée de broyage nécessaire pour la formation de l’alliage a été déterminée pour chaque teneur en Si. Pour les faibles temps de broyage, le recuit conduit à la formation du composé Fe3Si. Après la formation de l’alliage par le broyage mécanique, l’effet du recuit est seulement de réduire les tensions internes du second ordre, induites dans la poudre par le broyage. L’addition de Si conduit à la diminution de la température de Curie de 770 °C pour le Fe pur, à 725 °C pour une teneur de 4,5% massique de Si et à 550 °C pour 15% massique de Si. Pour les temps faibles de broyage, l’écart entre l’aimantation de la poudre avant et après recuit est dû à la formation du composé Fe3Si pendant le recuit, lequel a une aimantation plus faible que la solution solide de Feα(Si). Pour les longs temps de broyage, le recuit à 400 °C pour 4 heures n’a pas d’effet sur la valeur de l’aimantation à saturation. En augmentant la teneur en Si, l’aimantation à saturation de l’alliage Fe-Si décroit.Les alliages Ni3Fe (aussi connus comme Permalloys) présentent de meilleures propriétés magnétiques, mais ils ont une résistivité inférieure à celles des Fe-Si. Une voie attractive semble la combinaison des propriétés des 2 classes de matériaux doux en formant un composite. Les alliages Fe-Si précédemment obtenus ont été utilisés pour l’élaboration des poudres composites de type Permalloy/Fe-Si par la mécanosynthèse. Le broyage mécanique conduit à la formation des particules composites avec un aspect stratifié. Quatre heures de broyage de l’alliage Fe-Si avec du Ni3Fe ne conduisent pas à la formation des nouvelles phases, mais la formation d’un alliage ternaire Ni-Fe-Si résulte d’un recuit ultérieur à 900 °C. L’aimantation à saturation du composite augmente avec la croissance de la teneur le d’alliage Fe-Si, mais le temps de broyage ne semble avoir aucun effet sur cela.Une étude préliminaire a été réalisée sur l’élaboration des compacts composites de type Ni3Fe/Fe-Si par frittage flash, dans le but de préserver l’état nanocristallin par de basses températures de frittage. L’influence de la température de frittage et de la durée de maintien sur la structure, et les propriétés physiques des compacts est discutée. Des températures allant jusqu'à 750 °C pour une durée de maintien minimale ou un palier de 2 minutes maximum à 700 °C ne conduisent pas à la diffusion des éléments des alliages. L'augmentation de la température ou de la durée de frittage conduit à des cristallites plus grandes, mais qui restent dans le domaine nano pour les températures étudiées. La densité des compactes augmente avec la température et le palier. En outre, la résistivité diminue en augmentant ces 2 paramètres. L'effet de la teneur en Fe-Si est de diminuer la densité et en même temps d'augmenter la résistivité des compacts. La perméabilité magnétique est réduite avec l'augmentation de la température et de la durée de frittage, ainsi que lors de la diminution du contenu de Ni3Fe. Une température élevée et un long temps de maintien à la température de frittage conduisent à l’augmentation des pertes magnétiques. Le champ coercitif est également influencé par les paramètres de frittage, via l'effet qu'ils ont sur la taille des cristallites. / Fe-Si alloys are known for combining excellent magnetic properties with good electric characteristics (high resistivity). In this context we sought to develop materials with a relatively high Si content, often difficult to obtain and shape industrially.In this thesis, soft magnetic Fe-Si alloys with high Si content (4.5, 6.5, 10 and 15 wt. %) were successfully obtained in nanocrystalline state by mechanical alloying and annealing. The formation of the alloy was studied by X-ray and neutron diffraction, Mossbauer spectroscopy and thermomagnetic analysis. DSC technique was used in order to study the powder’s thermal stability. Magnetisation measurements were also made in order to characterise their magnetic performances. The milling duration necessary for the formation of the alloy was determined for each Si content. For low milling times, annealing leads to the formation of the Fe3Si compound. Once the alloy is formed by mechanical milling, the effect of the annealing is only to reduce the second order stress induced in the powder by the milling process. Si addition leads to the decrease of the alloy’s Curie temperature from 770 °C for pure Fe to 725 °C for a 4.5 wt. % Si and down to 550 °C if the Si content increases to 15 wt. %. For low milling times, a gap between the magnetisation of the as-milled alloy and of the milled and subsequently annealed one is due to the formation of the Fe3Si compound during annealing which has a lower magnetisation than that of the αFe (Si) solid solution. For longer milling durations, annealing at 400 °C for 4 hours has no effect on the saturation magnetisation value. By increasing the Si content, the Fe-Si alloy’s saturation magnetisation decreases.Fe-Ni alloys whose composition is close to Ni3Fe (commonly known as Permalloys) have better magnetic properties, but a resistivity well inferior to that of Fe-Si alloys. Therefore, a combination of the properties of these 2 alloy classes of soft magnetic materials into a composite seems to be an attractive route. The previously obtained Fe-Si alloys were used for the preparation of Permalloy/Fe-Si composite powders by mechanical milling. Milling leads to the formation of composite powder particles with a stratified aspect. Milling of the Fe-Si and Ni3Fe alloys for 4 hours does not lead to the formation of new phases, but a subsequent annealing at 900 °C results in the formation of a Ni-Fe-Si alloy. Saturation magnetisation of the composite increases with increasing of the Fe-Si content, but milling duration seems to have no effect on it.A preliminary study was made on the elaboration of Ni3Fe/Fe-Si composite compacts obtained by spark plasma sintering, aiming to preserve the nanocrystalline state by lower sintering temperatures. The influence of the sintering temperature and temperature holding duration on the structure, density, resistivity and magnetic properties of the compacts is discussed. Temperatures of up to 750 °C for minimal holding duration or a maintain at the temperature of 700 °C for a duration of up to 2 minutes does not lead to a diffusion of the alloys’ elements. Increasing of the sintering temperature or duration leads to larger crystallite sizes, but they remain in the nano domain for the studied temperatures. The compacts’ density increases with temperature and sintering duration. Resistivity, on the other hand decreases when increasing the aforementioned parameters. The effect of the Fe-Si content is to decrease the density and at the same time increase the compacts’ resistivity. Magnetic permeability is reduced with increasing sintering temperature and duration, as well as when decreasing of the Ni3Fe content. High temperature and long maintaining duration leads to an increase of magnetic losses. Coercive field is also influenced by sintering parameters by the effect they have on the crystallite size.

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