Ímãs híbridos aglomerados foram preparados por compactação uniaxial de pós magnéticos e curados ao ar e sob vácuo. Correlações entre tratamentos de cura, propriedades mecânicas e propriedades magnéticas foram estabelecidas com base em resultados obtidos por Histeresigrafia, Magnetometria de Amostra Vibrante, ensaios de Compressão e análises de Microscopia Óptica e Eletrônica de Varredura. Parâmetros como pressão de compactação, tempo e influência da temperatura e da atmosfera de cura nas propriedades mecânicas e magnéticas de ímãs aglomerados utilizados como padrão de referência, preparados com pós MQEP de NdFeB (partículas magnéticas impregnadas com resina epóxi), foram discutidos na primeira parte deste trabalho. A melhor condição de cura foi à temperatura de 200°C por cinco horas, sob vácuo. O produto de energia máximo (BHMáx) obtido para os ímãs padrão, curados ao ar e sob vácuo, foi de 76,2 KJ/m³ e 80,5 KJ/m³, respectivamente. Na segunda parte deste trabalho, ímãs híbridos foram produzidos a partir da mistura do pó MQEP aditivado com diferentes quantidades de pós de ferrite de estrôncio e NdFeB reprocessado por HDDR. O melhor resultado de BHMáx obtido para os ímãs híbridos de MQEP com ferrite de estrôncio e MQEP com pó reprocessado por HDDR, curados sob vácuo, foi de 73,2 KJ/m³ e 78,3 kJ/m³, respectivamente. Ímãs híbridos de MQEP com pó reprocessado por HDDR apresentaram melhor desempenho magnético que os ímãs híbridos de MQEP com pós de ferrite de estrôncio. / Bonded hybrid magnets were prepared by uniaxial pressing of magnetic powders cured in air and under vacuum. Correlations between cure treatments, mechanical properties and magnetic properties were established based on results obtained by Hysteresigraphy, Vibrating Sample Magnetometry, Compression tests, Optical Microscopy and Scanning Electron Microscopy. Parameters such as compaction pressure and the influence of time, temperature and atmosphere during the curing step in the mechanical and magnetic properties of the bonded magnets used as reference patterns, produced with NdFeB MQEP powder (epoxy encapsulated magnetic particles) were discussed in the first part of this work. The better cure condition was that performed at 200 oC for 5 hours under vacuum. The maximum energy product (BHMax) obtained for the patterns bonded magnets cured in air and under vacuum was 76.2 KJ/m³ and 80.5 KJ/m³, respectively. In the second part of this work, hybrid bonded magnets were produced by the mixture of MQEP powder with different amounts of strontium ferrite powder and NdFeB powder reprocessed by HDDR. The best results of BHMax obtained for the hybrid MQEP magnets with strontium ferrite powder and NdFeB reprocessed by HDDR, cured under vacuum were 73.2 KJ/m³ and 78.3 kJ/m³, respectively. Hybrid MQEP bonded magnets produced with the addition of HDDR reprocessed powder presented better magnetic performance than that obtained with strontium ferrite powders.

Neste trabalho, avaliou-se inicialmente a preparação de ímãs sinterizados de Pr16Fe76B8 (% at.) por meio de moagem de alta energia em moinho tipo planetário, averiguando-se os efeitos do tempo de moagem bem como da velocidade rotacional do moinho. Encontraram-se as melhores propriedades magnéticas para um magneto preparado com a matéria-prima cominuída durante 75 minutos e velocidade rotacional de 200rpm [JR = (1,02 ± 0,02) T, 0JHc = (1,42 ± 0,03) T e (BH)max = (200 ± 4) kJm-3]. De forma a melhorar a remanência, reduziu-se o tempo de exposição da liga ao hidrogênio, de 60 minutos para 2 minutos, obtendo-se um ímã com JR = (1,14 ± 0,02) T, 0JHc = (1,44 ± 0,03) T e (BH)max = (250 ± 5) kJm-3, constatando-se que a causa para a reduzida remanência no primeiro caso decorria do baixo grau de orientação cristalográfica. Durante esta investigação, desenvolveu-se e validou-se uma nova metodologia para quantificação do parâmetro . Posteriormente, propôs-se uma correlação quantitativa inédita entre a microestrutura e o fator de quadratura em magnetos anisotrópicos de TR16Fe76B8 (TR = Nd ou Pr) sinterizados. A expressão apresentada utiliza o tamanho, a elongação e a circularidade médios dos grãos e seus respectivos desvios padrões. Melhora-se o fator de quadratura quando a microestrutura apresenta grãos arredondados e com estreita distribuição de tamanho. A homogeneidade de tamanho dos grãos apresenta uma influência maior sobre o fator de quadratura quando comparada à homogeneidade de forma dos grãos. Ademais, verificou-se que o tratamento térmico após a sinterização melhora a ix homogeneidade de forma ao passo que a moagem melhora a homogeneidade de tamanho dos grãos. Avaliou-se, adicionalmente, o efeito da temperatura sobre o fator de quadratura em magnetos sinterizados anisotrópicos, verificando-se que o mesmo é controlado principalmente por sua microestrutura e confirmando a expressão previamente proposta. Além disso, propôs-se uma correlação quantitativa entre o produto de energia máximo e o fator de quadratura. Compararam-se valores experimentais e calculados, utilizando a expressão apresentada, e a discrepância encontrada foi de 5%. Por fim, avaliou-se qual seria o valor mínimo do fator de quadratura em ímãs sinterizados, constatando-se que magnetos isotrópicos devem apresentar o menor valor para tal parâmetro em virtude do reduzido grau de alinhamento cristalográfico. Ademais, verificou-se que para este tipo de amostra, em geral, 0,20 FQ 0,30. / In this work, it has firstly been evaluated the preparation of Pr16Fe76B8 sintered permanent magnets (% at.) by means of high-energy milling using a planetary ball mill. The influence of both milling speed and time has been verified. The best magnetic properties [JR = (1.02 ± 0.02) T, 0JHc = (1.42 ± 0.03) T and (BH)max = (200 ± 4) kJm-3] have been found for a permanent magnet prepared with the magnetic alloy milled during 75 minutes using a rotational milling speed of 200 rpm. In order to improve the remanence, the hydrogen decrepitation process time has been reduced from 60 minutes to 2 minutes. In this case, it has been obtained a sintered magnet with JR = (1.14 ± 0.02) T, 0JHc = (1.44 ± 0.03) T and (BH)max = (250 ± 5) kJm-3 due to the improvement of crystallographic alignment of the hard magnetic phase. During such investigation, a new methodology to quantify the parameter has been developed. Subsequently, for the first time, a quantitative correlation between the microstructure and the squareness factor in anisotropic sintered RE16Fe76B8 (RE = Nd or Pr) magnets has been proposed. The presented expression utilizes the mean size, the mean elongation and the mean roundness of the hard magnetic grains as well as their respective standard deviations. The squareness factor can be improved with a microstructure with rounder grains and with a sharp grain size distribution. The grain size homogeneity is more important to enhance the squareness factor compared to grain shape homogeneity. Furthermore, it has also been verified that the annealing after sintering improves the grain shape homogeneity and the milling enhances the xi grain size homogeneity. Moreover, the effect of the temperature on the squareness factor of anisotropic sintered magnets has also been evaluated. Such parameter is mainly controlled by the samples microstructure, in agreement with the proposed expression. Furthermore, a quantitative correlation between the maximum energy product and the squareness factor has been proposed. Experimental and calculated values have been compared and the discrepancy found has been, in general, inferior to 5%. At last, the minimum squareness factor value of sintered permanent magnets has also been evaluated. Isotropic samples should show the smallest squareness factor due to the reduced degree of crystallographic alignment. In general, for this kind of sample, 0.20 SF 0.30

Ímãs híbridos aglomerados foram preparados por compactação uniaxial de pós magnéticos e curados ao ar e sob vácuo. Correlações entre tratamentos de cura, propriedades mecânicas e propriedades magnéticas foram estabelecidas com base em resultados obtidos por Histeresigrafia, Magnetometria de Amostra Vibrante, ensaios de Compressão e análises de Microscopia Óptica e Eletrônica de Varredura. Parâmetros como pressão de compactação, tempo e influência da temperatura e da atmosfera de cura nas propriedades mecânicas e magnéticas de ímãs aglomerados utilizados como padrão de referência, preparados com pós MQEP de NdFeB (partículas magnéticas impregnadas com resina epóxi), foram discutidos na primeira parte deste trabalho. A melhor condição de cura foi à temperatura de 200°C por cinco horas, sob vácuo. O produto de energia máximo (BHMáx) obtido para os ímãs padrão, curados ao ar e sob vácuo, foi de 76,2 KJ/m³ e 80,5 KJ/m³, respectivamente. Na segunda parte deste trabalho, ímãs híbridos foram produzidos a partir da mistura do pó MQEP aditivado com diferentes quantidades de pós de ferrite de estrôncio e NdFeB reprocessado por HDDR. O melhor resultado de BHMáx obtido para os ímãs híbridos de MQEP com ferrite de estrôncio e MQEP com pó reprocessado por HDDR, curados sob vácuo, foi de 73,2 KJ/m³ e 78,3 kJ/m³, respectivamente. Ímãs híbridos de MQEP com pó reprocessado por HDDR apresentaram melhor desempenho magnético que os ímãs híbridos de MQEP com pós de ferrite de estrôncio. / Bonded hybrid magnets were prepared by uniaxial pressing of magnetic powders cured in air and under vacuum. Correlations between cure treatments, mechanical properties and magnetic properties were established based on results obtained by Hysteresigraphy, Vibrating Sample Magnetometry, Compression tests, Optical Microscopy and Scanning Electron Microscopy. Parameters such as compaction pressure and the influence of time, temperature and atmosphere during the curing step in the mechanical and magnetic properties of the bonded magnets used as reference patterns, produced with NdFeB MQEP powder (epoxy encapsulated magnetic particles) were discussed in the first part of this work. The better cure condition was that performed at 200 oC for 5 hours under vacuum. The maximum energy product (BHMax) obtained for the patterns bonded magnets cured in air and under vacuum was 76.2 KJ/m³ and 80.5 KJ/m³, respectively. In the second part of this work, hybrid bonded magnets were produced by the mixture of MQEP powder with different amounts of strontium ferrite powder and NdFeB powder reprocessed by HDDR. The best results of BHMax obtained for the hybrid MQEP magnets with strontium ferrite powder and NdFeB reprocessed by HDDR, cured under vacuum were 73.2 KJ/m³ and 78.3 kJ/m³, respectively. Hybrid MQEP bonded magnets produced with the addition of HDDR reprocessed powder presented better magnetic performance than that obtained with strontium ferrite powders.

Neste trabalho, avaliou-se inicialmente a preparação de ímãs sinterizados de Pr16Fe76B8 (% at.) por meio de moagem de alta energia em moinho tipo planetário, averiguando-se os efeitos do tempo de moagem bem como da velocidade rotacional do moinho. Encontraram-se as melhores propriedades magnéticas para um magneto preparado com a matéria-prima cominuída durante 75 minutos e velocidade rotacional de 200rpm [JR = (1,02 ± 0,02) T, 0JHc = (1,42 ± 0,03) T e (BH)max = (200 ± 4) kJm-3]. De forma a melhorar a remanência, reduziu-se o tempo de exposição da liga ao hidrogênio, de 60 minutos para 2 minutos, obtendo-se um ímã com JR = (1,14 ± 0,02) T, 0JHc = (1,44 ± 0,03) T e (BH)max = (250 ± 5) kJm-3, constatando-se que a causa para a reduzida remanência no primeiro caso decorria do baixo grau de orientação cristalográfica. Durante esta investigação, desenvolveu-se e validou-se uma nova metodologia para quantificação do parâmetro . Posteriormente, propôs-se uma correlação quantitativa inédita entre a microestrutura e o fator de quadratura em magnetos anisotrópicos de TR16Fe76B8 (TR = Nd ou Pr) sinterizados. A expressão apresentada utiliza o tamanho, a elongação e a circularidade médios dos grãos e seus respectivos desvios padrões. Melhora-se o fator de quadratura quando a microestrutura apresenta grãos arredondados e com estreita distribuição de tamanho. A homogeneidade de tamanho dos grãos apresenta uma influência maior sobre o fator de quadratura quando comparada à homogeneidade de forma dos grãos. Ademais, verificou-se que o tratamento térmico após a sinterização melhora a ix homogeneidade de forma ao passo que a moagem melhora a homogeneidade de tamanho dos grãos. Avaliou-se, adicionalmente, o efeito da temperatura sobre o fator de quadratura em magnetos sinterizados anisotrópicos, verificando-se que o mesmo é controlado principalmente por sua microestrutura e confirmando a expressão previamente proposta. Além disso, propôs-se uma correlação quantitativa entre o produto de energia máximo e o fator de quadratura. Compararam-se valores experimentais e calculados, utilizando a expressão apresentada, e a discrepância encontrada foi de 5%. Por fim, avaliou-se qual seria o valor mínimo do fator de quadratura em ímãs sinterizados, constatando-se que magnetos isotrópicos devem apresentar o menor valor para tal parâmetro em virtude do reduzido grau de alinhamento cristalográfico. Ademais, verificou-se que para este tipo de amostra, em geral, 0,20 FQ 0,30. / In this work, it has firstly been evaluated the preparation of Pr16Fe76B8 sintered permanent magnets (% at.) by means of high-energy milling using a planetary ball mill. The influence of both milling speed and time has been verified. The best magnetic properties [JR = (1.02 ± 0.02) T, 0JHc = (1.42 ± 0.03) T and (BH)max = (200 ± 4) kJm-3] have been found for a permanent magnet prepared with the magnetic alloy milled during 75 minutes using a rotational milling speed of 200 rpm. In order to improve the remanence, the hydrogen decrepitation process time has been reduced from 60 minutes to 2 minutes. In this case, it has been obtained a sintered magnet with JR = (1.14 ± 0.02) T, 0JHc = (1.44 ± 0.03) T and (BH)max = (250 ± 5) kJm-3 due to the improvement of crystallographic alignment of the hard magnetic phase. During such investigation, a new methodology to quantify the parameter has been developed. Subsequently, for the first time, a quantitative correlation between the microstructure and the squareness factor in anisotropic sintered RE16Fe76B8 (RE = Nd or Pr) magnets has been proposed. The presented expression utilizes the mean size, the mean elongation and the mean roundness of the hard magnetic grains as well as their respective standard deviations. The squareness factor can be improved with a microstructure with rounder grains and with a sharp grain size distribution. The grain size homogeneity is more important to enhance the squareness factor compared to grain shape homogeneity. Furthermore, it has also been verified that the annealing after sintering improves the grain shape homogeneity and the milling enhances the xi grain size homogeneity. Moreover, the effect of the temperature on the squareness factor of anisotropic sintered magnets has also been evaluated. Such parameter is mainly controlled by the samples microstructure, in agreement with the proposed expression. Furthermore, a quantitative correlation between the maximum energy product and the squareness factor has been proposed. Experimental and calculated values have been compared and the discrepancy found has been, in general, inferior to 5%. At last, the minimum squareness factor value of sintered permanent magnets has also been evaluated. Isotropic samples should show the smallest squareness factor due to the reduced degree of crystallographic alignment. In general, for this kind of sample, 0.20 SF 0.30

ABSTRACT The design and fabrication of a rotating electromagnetic generator of low-speed and small bicycle were presented in this study. In accordance with the standard of generator the finite element analysis was used to design the prototype generator. In the simulation, the different parameters of the magnet, coil and iron yoke were set into the Taguchi method to find the best configuration. The parameters included the magnet poles, coil size, wire thickness, winding way, with or without iron yoke, and the distance between the magnet and yoke. When a permanent magnet is moved relative to a coil, an electromotive force is created. According to the theory of electromagnetic induction, the electricity was generated by the electromagnetic power generator. In this study, power produced by the relative motion between coil and magnet. This project innovatively uses Low-Temperature Co-fired Ceramic(LTCC) technology to fabricate micro-coil, and the required magnetic characteristics of permanent magnet are produced by sintered Nd-Fe-B. The technology and simulation were combined to achieve the requirements of lightweight, compact, high energy density. A prototype of the micro-generator is 50x50x4.5 mm3 in volume size. The 28 poles hard magnet Nd/Fe/B with an outer diameter of 50 mm and a thickness of 2 mm was molded and sintered, and provides the magnetic field of 3.5 Tesla. The coils with a width of 200£gm, a pitch 100£gm and the thickness of 40£gm were fabricated by silver. The coils had 30 layers and 22 poles. A steel yoke can improve the efficiency of power generation. The results of induced electromotive force were 0.61, 0.97 and 1.45V at the rotational speeds of 37rpm, 74rpm and 111rpm respectively in the simulation.

Neste estudo, as propriedades magnéticas dos ímãs sinterizados, produzidos a partir de uma mistura de ligas Pr16Fe76B8 e Pr14FebalCo16B6Nb0,1Mx, onde M= Al, Cu, P, Si, Gd, Ga, Dy, Tb e x= 0,1, 0,3, 0,5 % at. em iguais proporções, foram correlacionadas com as características microestruturais através de microscopia eletrônica de varredura (MEV) e de transmissão (MET). Utilizou-se microscopia eletrônica de varredura (MEV) e processamento computacional das micrografias, na investigação das características associadas ao tamanho e formato dos grãos magnéticos (Φ). A correlação utilizada indicou que fatores de quadratura superiores estão associados a grãos mais arredondados e com distribuição de tamanho mais estreita. Considerando que a variação no tamanho de grão e os valores de coercividade não se mostraram conclusivas com MEV, utilizou-se o recurso da microscopia eletrônica de transmissão (MET), microanálise com EDS e padrão de difração eletrônica. A associação da coercividade com a microestrutura foi feita com base nas investigações das fases não magnéticas, ricas em praseodímio dos pontos triplos e nos contornos de grãos. Com o microscópio de transmissão de alta resolução (HRTEM), foi possível observar a presença de uma camada contínua e regular entre os grãos da fase magnética para o ímã com adição de Ga 0,25% at. A modificação da microestrutura no contorno de grão do ímã com adição de Ga pode ser indicada como responsável pelo aumento de 10% na coercividade (1100 mT) comparado com o ímã Pr15FebalCo8B7Nb0,05. / In this study the magnetic properties of sintered magnets, prepared with a mixture of Pr16Fe76B8 and Pr14FebalCo16B6Nb0.1Mx alloys, where M = Al, Cu, P, Si, Gd, Ga, Dy, Tb and x = 0.1, 0.3, 0.5 at.% in the same proportions, were correlated with the microstructural features by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM and computer processing of the micrographs were used in order to provide the characteristics associated with the size and shape of the magnetic grains (Φ phase). The correlation used shows that superior squareness factors are associated with rounder and narrower size distribution grains. Considering that the variation in the grain size and coercivity values were not conclusive with SEM, it has been used TEM, micro analysis by EDS and electron diffraction pattern. The coercivity relation with the microstructure was based on investigations of non-magnetic phases, in triple points, and in the grain boundary. With a high resolution transmission microscope (HRTEM), it was possible to observe a regular and continuous layer between the grains of the magnetic phase for the magnet with 0.25 at.% of Ga. The presence of such boundary can be indicated as responsible for higher coercivity values of this magnet. Microstructure was modified in the grain boundary by Ga addition and can be indicated as responsible for coercivity value (1100 mT) 10% higher than Pr15FebalCo8B7Nb0.05 magnet.

Neste estudo, as propriedades magnéticas dos ímãs sinterizados, produzidos a partir de uma mistura de ligas Pr16Fe76B8 e Pr14FebalCo16B6Nb0,1Mx, onde M= Al, Cu, P, Si, Gd, Ga, Dy, Tb e x= 0,1, 0,3, 0,5 % at. em iguais proporções, foram correlacionadas com as características microestruturais através de microscopia eletrônica de varredura (MEV) e de transmissão (MET). Utilizou-se microscopia eletrônica de varredura (MEV) e processamento computacional das micrografias, na investigação das características associadas ao tamanho e formato dos grãos magnéticos (Φ). A correlação utilizada indicou que fatores de quadratura superiores estão associados a grãos mais arredondados e com distribuição de tamanho mais estreita. Considerando que a variação no tamanho de grão e os valores de coercividade não se mostraram conclusivas com MEV, utilizou-se o recurso da microscopia eletrônica de transmissão (MET), microanálise com EDS e padrão de difração eletrônica. A associação da coercividade com a microestrutura foi feita com base nas investigações das fases não magnéticas, ricas em praseodímio dos pontos triplos e nos contornos de grãos. Com o microscópio de transmissão de alta resolução (HRTEM), foi possível observar a presença de uma camada contínua e regular entre os grãos da fase magnética para o ímã com adição de Ga 0,25% at. A modificação da microestrutura no contorno de grão do ímã com adição de Ga pode ser indicada como responsável pelo aumento de 10% na coercividade (1100 mT) comparado com o ímã Pr15FebalCo8B7Nb0,05. / In this study the magnetic properties of sintered magnets, prepared with a mixture of Pr16Fe76B8 and Pr14FebalCo16B6Nb0.1Mx alloys, where M = Al, Cu, P, Si, Gd, Ga, Dy, Tb and x = 0.1, 0.3, 0.5 at.% in the same proportions, were correlated with the microstructural features by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM and computer processing of the micrographs were used in order to provide the characteristics associated with the size and shape of the magnetic grains (Φ phase). The correlation used shows that superior squareness factors are associated with rounder and narrower size distribution grains. Considering that the variation in the grain size and coercivity values were not conclusive with SEM, it has been used TEM, micro analysis by EDS and electron diffraction pattern. The coercivity relation with the microstructure was based on investigations of non-magnetic phases, in triple points, and in the grain boundary. With a high resolution transmission microscope (HRTEM), it was possible to observe a regular and continuous layer between the grains of the magnetic phase for the magnet with 0.25 at.% of Ga. The presence of such boundary can be indicated as responsible for higher coercivity values of this magnet. Microstructure was modified in the grain boundary by Ga addition and can be indicated as responsible for coercivity value (1100 mT) 10% higher than Pr15FebalCo8B7Nb0.05 magnet.

In dieser Arbeit wurde der Einfluss der Schmelzkonvektion auf das erstarrende Gefüge von peritektischen Nd-Fe-B – und TiAl-Legierungen mit Hilfe neuartiger Methoden untersucht. Da die magnetischen und mechanischen Eigenschaften dieser technisch relevanten Legierungen stark vom Gefüge und insbesondere vom Volumenanteil der properitektischen Phase abhängen, sind diese Untersuchungen von großem Interesse. Auf der Basis der numerischen Simulationen der Schmelzkonvektionsmoden und des elektromagnetischen Problems in einer induktiv beheizten Schmelze, die am Forschungszentrum Dresden-Rossendorf durchgeführt wurden, wurden am IFW Dresden neuartige Versuchsaufbauten entwickelt, die die Modifizierung der Konvektion in einer Metallschmelze ermöglichen. Dies sind ein Aufbau zur erzwungenen Schmelzrotation in einem Tiegel und eine modifizierte Floating-Zone-Anlage. Die erzwungene Schmelzrotation, bei der der Schmelztiegel mit einer definierten Frequenz rotiert, führt in Übereinstimmung mit der Simulation zu einer starken Reduzierung der Konvektion in Abhängigkeit von der Frequenz. Diese Methode wurde auf Nd-Fe-B-Legierungen angewendet mit dem Ziel, die Bildung der unerwünschten weichmagnetischen Eisenphase zu unterdrücken bzw. deren Volumenanteil zu reduzieren. Im Ergebnis konnte der Volumenanteil der properitektischen Phase mit diesem Verfahren um 38.5 % reduziert werden. Das dendritische Gefüge wurde einer ausführlichen statistischen Analyse unterzogen, bei der die Abstände der sekundären Dendritenarme (SDAS) gemessen wurden. Es konnte gezeigt werden, dass die SDAS sich mit steigender Frequenz der Tiegelrotation, was einer reduzierten Schmelzkonvektion entspricht, verringern. Die Verringerung des Volumenanteils der properitektischen Eisenphase und der SDAS wird mit dem reduzierten konvektiven Massentransport unter reduzierter Schmelzkonvektion erklärt. Starke interdendritische Strömung reduziert die Dicke der Diffusionsgrenzschicht um die properitektische Phase. Dadurch wird der Stofftransport durch die Grenzschicht erleichtert. Kleinere Dendritenarme werden in die Schmelze zurückgeschmolzen, wodurch sich der Abstand zwischen den verbleibenden Dendritenarmen vergrößert. Eine Floating-Zone-Anlage, die das tiegelfreie Prozessieren von Metallschmelzen erlaubt wurde so modifiziert, dass mit Hilfe eines Doppelspulensystems eine zusätzliche wohl definierte elektromagnetische Kraft eingebracht wird, über die eine sehr intensive (Zweiphasenrührer in Parallelschaltung) bzw. stark verringerte Strömung (Doppelspule in Reihenschaltung) in der Schmelze eingestellt werden kann. Die experimentellen Ergebnisse der Untersuchungen am Nd-Fe-B-System mit der Doppelspule in Reihenschaltung zeigten, dass sich bei einem optimalen Spulenabstand von 5,1 mm die geringste Schmelzkonvektion ergab, wobei der Anteil des a-Eisen-Volumenanteils weiter verringert werden konnte. Im Gegensatz dazu wurde mit dem Zweiphasenrührer in Parallelschaltung eine sehr starke Schmelzkonvektion mit einem maximalen Volumenanteil der a-Eisen-Phase eingestellt, wobei durch die starke Rührung ein Wechsel der Morphologie von dendritisch zu globular zu beobachten war. Die Untersuchungen zum Einfluss der starken Schmelzkonvektion wurden auf ein weiteres peritektisch erstarrendes System ausgedehnt, um eine generalisierte Aussage zum Einfluss der Konvektion auf Gefüge und Eigenschaften peritektisch erstarrender Legierungen zu erhalten. Die ausgewählte Ti45Al55 - Legierung erstarrte unter starker Schmelzkonvektion ebenfalls globulitisch, wobei Reste dendritisch erstarrter properitektischer Phase gefunden wurden. Der Volumenanteil der properitektischen Phase steigt dabei mit zunehmender Rührwirkung an. Der Wechsel der Morphologie von dendritisch zu globular/dendritisch kann mit sphärischem Wachstum oder Fragmentierung der Dendritenarme erklärt werden. Die mechanischen Eigenschaften unter unterschiedlicher Schmelzkonvektion erstarrter Ti45Al55 – Legierung wurden bei Druckversuchen untersucht. Es wurde eine signifikant höhere plastische Verformbarkeit an der unter starker Schmelzkonvektion erstarrten Ti45Al55 – Legierung gefunden. Dies wird der isotropen spherischen Morphologie der lamellaren a2/g-Phase zugeordnet, während die anisotrope Orientierung der dendritisch- lamellaren Phase unerwünschte plastische Eigenschaften zeigt. Die Untersuchungen des Einflusses der Schmelzkonvektion auf das Gefüge peritektisch erstarrender Legierungen zeigten, dass ein maßgeschneidertes Gefüge durch optimale Wahl der Schmelzkonvektion möglich ist und damit magnetische bzw. mechanische Eigenschaften verbessert werden können. Die Kontrolle der Schmelzkonvektion ist daher ein geeignetes Mittel gewünschte Gefüge und Eigenschaften in Abhängigkeit von den Prozessabläufen einzustellen. / In this work, the effect of melt convection on the microstructure evolution of peritectic Nd-Fe-B and Ti-Al alloy systems was studied using novel techniques. The microstructural formation including the change in volume fraction and morphology of the properitectic phase influences the magnetic and mechanical properties for the Nd-Fe-B and Ti-Al alloy systems, respectively. On the basis of numerical simulations by the research group of Dr. Gunter Gerbeth from Department of Magnetohydrodynamics, Forschungszentrum Dresden-Rossendorf, two types of specially designed facilities were developed where melt convection can be altered by changing a number of parameters. These are: forced rotation facility and modified floating zone facility. According to the numerical simulation, an additional crucible rotation suppresses the internal melt motion significantly during forced rotation experiments, where the molten alloy is rotated at a well-defined frequency. This method was applied during the solidification of Nd-Fe-B alloys with the aim to suppress the volume fraction of undesired soft magnetic a-Fe phase. As a result, the volume fraction of properitectic phase with this method can be reduced up to 38 %. A detailed statistical analysis of secondary dendritic arm spacing (SDAS) measurements of a-Fe showed that the SDAS decreases as the rotational frequency increases and melt convection decreases. The reduction in the phase fraction and SDAS of properitectic phase is attributed to the reduced convective mass transfer under reduced melt motion. At high fluid velocity and low rotational frequency, the stronger interdendritic flow reduces the solute boundary layer and increases the transfer of solute through the interface. The smaller dendrite arms dissolve into the melt and thus the SDAS becomes higher than that of the samples solidified at higher rotational frequencies with reduced melt convection. Floating zone facility, which allows contactless heating without any contamination for highly reactive melts, was modified with a double coil system so that an additional electromagnetic force is introduced inside the melt. This induces either very intensive (two-phase stirrer in parallel connection coil system) or very reduced flow (series connection coil system) inside the melt The experimental results of series connection coil system showed that a reduced melt convection state is achieved near 5.1 mm coil distance where a-Fe volume fraction becomes minimum. On the contrary, the parallel coil system experiments showed that a-Fe volume fraction becomes maximum when the phase shift between the coils is close to 90°. The morphology of the a-Fe becomes globular due to spherical growth under strong convection. The study on the effect of strong stirring was extended to another alloy to get a generalized idea about the influence of melt convection on the microstructure development and resulting properties of peritectic alloys. Peritectic Ti45Al55 alloys were investigated by the two-phase stirrer using the coils connected in parallel to study the effect of enhanced melt convection. The increase in the properitectic phase fraction together with a strong change in the morphology from dendritic to spherical were observed in the stirred samples. The increase in the properitectic phase fraction occurs due to the enhanced effective mass transfer under strong melt convection. The change in morphology of the properitectic phase is attributed to spherical growth or fragmentation of dendrite arms under strong convection. The mechanical properties of Ti45Al55 alloys, which are solidified at different convection states, were studied. There was a significantly higher plastic deformability of stirred samples compared to unstirred samples. The coarse anisotropic orientation of the dendritic lamellar phase is detrimental for the plastic deformability, which is absent in the stirred samples due to the spherical and discrete morphology of the properitectic phase. This study indicates that tailored microstructure can be obtained either by decreasing (e.g. for Nd-Fe-B alloy) or increasing (e.g. for Ti-Al alloy) the convection state using effective techniques inside the melt to improve the magnetic and mechanical properties, respectively. Thus, controlling convection is a useful way to get favorable microstructure according to the process need.

Les aimants NdFeB sont les aimants les plus puissants que l’on peut trouver actuellement sur le marché. Leurs propriétés exceptionnelles proviennent des propriétés intrinsèques de la phase Nd2Fe14B mais également de la microstructure imposée par le mode d’élaboration. Ces aimants sont généralement réalisés par frittage avec phase liquide à partir d’une poudre monocristalline préalablement orientée sous champ magnétique. Cette voie permet d’obtenir une microstructure à grains fin découplés magnétiquement les uns des autres par une fine couche de phase riche en néodyme, dont la distribution est optimisée après un recuit à une température donnée. Pour une utilisation dans des moteurs et générateur électriques, il est courant d’ajouter du dysprosium pour conserver une coercitivité suffisante à la température de fonctionnement. Mais ce gain de coercitivité se fait au détriment de l’induction rémanente et du coût de l’aimant de par la rareté du dysprosium. Il est donc nécessaire de pouvoir s’affranchir de son utilisation par une meilleure compréhension des liens entre le procédé d’élaboration et la microstructure du matériau, afin d’optimiser les propriétés magnétiques finales.Cette thèse s’intéresse tout d’abord au frittage d’aimants NdFeB pour une nuance du commerce et donc fortement alliée. La forte anisotropie de retrait lors de la densification n’est pas clairement expliquée dans la littérature et son interprétation peut apporter un éclairage sur les propriétés magnétiques. Le frittage a ainsi été étudié à l’aide d’essais de dilatométrie dans la direction d’orientation de la poudre ainsi que dans la direction transverse. Le frittage a également été interrompu à différents moments et la microstructure analysée. Des analyses d’images ont permis de comprendre, à l’aide d’un modèle analytique du frittage, qu’une partie de l’anisotropie de retrait s’expliquait par une distribution anisotrope des surfaces de contact entre les grains de poudre, issue de l’étape d’orientation sous champ. Cette analyse a été confirmée par des simulations par éléments discrets.Le deuxième volet de la thèse s’intéresse au rôle des éléments d’alliage les plus couramment rencontrés dans les aimants hors dysprosium. Le rôle de l’aluminium, du cobalt et du cuivre sur les propriétés magnétiques a été examiné en étudiant une vingtaine de compositions simplifiées avec des quantités d’éléments d’alliage voisines des valeurs que l’on retrouve dans les aimants du commerce. Les différents échantillons ont été recuits à des températures déduites d’essais DSC. Les résultats montrent que ces trois éléments d’alliage agissent de manière croisée sur la coercitivité. Au-delà de la mesure de coercitivité, l’évolution de la forme de la courbe de désaimantation en fonction de la composition et de la température de recuit apporte des informations importantes sur l’action des éléments d’alliage sur la microstructure. / NdFeB hard magnets are the most powerful magnets commercially available. Their outstanding properties originate from Nd2Fe14B intrinsic properties and from the microstructure imposed by the manufacturing process. These magnets are generally obtained by liquid phase sintering of an oriented monocrystalline powder which enables a microstructure made of grain magnetically decoupled by a thin neodymium-rich layer which is optimally distributed in the magnet after a low temperature annealing. For them to be used in electrical engines and generators, dysprosium is usually added so that the coercivity is high enough at the working temperature. But dysprosium is rare and expensive and lowers the remnant induction. It is therefore important to get free of its usage by a better understanding of the links between the manufacturing process and the microstructure, so that the final magnetic properties can be optimized.First, this thesis deals with NdFeB sintering on an alloyed commercial grade. The high shrinkage anisotropy during densification is not clearly explained and its interpretation could bring information on the magnetic properties. Dilatometric studies have been performed along orientation direction as well as along the transverse direction. Sintering has been interrupted at different times and the microstructure was observed. Image analysis has enabled to understand, thanks to an analytical model, that a part of the anisotropy could be explained by an anisotropic contact orientation distribution, originating from the magnetic orientation step. Discrete element modelling has confirmed this approach.The second part of the thesis deals with the role of the most commonly used alloying elements on the magnetic properties: aluminum, cobalt and copper. Around twenty different model grades were examined with composition close to the ones of commercial magnets. After having been sintered, the samples were annealed at temperatures deduced from DSC measurements. Results show that the three elements have cross effects on coercivity. Beyond coercivity, demagnetizing curve shape is sensitive to the composition and annealing temperature and gives important information on the role of the alloying elements on the microstructure.

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.