Orientador: Célia Marina de Alvarenga Freire / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-22T11:43:34Z (GMT). No. of bitstreams: 1 Costa_GiselleBarata_D.pdf: 6195639 bytes, checksum: 7b424607db5a3372771d157f6bac717c (MD5) Previous issue date: 2013 / Resumo: O hidrogênio é reconhecido como sendo um elemento residual sempre prejudicial ao aço. Proveniente de reações químicas e eletroquímicas, tais como, corrosão, proteção catódica e reações de processo, é absorvido pelo aço e retido nos defeitos da rede cristalina podendo causar a fragilização do aço e a propagação de trincas e fraturas. O presente trabalho visa analisar a influência do hidrogênio na estrutura cristalina e no comportamento magnético do aço AISI 4340 obtido pelas normas AMS 6414K e 6415S, nas condições como recebido, temperado e revenido. Para tanto corpos-de-prova foram retirados da posição transversal dos lingotes, temperados a 845°C e revenidos a três diferentes temperaturas (350°C, 400°C e 500°C). Para a caracterização do material foram feitas micrografias, ensaios de dureza, difração de raios-X, voltametria cíclica e análise de difusão. As propriedades magnéticas foram obtidas utilizando-se um magnetômetro de amostra vibrante (VSM) onde a magnetização de saturação foi obtida e foram analisadas amostras antes da hidrogenação e após hidrogenação. O carregamento de hidrogênio foi feito em solução de H2SO4 a 0,05 M em temperatura ambiente. Os resultados obtidos nos ensaios de voltametria cíclica e difusão foram correlacionados às difrações de raios-x e magnetização de saturação em função da contaminação por hidrogênio e as diferentes condições de tratamento térmico. A comparação das curvas antes e após hidrogenação para as difrações de raios-X mostraram que a hidrogenação provoca uma diminuição das curvas em todas as condições de tratamento térmico para os dois tipos de aço. As curvas de difusão mostraram que os coeficientes de difusão da amostra como recebida é menor que as tratadas com revenimento para o aço AISI 4340 AMS 6415S e maior para o aço AISI6414K. A magnetização de saturação mostrou que os aços AISI 6414K e 6415S antes da hidrogenação apresentaram magnetização de saturação maior que após hidrogenação / Abstract: Hydrogen is recognized as a residual element always harmful to steel. From chemical and electrochemical reactions, such as corrosion, cathodic protection and reaction process, the steel is absorbed and retained in the crystal lattice defects may cause embrittlement of steel and propagation of cracks and fractures. This study aims to analyze the influence of hydrogen in the crystal structure and magnetic behavior of AISI 4340 obtained by the rules AMS 6414K 6415S and the conditions as received, quenched and tempered. For this purpose the test piece bodies were removed from the transverse position of the ingots, quenched to 845 ° C and tempered at three different temperatures (350 ° C, 400 ° C and 500 ° C). For the characterization of the micrographs were taken, hardness tests, X-ray diffraction, cyclic voltammetry analysis and dissemination. The magnetic properties were obtained using a vibrating sample magnetometer (VSM), where the saturation magnetization was obtained and analyzed samples before hydrogenation and after hydrogenation. The hydrogen loading was done in a solution of 0.05M H2SO4 at room temperature. The results obtained in the test and cyclic voltammetry were correlated to diffusion x-ray diffraction and saturation magnetization due to hydrogen contamination and different heat treatment conditions. A comparison of the curves before and after hydrogenation for X-ray diffraction showed that the hydrogenation causes a decrease of the curves in all heat treatment conditions for both types of steel. The curves show that the diffusion coefficient of diffusion of the sample as received is lower than those treated with tempering for the steel AISI 6415S AMS 4340 steel and higher for AISI6414K. The saturation magnetization showed that AISI 6415S 6414K and exhibited before the hydrogenation higher than saturation magnetization after hydrogenation / Doutorado / Materiais e Processos de Fabricação / Doutora em Engenharia Mecânica

Les travaux présentés dans ce document s’inscrivent dans un projet (dBET : diminution des Bruits Electriques de Trains) qui vise une meilleure compréhension des phénomènes vibratoires (indirectement le bruit) d’origine électromagnétique des dispositifs électrotechniques (transformateurs, inductances, moteurs électriques) des trains. Ce projet met en collaboration plusieurs laboratoires (le laboratoire Roberval et électromécanique de l’université de technologie de Compiègne...) et industriels parmi lesquels Alstom Transport, ESI Group… Notre contribution, dans ce projet, consiste en la proposition d’un modèle pertinent permettant de prédire la déformation magnétostrictive, considérée comme l’une des causes des bruits d’origine électromagnétique des dispositifs électrotechniques. Un processus d’identification des paramètres du modèle, à partir de données expérimentales, est présenté ainsi que l’application du modèle à un dispositif expérimental grâce à l’utilisation des éléments finis. Les résultats du modèle seront confrontés aux mesures faites à l’échelle d’une tôle ferromagnétique et d’un dispositif expérimental constitué d’un ensemble de tôles. / The work presented in this document is part of a project (dBET : diminution des Bruits Electriques de Trains) which aims a better understanding of electromagnetic-origin vibration phenomena (indirectly noise) from electrical devices (transformers, inductors, motors) in trains. This project results from the collaboration of several laboratories and companies including Alstom, ESI Group.... Our contribution in this project consists in building a relevant model to predict the magnetostrictive strain, considered as one of the causes of electromagnetic-origin noise of electrical devices. A process of identification of the model parameters from experimental data is presented. The model is used to compute the magnetostrictive strain of a test bench thanks to finite elements method. Model results will be compared with measurements about ferromagnetic single sheet and the test bench which is a stack of ferromagnetic sheets.

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Válvulas de Spin têm sido utilizadas na fabricação de sensores magnéticos e memórias de acesso randômico, sendo muito importantes do ponto de vista tecnológico. Neste trabalho, foram exploradas as análises das curvas de reversão de primeira ordem da magnetorresistência (MR-FORC), bem como ajustes das curvas de histereses da magnetização e magnetorresistência, para estudar o fenômeno de exchange-bias, anisotropia magnética e propriedades magnetorresistivas. As válvulas de spin estudadas foram do tipo NiFe/Cu/NiFe/IrMn, tendo camadas semente e de cobertura de Ta, preparadas por sputtering. Um modelo fenomenológico de parede de domínios no material antiferromagnético (AFM) foi utilizado, levando em conta as anisotropias magnéticas e interações entre as camadas. Também foram consideradas certas dispersões da anisotropia dos grãos ferromagnéticos (FM) e antiferromagnéticos (com distribuições Gaussianas) em torno dos respectivos eixos de anisotropia uniaxiais. Para o ajuste da magnetização para algumas amostras, foi necessário utilizar uma rotação no plano de um ângulo nos eixos de anisotropia uniaxiais do FM e AFM, em relação à direção do campo magnético aplicado durante a deposição dos filmes. Bons ajustes das curvas de histereses das magnetizações foram obtidos nas direções medidas do campo magnético aplicado. Um método baseado em medidas de variações angulares da magnetorresistência em campos constantes foi proposto para extrair este ângulo para cada amostra. Foram obtidas razoáveis concordâncias entre estes ângulos e os correspondentes extraídos dos ajustes das curvas de magnetização. Através da análise dos diagramas da MR-FORC e de simulações indicados dos resultados dos ajustes das histereses da magnetização, foi encontrada uma relação direta entre os campos de interação (e suas incertezas) com os campos de exchange-bias (HEB) dos grãos da distribuição (extraídos das simulações, usando a largura da distribuição obtida do ajuste). Resumindo, esta análise mostrou que esta técnica permite extrair informações comparativas sobre a dispersão dos eixos de anisotropia dos grãos FM e AFM em torno do eixo de anisotropia uniaxial, o que pode ser importante na caracterização dos sensores magnetorresistivos. Além disso, análise dos diagramas MR-FORC indicaram início da presença de descontinuidade na camada de NiFe presa em 27, com um aumento acentuado (acima do previsto) para a amostra com 25. Este aumento acima do previsto corrobora com nossa hipótese. As simulações das curvas de histerese da magnetorresistência não foram muito bons, indicando que melhorias devem ser introduzidas no modelo utilizado para a simulação da histerese da magnetorresistência, obtidos a partir dos ângulos das camadas ferromagnéticas livre e presa. A questão referente a presença em algumas das amostras de um desalinhamento entre os eixos fácéis do FM e do AFM ainda é uma questão em aberta, mas neste trabalho foi encontrado que este ângulo é igual a 2. / Spin Valves have been employed as magnetic sensors and used in random access memories, showing they are very important in terms of technological point of view. In this work, analyses of the magnetoresistance first order reversal curves (MR-FORC) have been used, as well as fittings of the magnetization and magnetoresistance hysteresis, to study the exchange-bias phenomena, magnetic anisotropies and magnetoresistance in spin valves. Sputtering has been used to the deposition of NiFe/Cu/NiFe/IrMn, and Ta has been deposited as seed and buffer layers. A domain wall model (in the antiferromagnetic layer) taking into account the magnetic anisotropies and the interactions between the layers has been employed to fit the magnetization hysteresis. Some textures have been also introduced to take into account the ferromagnetic (FM) and antiferromagnetic (AFM) grains dispersion (with Gaussian distributions) centered around the respective uniaxial anisotropy axes. However, to obtain good fits for some samples, it has been necessary to include an in-plane rotation of an angle of the both FM and AFM easy axes in relation to the field direction applied during the growing of the films. Good fits of the magnetization hysteresis have been obtained for all measured directions of the applied field. A new method based on the angular variation of the magnetoresistance to constant fields has been proposed to extract directly these angles. Reasonable agreements have been obtained between these angles and the corresponding ones extracted from the fits of the magnetization loops. Through the analyses of the MR-FORC and from the simulations indicated by the parameters (obtained from the fittings of magnetization loops), a direct relation between the interaction fields (and its uncertainties) and the exchange-bias fields of the grains of the distribution (extracted from the simulations, using the width of the distribution obtained from the magnetization fittings) has been identified. In summary, this analysis has showed that this technique allows to extract comparative information about the dispersion of the anisotropy axes of the FM and AFM grains around the uniaxial axis, which can be very import to the characterization of spin-valve based sensors. Besides, MR-FORC analyses have also indicated the presence of a threshold of discontinuity of the pinned NiFe layer at 27, showing a huge increase (above of the expected) to the sample at 25, and this unexpected increasing has corroborated with our hypothese. Simulations of the magnetoresistance loops have not been good, indicating that improvements should be included in the model employed to simulate these curves, obtained from the pinned and free angles of the NiFe layers. Concerning the case of the presence of misalignments of FM and AFM for some samples, it is still an open question, but in this work, we have found that this angle () is equal to 2.

On utilise en IRM clinique T2, T1 et la densité de protons comme biomarqueurs de diagnostic et de suivi. Cependant, seuls les tissus à T2 long sont visibles par IRM classique. La séquence UTE (Ultra-short TE) a été récemment développée pour des études quantitatives de l’os cortical. Nous avons dans une première étape confronté des mesures de porosité de l’os cortical par IRM-UTE et par microtomographie par rayonnement synchrotron, car la porosité est un paramètre déterminant de la qualité osseuse. L’étude a été menée sur 38 échantillons de diaphyses fémorales humaines en collaboration avec une équipe du B2OA (UMR7052). La porosité par IRM-UTE à 4.7 T (TE = 51 µs) est entre 18 et 43% (moyenne 30%). La porosité par microtomographie (résolution spatiale : 6.5 µm) est entre 3 et 27% (moyenne 14%). Aucune corrélation n’a pu être observée entre les deux mesures. Une importante dispersion a été observée sur les valeurs de T1 entre les échantillons, que nous proposons d’attribuer à des effets de transfert d’aimantation (MT) entre les protons de l’eau liée au collagène et les protons des terminaisons méthylène du collagène. Pour confirmer cette interprétation, nous avons dans une seconde étape confronté plusieurs méthodes d’évaluation de la relaxation longitudinale dans des échantillons d’os bovin. Les mesures réalisées par différentes séquences (inversion-récupération, saturation hors-résonance, saturation par répétition de binomiales et angle de bascule variable) confirment des effets de MT importants. Les méthodes les plus robustes pour évaluer les paramètres sont la saturation hors-résonance et par répétition de binomiales, ce qui suggère leur utilisation pour de futures applications in vivo. / Longitudinal and transverse relaxations are quantitative tools used in MRI for diagnosis and follow up. However only tissues with long T2 can be detected with MRI. Quantitative evaluation of cortical bone porosity is now feasible with UTE.In this work, porosity measurements from UTE in human cortical bone samples were compared with those from micro-computed tomography (µCT). 38 human cortical bone samples (upper diaphysis) were examined in collaboration with a team from B2OA (UMR7052). Porosity from UTE (TE = 51 µs) was between 18% and 43% (mean 30%) and from µCT (spatial resolution = 6.5 µm) between 3% and 27% (mean 14%). No correlation could be established between the two measurements. T1 values from few samples were dispersed; a possible explanation could be the magnetization transfer (MT) between collagen-bound water protons and collagen methylene protons.For a quantitative interpretation of this phenomenon, 11 bovine cortical bone samples were examined. Several sequences (inversion-recovery, off-resonance saturation, repeated binomial excitations, variable flip angle) were implemented at 4.7 T to assess MT parameters. The aim was to compare which method may provide accurate parameter estimation. Off-resonance saturation and repeated binomial excitation seem to be more suitable for in vivo MT quantification.

In the thesis at hand, different concepts of magnetic recording were investigated both from an experimental and theoretical point of view. On the one hand, micromagnetic simulations of bit patterned media were performed examining the influence of magnetic and geometrical parameters on the magnetization reversal mechanism of the bit array. In this regard, the recording concept called exchange coupled composite (ECC) media was applied in combination with bit patterned media (BPM). It was demonstrated that ECC/BPM is superior in terms of narrowing the SFD which is vital for the implementation of BPM as a recording scheme in magnetic data storage deviced. Moreover, the stability of the magnetic state was calculated for single nanomagnets using the nudged elastic band algorithm. It was found out that the magnetic and geometrical properties have a severe influence on both, the energy barrier for magnetization reversal and the magnetization reversal process of the single nanomagnets. On the other hand, experimental studies of granular CoCrPt:SiO2 films deposited on self-assembled arrays of SiO2 nanoparticles with a size from 10 nm to 330 nm have been carried out, showing a distinct size-dependence of the coercive field and remanent magnetization with changing nanoparticle size. Moreover, these films have been irradiated with Co+ ions with different fluences, resulting in a change of the magnetic properties of the films due to both a change of the intergranular exchange coupling of the film and a degredation of the magnetic layers at higher irradiation fluences.

Title: The magnetocrystalline anizotropy in the TbTX compounds Author: Milan Klicpera Department: Department of Condensed Matter Physics Supervisor: doc. Mgr. Pavel Javorský, Dr. Supervisor's e-mail address: javor@mag.mff.cuni.cz Abstract: The subject of this work is the study of structural, magnetic and trans- port properties of the TbNi(Al,In) series to finding connections between magne- tocrystalline anisotropy and lattice parameters of the structure of the TbTX com- pounds. Polycrystalline TbNiAl1−xInx samples were prepared by melting. The phase and crystal structure analysis were provided on samples. We performed the measurements of the magnetization, susceptibility, specific heat, resistivity, low temperature X-ray diffraction and powder neutron diffraction. From the neutron diffraction data we refined lattice parameters and propagation vectors of the series. The main propagation is (000) and second weaker component has the propagation vector (1 2 0 1 2 ). The change of the magnetocrystalline anisotropy from uniaxial to planar type occurs for compounds with x between 0.4 and 0.5. Keywords: magnetization, X-ray and neutron diffraction, electrical resistivity.

Masters of Science / Rare-earth (RE) compounds have been an attractive subject, based on the unique electronic structures of the rare-earth elements. In particular, the RETX (RE = rare-earth, T = 3d/4d/5d, transition metals, and X = p – block elements) series is a large family of intermetallic compounds which crystallizes in different crystal structure depending on the constituents. Most of these compounds crystalize in the hexagonal, orthorhombic, and tetragonal crystal structure. On the other hand, the family of compounds RET2X2 adopted the tetragonal crystal structure of the ThCr2Si2 or the CaBe2Be2 with different space groups. Owing to the different crystal structure, these compounds show versatile magnetic and electrical properties such as Kondo effect, complex magnetic behaviour, valence fluctuation, unconventional and conventional superconductivity, heavy fermion behaviour, Fermi and non – Fermi liquid behaviour, metamagnetism, spin – glass, memory effect, crystal electric field (CEF), magnetoresistance and magnetocaloric effect. The history of magnetism reveals that it is closely related to practical applications and magnetic materials from the most vital components in many applications. These are memory devices, permanent magnets, transformer cores, magneto-mechanical devices and magneto-electronic devices. Recent additions to this list include magnetic refrigeration through the studies of magnetocaloric effect as well as spintronics. Magnetic refrigeration (MR) is an emerging technology and shows real potential to enter conventional markets and the principles of MR obeys the magnetocaloric effect (MCE), which is based on the effect caused by a magnetic field on the materials that accept the property of varying the magnetic entropy, as well as its temperature when varying the magnetic field. In this thesis, we report giant magnetocaloric effect and magnetic properties of NdPd2Al2 and RECuGa (RE = Nd, Dy, and Ho) compounds. These investigations were done through measurements of X – ray diffraction (XRD), magnetic susceptibility, ((T)), magnetization, (M(H)), isothermal magnetization, (M(H, T)), heat capacity, (Cp(T)) and electrical resistivity, ((T)). MCE has been studied from the isothermal magnetization and heat capacity measurements.The first chapter of the thesis describes the theoretical background from which the experimental results have been analyzed and interpreted. This is followed by the chapter which presents experimental details and methodology carried out in this thesis. Chapter three presents the results and discussion of the transport, magnetic and magnetocaloric properties of NdPd2Al2 compounds. XRD studies confirm the tetragonal CaBe2Ge2 – type structure with space group P4/nmm (No. 129). The results of (T), (T) and Cp(T) indicate a putative antiferromagnetic (AFM) phase transition at low temperature at, TN = 3 K. On the other hand, (T) data at high temperatures follow the Curie – Weiss relationship giving an effective magnetic moment close to that expected for the trivalent Nd3+ ion. The magnetization results indicate metamagnetic – like transition at a low field that bears a first-order character which corroborates with the Below – Arrott plots. Giant MCE was obtained for the NdPd2Al2 compound similar to those reported for potential magnetic refrigerant materials. Chapter four discusses the magnetic and thermodynamic properties of the series of compounds RECuGa where RE = Nd, Dy, and Ho. XRD studies indicate the orthorhombic CeCu2 – type crystal structure with space group Imma (No. 74) for all three compounds. Magnetic measurements indicate a putative AFM phase transition below 𝑇𝑁 = 7.1, 8.5, and 3.7 K for Nd, Dy, and Ho compounds, respectively. The high-temperature (T) data for all three compounds follow the Curie – Weiss relationship giving an effective magnetic moment close to that expected for the trivalent rare-earth ion. Again, large MCE were obtained for all three compounds similar to those reported for materials that can be used as magnetic refrigerant materials.

The FeCo-V alloy, commercially referred to as Hiperco, is known for its great soft magnetic properties. However, the high cost of production has limited the usage of this alloy to small-scale applications, where the small volume and high magnetic performance are critical. Additive manufacturing (AM) has the potential to solve the production problems that exist in Hiperco manufacturing. The present research has focused on selective laser melting (SLM) based AM processing of Hiperco. The goal was to perform a detailed examination of SLM processed Hiperco and determine how the process parameters affect the microstructure, mechanical and magnetic properties. While a systematic set of SLM process parameters were employed, the results indicate that the energy density was quite similar for this set of process parameters, resulting in similar properties. Overall, the saturation magnetization (Ms) values were very good, but the coercivity (Hc) values were very high, in the case of all as SLM processed conditions. Additionally, a large variation in porosity was observed in the as SLM processed samples, as a function of process parameters. Interestingly, long-term heat-treatments of these samples in an Ar+H2 atmosphere resulted in substantial decreases in the Hc values. These results are presented and discussed.

Cette étude s’intéresse en premier lieu aux caractéristiques magnétiques d’échantillons de BIFs (Banded Iron Formations) en provenance de Mauritanie, où est observable la plus grande partie de l’Anomalie Magnétique Ouest Africaine (AMOA). On met en évidence des valeurs de susceptibilité magnétique allant jusqu’à 3.4 SI, et d’aimantation rémanente jusqu’à 1350 A/m, dans les BIFs. Des valeurs de rapport de Koenigsberger pour la plupart supérieures à 1 impliquent également que la rémanence devrait être prise en compte pour expliquer l’AMOA. L’effet de la pression sur les propriétés magnétiques de la titanomagnétite a également été étudié, car ce paramètre est peu connu, et la plupart du temps négligé dans les modèles numériques des sources des anomalies magnétiques. On montre ainsi une dépendance à la pression de la température de Curie de l’hématite et de la titanomagnétite, ainsi qu’une augmentation de l’Aimantation Thermo Rémanente (ATR) acquise à des pressions lithosphériques, allant jusqu’à +100% à 675 MPa. Un modèle numérique de la croûte sous l’AMOA est ensuite construit, à l’aide de ces contraintes et de données magnétiques et gravimétriques. On utilise une approche directe pour investiguer la profondeur, l’épaisseur et l’intensité d’aimantation des lithologies crustales. Nos résultats montrent que des couches de BIFs sont les seules sources crustales aimantées nécessaires pour expliquer l’anomalie, et qu’elles pourraient être enfouies à plusieurs kilomètres de profondeur. Les résultats de cette étude fournissent de nouvelles perpectives pour l’étude des sources d’anomalies magnétiques dans d’autres régions cratoniques comportant des affleurements de BIFs / The geological sources of major magnetic field anomalies are still poorly constrained, in terms of nature, geometry and vertical position. A common feature of several anomalies is their spatial correlation with cratonic shields and, for the largest anomalies, with Banded Iron Formations (BIF). This study first unveils the magnetic properties of some BIF samples from Mauritania, where the main part of the West African magnetic anomaly is observed. It shows magnetic susceptibility values up to 3.4 SI and natural remanent magnetization up to 1350 A/m can be reached by BIF rocks. Koenigsberger ratios mostly superior to 1 imply that the remanent magnetization should be taken into account to explain the anomaly. I also investigated the impact of pressure on magnetic properties of titanomagnetite, because it is not well known and most of the time neglected in numerical models of the geological sources of magnetic anomalies. My results show a pressure-dependent Curie temperature increase, as well as an intensity increase for TRM acquired under lithospheric pressure (up to +100% at 675 MPa). A numerical modeling of the crust beneath the West African anomaly is then performed using these constraints and both gravity and magnetic field data. A forward approach is used, investigating the depth, thickness and magnetization intensity of all possible crustal lithologies. Our results show that BIF slices may be the only magnetized lithology needed to explain the anomaly, and that they could be buried several kilometers deep. The results of this study provide a new perspective to address the investigation of magnetic field anomaly sources in other cratonic regions with BIF outcrops