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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.
221

Propriétés de transport électronique de nanotubes de carbone remplis de particules magnétiques / Electrical transport properties of carbon nanotube filled with magnetic particles

Datta, Subhadeep 14 February 2011 (has links)
Les nanotubes de carbone (CNT) à basse température se comportent comme des points quantiques pour lesquelles les niveaux électroniques deviennent quantifiés. Le transport électronique à travers une jonction-CNT est caractérisé par le phénomène de blocage de Coulomb, dont les spécificités dépendent du couplage entre le nanotube et les électrodes métalliques. Le blocage de Coulomb est extrêmement sensible au moindre changement électrostatique, faisant des jonctions-CNT de précis électromètres. Par exemple, si l'on couple un système magnétique à un nanotube, le transport électronique sera influencé par l'état de spin du système magnétique (effet magnéto-Coulomb). Ce projet de thèse présente des mesures de transport électrique sur un système hybride se composant d'un nanotube de carbone rempli de nanoparticules magnétiques (Fe). Ces mesures, réalisées à très basses températures (40 mK), ont permis de mettre en évidence le comportement hystérétique de la conductance en fonction du champ magnétique, et en particulier la présence de saut de conductance à champ magnétique fini. Nous expliquons ces résultats en termes d'effet magnéto-Coulomb : le renversement d'aimantation des particules de fer à champ magnétique fini provoquant une variation de charge effective due à l'effet Zeeman. Ces mesures sont une étape vers l'étude de l'anisotropie magnétique de nanoparticules individuelles. / Carbon Nanotubes at low temperature behave as Quantum Dots for which charging processes become quantized, giving rise to Coulomb Blockade depending upon the coupling to the leads. Any small change in the electrostatic environment (tuned by the gate electrode) can induce shift of the stability diagram (so called Coulomb Diamonds) of the device, leading to conductivity variation of the Quantum Dot. A carbon nanotube can therefore be a very accurate electrometer. For example, if a magnetic system is electronically coupled to a nanotube, its electron conduction may be influenced by the spin state of the magnetic system (magneto- Coulomb effect). In this thesis, we report on the electrical transport measurements of such hybrid systems where a carbon nanotube is filled with magnetic nanoparticles such as Iron(Fe). We find that low-temperature (~40mK) current-voltage measurements of such devices can show a hysteretic behaviour in conductance with sharp jumps at certain magnetic fields. We explain the results in terms of the magneto-Coulomb effect where the spin flip of the iron island at non-zero magnetic field causes an effective charge variation in the Nanotube due to the Zeeman energy. Our studies are a step forward towards the study of the magnetic anisotropy of individual nanoparticles. We believe our findings have important implications for sensitive magnetic detectors to study the magnetization reversal of individual magnetic nanoparticle or molecule, even weakly coupled to a carbon nanotube.
222

Applications des micro-aimants aux Lab-on-Chip / Lab-on-Chip applications of micro-magnets

Fratzl, Mario 19 October 2018 (has links)
Les fonctions magnétiques sont aujourd'hui omniprésentes dans les systèmes Lab-on-Chip. Une découverte surprenante est que tandis que la recherche Lab-on-Chip se concentre sur la miniaturisation, les fonctions magnétiques sur puce sont généralement assurées par des aimants centimétriques. Comparés à ces aimants centimétriques, les champs générés par les micro-aimants bénéficient de lois d'échelle conduisant à des gradients de champ considérablement amplifiés et donc à des forces magnétiques proportionnellement accrues. Le but de cette thèse était de démontrer le potentiel des Lab-on-Chips à base de micro-aimants. Les micro-aimants haute performance ont été intégrés avec succès dans les matériaux Lab-on-Chip les plus pertinents, y compris le polymère, le silicium et le papier. Nous avons étudié des fonctions sur puce basées sur l'interaction de structures mécaniques et de micro-aimants actionnés par des gradients magnétiques, des forces et des couples. Enfin, nous avons simulé, fabriqué et testé une variété de nouvelles puces couvrant un large champ d'applications telles que les études cellulaires-mécaniques, la magnétophorèse, la manipulation de fluides sur puce et le diagnostic auprès du patient. Nous concluons que les micro-aimants intégrés présentent un grand potentiel pour les applications de laboratoire sur puce et devraient être plus largement exploités. / Magnetic functions are nowadays ubiquitous in Lab-on-Chip systems. A surprising finding is that while Lab-on-Chip research focalizes on miniaturization, on-chip magnetic functions are usually driven by centimetric magnets. Compared to those centimetric magnets, fields generated by micro-magnets benefit from scaling laws leading to dramatically increased field gradients and thus proportionally improved magnetic forces. The aim of this thesis was to demonstrate the potential of micro-magnet based Lab-on-Chips. High-performance micro-magnets were successfully integrated in the most relevant Lab-on-Chip materials including polymer, silicon and paper. We studied on-chip functions based on the interaction of mechanic structures and micro-magnets actuated by magnetic gradients, forces and torque. Finally, we simulated, fabricated and tested a variety of new chips covering a large field of applications such as cell-mechanics studies, magnetophoresis, on-chip fluid handling and Point-of-Care diagnostics. We conclude that integrated micro-magnets show great potential for lab-on-chip applications and should be more widely exploited.
223

Aplicação do Modelo de Preisach em Ímãs Nanocristalinos / Application of Preisach model in nanocrystalline magnets

Cornejo, Daniel Reinaldo 28 May 1998 (has links)
Estudamos propriedades magnéticas de ligas nano cristalinas de Sm-F e-Co. As ligas foram preparadas por mecano-síntese e posterior tratamento térmico. Como resultado, obtivemos ímãs nanocristalinos de Sm18 (Fe,Co)82 , com Sm(Fe,Co)7 como fase principal. As ligas apresentaram excelentes propriedades magnéticas: remanências relativas Mn/ Ms ~ 0.6 e coercividades na faixa 5-20 kOe, dependendo do teor de Fe nos materiais. Interações magnéticas nas ligas foram estudadas com base nos gráficos ele Henkel. Interpretamos, nestes gráficos, de maneira consistente a influência elas interações e dos estados desmagnetizados. / We studied the magnetic properties of nanocrystalline Sm-Fe-Co alloys. These alloys were prepared by mechanical alloying and subsequent annealing. We obtained nanocrystalline rnagnets of composition Sm18 (Fe, Co )82 , for which the main hard magnetic phase is Sm(Fe, Co)82. The alloys showed excellent magnetic properties: relative remanence Mn/ Ms :2; 0.6 and coercive fields ranging from 5 to 20 k0e, depending upon the amount of Fe present. Henkel plots were used in order to study magnetic interactions in these alloys. The influence of the interactions and the demagnetized state on the Henkel plots was also studied.
224

Influência dos parâmetros de processamento na microestrutura e nas propriedades magnéticas de ímãs permanentes de (Nd,Pr)FeB / Influence of processing parameters on the microstructure and magnetic properties of (Nd,Pr)FeB permanent magnets

Rafael Gitti Tortoretto Fim 07 February 2018 (has links)
Os ímãs permanentes de terras-raras desempenham um papel vital na indústria de dispositivos eletromagnéticos. As principais aplicações destes materiais na indústria são na produção de motores para veículos elétricos e híbridos e geradores para turbinas eólicas. Com a restrição chinesa a exportação de terras-raras em 2010, os elevados preços e a necessidade de substituição dos terras-raras pesados (Dy e Tb) nos ímãs permanentes, há um interesse mundial por alternativas. No processamento de ímãs permanentes de terras-raras, a moagem é uma etapa determinante, controlando e homogeneizando a microestrutura final do ímã, aumentando as propriedades magnéticas. O presente trabalho avalia a influência de diferentes tempos de moagem na microestrutura e nas propriedades magnéticas de ímãs permanentes sinterizados. Os ímãs foram preparados via metalurgia do pó, a partir de pós obtidos pelo processo de decrepitação por hidrogênio (HD) feito na liga Strip-Casting de composição (Nd,Pr)13,49Fe77,72B6Co1,1Al1,2Nb0,28Cu0,2. A moagem dos pós foi realizada em meio de ciclohexano em Moinho Planetário de Alta Energia, durante um período entre 30 e 75 minutos, com intervalos regulares de 15 minutos, a uma velocidade fixa de 200 rpm. Os ímãs produzidos foram caracterizados por Microscopia Eletrônica de Varredura (MEV), Espectroscopia de Energia Dispersiva (EDS), Difração de Raios-X (DRX), as propriedades magnéticas foram obtidas por meio de Permeâmetro e a textura cristalográfica dos ímãs foi calculada a partir dos difratogramas obtidos. O ímã produzido com 45 minutos de moagem (45-B) apresentou remanência Br = 1,38 T, coercividade intrínseca iHc = 880 KA.m-1, produto de energia máximo BHmáx = 330 KJ.m-1, fator de quadratura SF= 0,95 e grau de alinhamento < cos&theta; > = 0,96. / Rare-earth permanent magnets plays a vital role on the electromagnetic devices industry. The major applications of this material industrially are in the production of motors for electric and hybrid vehicles and magnetic generators for wind turbines. With the Chinese restriction of rare-earth exportations in 2010, the high prices and the need to substitute the heavy rare-earths (Dy,Tb) in the permanent magnets, there is a global interest in alternatives. In the processing of rare earth permanent magnets, the milling process is a determinant step, controlling and homogenizing the microstructure of the magnet, increasing its properties. The present work evaluates the influence of different high energy planetary ball milling times on the microstructure and the magnetic properties of sintered permanent magnets. The magnets were prepared via conventional powder metallurgy route, using powders obtained by the hydrogen decrepitation process (HD) made in the (Nd, Pr)13.49Fe77.72B6Co1,1Al1,2Nb0,28Cu0,2. Strip-Casting alloy. The milling process was carried under ciclohexane medium, using a High Energy Planetary Mill for a period between 30 and 75 minutes, with regular intervals of 15 minutes at a speed of 200 rpm. The magnets were characterized by Scanning Electron Microscopy (SEM), Dispersive Energy Spectroscopy (EDS), X-ray Diffraction (XRD), and magnetic properties were obtained by Permeameter. The magnet produced with 45 minutes of milling (45-B) presented Br = 1.38 T, intrinsic coercivity iHc = 880 KA.m-1, maximum energy product BHMÁX = 330 KJ.m-1 , squareness factor SF = 0,95 and alignment degree < cos&theta; > = 0,96.
225

Influência de elementos de liga na microestrutura e propriedades magnéticas de ímãs à base de PrFeCoB / Influence of alloying elements on the microstructure and magnetic properties of PrFeCoB based magnets

Silva, Melissa Rohrig Martins da 21 July 2017 (has links)
Os ímãs permanentes de terras-raras tem um papel relevante na indústria de dispositivos eletromagnéticos, principalmente no que se refere à produção de motores para veículos híbridos e elétricos e geradores para turbinas eólicas. Com a recente restrição chinesa a exportação de terras-raras, os altos preços e a necessidade de substituição do Dy nesses ímãs, há um interesse mundial por alternativas a essas questões. A adição de elementos de liga em ímãs permanentes de terras raras tem como objetivo a melhora das propriedades magnéticas. O presente trabalho avalia a influência do Ti, V, Cr, Ni, Zr, Nb e Mo na microestrutura e nas propriedades magnéticas de ímãs sinterizados. Os ímãs foram preparados via metalurgia do pó, a partir de pós obtidos pelo processo de decrepitação por hidrogênio (HD). Na produção do ímã Pr16Fe66,9Co10,7B5,7Cu0,7, sem adição de elementos de liga, foi utilizada a mistura das ligas Pr20Fe73B5Cu2 (33% em peso) e Pr14Fe64Co16B6 (67% em peso). Para avaliar a influência das adições foi utilizada a liga Pr14Fe64Co16B6M0,1, onde M = Ti, V, Cr, Ni, Zr, Nb e Mo (67% em peso). As ligas utilizadas e os ímãs produzidos foram caracterizados por Microscopia Eletrônica de Varredura (MEV) e Difração de Raios-X (DRX), e as propriedades magnéticas foram obtidas por meio de Permeâmetro. O ímã com adição de Cr (iHc = 836 KA.m-1) apresentou coercividade intrínseca 11,8% superior ao ímã sem adição de elemento de liga (iHc = 748 KA.m-1). A maior remanência foi observada para o ímã com adição de Nb (Br = 1,04 T). Os ímãs com as adições de Ti, V e Zr apresentaram os maiores valores de produto de energia (BHmáx = 145, 145 e 144 KJ.m-3, respectivamente). Já o ímã com adição de Mo apresentou o maior fator de quadratura (FQ = 0,73) entre todas as amostras, 28% superior ao ímã sem adição de elementos de liga. / Rare earth permanent magnets perform an important role in the electromagnetic devices industry, particularly in the production of hybrid and electric vehicle engines and generators for wind turbines. With the recent Chinese restriction on the export of rare-earth elements, the increasing prices and the need to replace the Dy in the permanent magnets, there is a worldwide interest in alternatives to these issues. The addition of alloying elements on rare-earth permanent magnets is one of the methods used to improve the magnetic properties. This present work evaluates the influence of Ti, V, Cr, Ni, Zr, Nb and Mo as alloying elements on the microstructure and magnetic properties of sintered Pr-Fe-Co-B based permanent magnets. The permanent magnets were produced by the conventional powder metallurgy route using powder obtained by hydrogen-decrepitation (HD) method. In order to produce the magnet Pr16Fe66,9Co10,7B5,7Cu0,7 without alloying elements the mixture of alloys method was employed, mixing two compositions: Pr20Fe73B5Cu2 (33% w.t) and Pr14Fe64Co16B6 (67% w.t). With the purpose of evaluating the influence of the alloying elements, the Pr14Fe64Co16B6M0,1 (where M= Ti, V, Cr, Ni Zr, Nb or Mo) (67% w.t) alloy was employed. The characterization of the alloys and the magnets was carried out using scanning electron microscopy (SEM), X-ray diffraction (XRD) and the magnetic properties were measured using a permeameter. The magnet with Cr addition (iHc = 836 KA.m-1) presented intrinsic coercivity 11,8% higher in comparsion with the magnet without any addition (iHc = 748 KA.m-1). The highest remanence was observed for the magnet with Nb addition (Br = 1.04 T). The magnets with additions of Ti, V and Zr produced the highest energy products (BHmáx = 145, 145 and 144 KJ.m3 respectively). The magnet with Mo addition showed the highest squareness factor (SF = 0.73) among of all samples, 28% higher than the magnet without addition.
226

Influência de elementos de liga na microestrutura e propriedades magnéticas de ímãs à base de PrFeCoB / Influence of alloying elements on the microstructure and magnetic properties of PrFeCoB based magnets

Melissa Rohrig Martins da Silva 21 July 2017 (has links)
Os ímãs permanentes de terras-raras tem um papel relevante na indústria de dispositivos eletromagnéticos, principalmente no que se refere à produção de motores para veículos híbridos e elétricos e geradores para turbinas eólicas. Com a recente restrição chinesa a exportação de terras-raras, os altos preços e a necessidade de substituição do Dy nesses ímãs, há um interesse mundial por alternativas a essas questões. A adição de elementos de liga em ímãs permanentes de terras raras tem como objetivo a melhora das propriedades magnéticas. O presente trabalho avalia a influência do Ti, V, Cr, Ni, Zr, Nb e Mo na microestrutura e nas propriedades magnéticas de ímãs sinterizados. Os ímãs foram preparados via metalurgia do pó, a partir de pós obtidos pelo processo de decrepitação por hidrogênio (HD). Na produção do ímã Pr16Fe66,9Co10,7B5,7Cu0,7, sem adição de elementos de liga, foi utilizada a mistura das ligas Pr20Fe73B5Cu2 (33% em peso) e Pr14Fe64Co16B6 (67% em peso). Para avaliar a influência das adições foi utilizada a liga Pr14Fe64Co16B6M0,1, onde M = Ti, V, Cr, Ni, Zr, Nb e Mo (67% em peso). As ligas utilizadas e os ímãs produzidos foram caracterizados por Microscopia Eletrônica de Varredura (MEV) e Difração de Raios-X (DRX), e as propriedades magnéticas foram obtidas por meio de Permeâmetro. O ímã com adição de Cr (iHc = 836 KA.m-1) apresentou coercividade intrínseca 11,8% superior ao ímã sem adição de elemento de liga (iHc = 748 KA.m-1). A maior remanência foi observada para o ímã com adição de Nb (Br = 1,04 T). Os ímãs com as adições de Ti, V e Zr apresentaram os maiores valores de produto de energia (BHmáx = 145, 145 e 144 KJ.m-3, respectivamente). Já o ímã com adição de Mo apresentou o maior fator de quadratura (FQ = 0,73) entre todas as amostras, 28% superior ao ímã sem adição de elementos de liga. / Rare earth permanent magnets perform an important role in the electromagnetic devices industry, particularly in the production of hybrid and electric vehicle engines and generators for wind turbines. With the recent Chinese restriction on the export of rare-earth elements, the increasing prices and the need to replace the Dy in the permanent magnets, there is a worldwide interest in alternatives to these issues. The addition of alloying elements on rare-earth permanent magnets is one of the methods used to improve the magnetic properties. This present work evaluates the influence of Ti, V, Cr, Ni, Zr, Nb and Mo as alloying elements on the microstructure and magnetic properties of sintered Pr-Fe-Co-B based permanent magnets. The permanent magnets were produced by the conventional powder metallurgy route using powder obtained by hydrogen-decrepitation (HD) method. In order to produce the magnet Pr16Fe66,9Co10,7B5,7Cu0,7 without alloying elements the mixture of alloys method was employed, mixing two compositions: Pr20Fe73B5Cu2 (33% w.t) and Pr14Fe64Co16B6 (67% w.t). With the purpose of evaluating the influence of the alloying elements, the Pr14Fe64Co16B6M0,1 (where M= Ti, V, Cr, Ni Zr, Nb or Mo) (67% w.t) alloy was employed. The characterization of the alloys and the magnets was carried out using scanning electron microscopy (SEM), X-ray diffraction (XRD) and the magnetic properties were measured using a permeameter. The magnet with Cr addition (iHc = 836 KA.m-1) presented intrinsic coercivity 11,8% higher in comparsion with the magnet without any addition (iHc = 748 KA.m-1). The highest remanence was observed for the magnet with Nb addition (Br = 1.04 T). The magnets with additions of Ti, V and Zr produced the highest energy products (BHmáx = 145, 145 and 144 KJ.m3 respectively). The magnet with Mo addition showed the highest squareness factor (SF = 0.73) among of all samples, 28% higher than the magnet without addition.
227

Histerisímetro de Entreferro Variável HEV : uma proposta alternativa para a caracterização de ímãs permanentes

Anocibar, Héctor Rolando January 2007 (has links)
A determinação das principais propriedades magnéticas de um ímã permanente geralmente requer sistemas de medição sofisticados e custosos. Este trabalho analisa e propõe um sistema de caracterização de ímãs permanentes de Terras Raras à temperatura ambiente de baixo custo e de implementação mais simples e rápida. Ele consiste de um circuito magnético formado pelo ímã permanente sob caracterização, uma culatra de aço, um entreferro variável e uma sonda de efeito Hall com seu respectivo gaussímetro para a medição da intensidade do campo magnético no entreferro. Como introdução se apresenta o estado da arte da caracterização dos ímãs permanentes, conceitos básicos de magnetismo e em relação aos ímãs permanentes, sua história, os principais tipos, sua importância e suas aplicações principais. Os resultados teóricos e experimentais são comparados a resultados certificados, validando o método como proposto. / Determining the main magnetic properties of a permanent magnet usually requires sophisticated and expensive measurement setups. This work analyses and proposes a low-cost system to characterize Rare Earth permanent magnets at ambient temperature with easy and fast implementation. It consists of a magnetic circuit with the permanent magnet under test, appropriate pole pieces, a variable air gap and a Hall Effect probe with its respective Gaussmeter. As an introduction, it is presented the state of the art of permanent magnets characterization, basic concepts of magnetism and its history, the main types of permanent magnets, their importance and applications. The theoretical and experimental results are compared to certified ones, validating so the method as proposed.
228

Influência dos parâmetros de processamento na microestrutura e nas propriedades magnéticas de ímãs permanentes de (Nd,Pr)FeB / Influence of processing parameters on the microstructure and magnetic properties of (Nd,Pr)FeB permanent magnets

Fim, Rafael Gitti Tortoretto 07 February 2018 (has links)
Os ímãs permanentes de terras-raras desempenham um papel vital na indústria de dispositivos eletromagnéticos. As principais aplicações destes materiais na indústria são na produção de motores para veículos elétricos e híbridos e geradores para turbinas eólicas. Com a restrição chinesa a exportação de terras-raras em 2010, os elevados preços e a necessidade de substituição dos terras-raras pesados (Dy e Tb) nos ímãs permanentes, há um interesse mundial por alternativas. No processamento de ímãs permanentes de terras-raras, a moagem é uma etapa determinante, controlando e homogeneizando a microestrutura final do ímã, aumentando as propriedades magnéticas. O presente trabalho avalia a influência de diferentes tempos de moagem na microestrutura e nas propriedades magnéticas de ímãs permanentes sinterizados. Os ímãs foram preparados via metalurgia do pó, a partir de pós obtidos pelo processo de decrepitação por hidrogênio (HD) feito na liga Strip-Casting de composição (Nd,Pr)13,49Fe77,72B6Co1,1Al1,2Nb0,28Cu0,2. A moagem dos pós foi realizada em meio de ciclohexano em Moinho Planetário de Alta Energia, durante um período entre 30 e 75 minutos, com intervalos regulares de 15 minutos, a uma velocidade fixa de 200 rpm. Os ímãs produzidos foram caracterizados por Microscopia Eletrônica de Varredura (MEV), Espectroscopia de Energia Dispersiva (EDS), Difração de Raios-X (DRX), as propriedades magnéticas foram obtidas por meio de Permeâmetro e a textura cristalográfica dos ímãs foi calculada a partir dos difratogramas obtidos. O ímã produzido com 45 minutos de moagem (45-B) apresentou remanência Br = 1,38 T, coercividade intrínseca iHc = 880 KA.m-1, produto de energia máximo BHmáx = 330 KJ.m-1, fator de quadratura SF= 0,95 e grau de alinhamento < cos&theta; > = 0,96. / Rare-earth permanent magnets plays a vital role on the electromagnetic devices industry. The major applications of this material industrially are in the production of motors for electric and hybrid vehicles and magnetic generators for wind turbines. With the Chinese restriction of rare-earth exportations in 2010, the high prices and the need to substitute the heavy rare-earths (Dy,Tb) in the permanent magnets, there is a global interest in alternatives. In the processing of rare earth permanent magnets, the milling process is a determinant step, controlling and homogenizing the microstructure of the magnet, increasing its properties. The present work evaluates the influence of different high energy planetary ball milling times on the microstructure and the magnetic properties of sintered permanent magnets. The magnets were prepared via conventional powder metallurgy route, using powders obtained by the hydrogen decrepitation process (HD) made in the (Nd, Pr)13.49Fe77.72B6Co1,1Al1,2Nb0,28Cu0,2. Strip-Casting alloy. The milling process was carried under ciclohexane medium, using a High Energy Planetary Mill for a period between 30 and 75 minutes, with regular intervals of 15 minutes at a speed of 200 rpm. The magnets were characterized by Scanning Electron Microscopy (SEM), Dispersive Energy Spectroscopy (EDS), X-ray Diffraction (XRD), and magnetic properties were obtained by Permeameter. The magnet produced with 45 minutes of milling (45-B) presented Br = 1.38 T, intrinsic coercivity iHc = 880 KA.m-1, maximum energy product BHMÁX = 330 KJ.m-1 , squareness factor SF = 0,95 and alignment degree < cos&theta; > = 0,96.
229

Développement d'un procédé électrochimique pour le recyclage du néodyme à partir de déchets électroniques / Development of an electrochemical process for the recycling of neodymium from electronic scraps

Mery, Mickaël 16 November 2018 (has links)
Le néodyme appartient à la série des lanthanides se trouvant dans le tableau périodique. Il est le composant clé des aimants permanents Nd2Fe14B implantés dans différents appareils électroniques mais aussi dans appareils dis « écologiques » comme les éoliennes, les voitures ou vélos électriques. De nos jours seulement 1 % du néodyme présent dans les déchets électroniques est recyclé. De fortes tensions géopolitiques ainsi que la croissance rapide de la demande pour ce type d’aimants conduisent à d’importantes spéculations et fluctuations sur le prix du néodyme aggravées par l’appauvrissement annoncé de la ressource.Depuis quelques décennies, plusieurs procédés de recyclage du néodyme ont été développés au niveau des laboratoires sans avoir été utilisés à l’échelle industrielle. Les procédés existants ont plusieurs désavantages comme un grand nombre d’étapes avant d’obtenir le produit final ou encore l’utilisation de grandes quantités de produits chimiques.Le but de ces recherches est le développement d’un procédé pyrochimique pouvant être une alternative à ceux déjà existants. Ce procédé permettrait de récupérer le néodyme sous sa forme métallique en seulement une étape. Pour atteindre cet objet, il a fallu élaborer un réacteur pouvant résister à de hautes températures ainsi qu’aux sels fondus pouvant être corrosifs selon leur composition. Par la suite, les propriétés électrochimiques du néodyme ont été étudiées dans différents sels fondus à base de chlorures et de fluorures afin trouver la configuration optimale pour l’extraction du néodyme contenu dans les aimants permanents.Nous avons ainsi prouvé qu’il était possible d’extraire le néodyme sous sa forme métallique contenu dans de vieux aimants permanents en une seule étape durant une électrolyse. / Neodymium belongs to the lanthanide’s serie of the period system and is the key component of the permanent magnets Nd2Fe14B which are implemented in electronic devices and “green” technologies like wind turbines or electric cars and bicycles. Nowadays, only one percent of the neodymium in electronic scraps is recycled. Due to the geopolitical considerations and a strong increase of the use of permanent magnets, there is an impoverishment of the raw material resources leading to an instable market.Since some decades, few recycling processes have been developed on a lab scale without any upscaling to the industrial scale. The existing processes have several drawbacks like multiple steps to obtain the final desired product. This means that these methods have a long process time or use a large amount of chemical productsThe aim of this research was the development of a pyrochemical process, which could be an alternative to the existing recycling processes in order to extract neodymium from electronic scraps with less steps, a smaller amount of chemical products and a higher recovery rate of the rare neodymium. For this purpose a special reaction chamber has been created which resists to the severe experimental conditions induced by the use of high temperatures and corrosive molten salts. Moreover the electrochemical behaviour of neodymium in different chloride- and fluoride-based molten salts was studied in order to find the most appropriated setup.We could prove that the pyrochemical method could be the solution to recover neodymium from the old permanent magnets under its metallic form in just one single reaction step during an electrolysis.
230

Mikrotextur und magnetische Mikrostruktur in Hartmagneten aus (Nd,Pr)2Fe14B-Verbindungen / Microtexture and magnetic microstructure of (Nd,Pr)2Fe14B permanent magnets

Khlopkov, Kirill 13 March 2007 (has links) (PDF)
In der vorliegenden Arbeit werden die Zusammenhänge zwischen der magnetischen Mikrostruktur und der Ausrichtung der Kristallite, sowohl in Sintermagneten als auch in feinkristallinen, warmumgeformten Magneten auf Nd2Fe14B- und Pr2Fe14B-Basis, untersucht. Die EBSD-Technik (electron backscatter diffraction) wurde für Sintermagnete und für feinkristalline, warmumgeformte Magnete auf Nd2Fe14B-Basis erstmals erfolgreich eingesetzt, um eine quantitative Texturanalyse durchzuführen. Die Polfiguren des hoch texturierten Sintermagneten bzw. warmumgeformten Magneten zeigen eine stark ausgeprägte [001] Fasertextur. Aus dem Vergleich von REM-, EBSD- und Kerr-Untersuchungen an ein- und derselben Probenoberfläche der Sintermagnete konnte quantitativ gezeigt werden, wie die Domänenstruktur von der individuellen Orientierung der Nd2Fe14B-Körner abhängt. Die Domänenstruktur der hoch texturierten Sintermagnete weist auf eine starke magnetostatische Wechselwirkung zwischen den Kristalliten hin. In den Heißpresslingen und in den warmumgeformten Magneten auf Nd2Fe14B-Basis und Pr2Fe14B-Basis wurden Wechselwirkungsdomänen mittels Magnetkraftmikroskopie nachgewiesen. Die Wechselwirkungsdomänen, deren Größe stark vom Umformgrad abhängt, sind immer größer als die einzelnen Kristallite. Die Bildung der Wechselwirkungsdomänen wurde auf magnetostatische Wechselwirkung zwischen den Kristalliten zurückgeführt, was mit Hilfe der Wohlfarth-Analyse der Remanenzverhältnisse bestätigt werden konnte. Die magnetische Mikrostruktur der warmumgeformten Magnete wurde mit einem Modell, das auf der Bildung von Ketten magnetischer Momente (parallel zur Kettenachse) beruht, beschrieben. Unterhalb der Temperatur des Spinumorientierungsüberganges der Nd2Fe14B-Phase weisen die Sintermagnete rechteckige Domänenmuster auf. Diese magnetische Mikrostruktur wird durch eine spezifische Verteilung der Domänenwände in Bezug auf Änderungen der magnetischen Anisotropie ausgebildet. Im Gegensatz dazu ändern sich die Wechselwirkungsdomänen in dem warmumgeformten Magneten nicht, was auf die starke magnetostatische Wechselwirkung zwischen den Kristalliten zurückgeführt wurde. / In this work, the correlation between magnetic domain structure and grain alignment in sintered and die-upset magnets, based on Nd2Fe14B and Pr2Fe14B compounds, is investigated. For the first time, EBSD (electron backscatter diffraction) has been successfully applied to conduct a quantitative analysis of the texture of sintered and die-upset Nd2Fe14B magnets. Pole figures of the highly textured sintered and die-upset magnets show a strong [001] fiber texture. By a comparison of SEM, EBSD and Kerr images of the same surface of sintered magnets it was possible to correlate the domain structure of individual grains to their orientation. The domain structure of the highly textured sintered magnet indicates to the presence of a strong magnetostatic interaction between individual grains. Interaction domains have been studied in hot-pressed und die-upset magnets based on Nd2Fe14B and Pr2Fe14B compounds by MFM. The lateral expansion of interaction domains is always larger than grain size and depends from the degree of deformation. The formation of interaction domains is attributed to magnetostatic interaction between individual grains, which has been confirmed by a Wohlfarth’s analysis of the remanence ratio. The magnetic domain structure of die-upset magnets can be described by a model, based on the formation of chains of magnetic moments parallel to the chain direction. Below the spinreorientation temperature of the Nd2Fe14B phase, sintered magnets show a rectangular domain structure. This domain structure is formed by a specific domain wall distribution corresponding to changes of the magnetocrystalline anisotropy. In contrast to this, the interaction domains in the die-upset magnets show no changes below the spinreorientation temperature, what can be also ascribed to the magnetostatic interaction between individual grains.

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