Dissertations / Theses on the topic 'Magnetite Heat treatment'

Pelletizing is a size enlargement technique employed to process fine-grained iron-bearing concentrates and powder ores. Mechanical strength of fired pellets is important for handling. When the pellets undergo metallurgical processing, their mechanical strength is a measure of their resistance to degradation by breakage due to impacts and abrasion to which they are exposed in the upper part of the blast furnace. In this study, heat treatment of iron ore agglomerates with microwave energy is investigated. First drying and then heat hardening tests were performed. Two main properties of pellets were taken into consideration: percent moisture and magnetite content for the dried pellets and compressive strength and also magnetite content for the fired pellets. The tests were conducted with different particle sized pellets, in different durations. In order to increase the oxidation rate in heat hardening tests, Na2O2 is also added in different percentages. The results of the study showed that, magnetite pellets can indeed be dried and heated with microwave energy. However, the attained compressive strength and v the oxidation of the fired pellets were not sufficient as compared to pellets produced by conventional heating

In treating cancer, a primary consideration is the target specificity of the treatment. This is a measure of the treatment dose that the cancerous (target) tissue receives compared to the dose that healthy tissue receives. Nanoparticle (NP) based treatments offer many advantages for target specificity compared to other forms of treatment due to their ability to selectively target tumors. One benefit of using magnetic NPs is their ability to release heat, which can both sensitize tumors to other forms of treatment as well as damage the tumor. The work here aims to incorporate a broad range of relevant physics into a comprehensive model. NP aggregation is known to be a large source of uncertainty in these treatments, thus a framework has been developed that can incorporate the effects of aggregation on NP diffusion, NP heat release, temperature rise, and overall thermal damage. To quanitify thermal damage in both healthy tissue and tumor tissue, the Cumulative Equivalent Minutes at 43 textcelsius~model is used. The Pennes bioheat equation is used as the governing equation for the temperature rise and included in it is a source heating term due to the NPs. NP diffusion and aggregation are simulated via a random walk process, with a probability of aggregation determining if nearest neighbor particles aggregate at each time step. Additionally, models are developed that attempt to incorporate aggregation effects into NP heat dissipation, though each proves to only be accurate when there is little aggregation occurring. In this work, verification analyses are done for each of the above areas and, at minimum, qualitatively accurate results have been achieved. Verification results of this work show that aggregation can be neglected at concentrations on the order of $100~nM$ or less. This however only serves as a rough estimation and further work is needed to gain a better quantitative understanding of the effects of NP concentration on aggregation. Using this concentration as a limitation, results are presented for a variety of tumor sizes and concentration distributions. Because this work incorporates a variety of physics and numerical methods into a single encompassing model, depth and physical accuracy in each area (bio-heat transfer, diffusion via random walk, NP energy dissipation, and aggregation) have been somewhat limited. This does however provide a framework in which each of the above areas can be further developed and their effects examined in the overall course of treatment.
Master of Science

Iron-cobalt-vanadium alloys can be processed to have excellent soft magnetic properties for use in high performance power generation applications such as the rotors and stators of aircraft integrated power units. These soft magnetic properties are, however, developed at the expense of mechanical strength and toughness. Small additions of niobium are reported to increase the strength of these Fe-Co-V alloys. This study evaluates the effects of heat treatment on the mechanical and magnetic properties of heavily cold work strip of a 48 wt.% iron-48 wt.% cobalt-2 wt.% vanadium alloy with a 0.3 wt.% addition of niobium. For heat treatments between 640 and 740°C for 1 hour the tensile and yield strengths and ductility of the alloy were all found to be superior to a similar alloy found in the literature without the addition of Nb and processed in a similar manner. Magnetic permeability, remnant induction, saturation induction, coercivity and core loss were only slightly degraded at all annealing temperatures when compared with the non-niobium containing alloy. All properties were shown to depend primarily on degree of recrystallization of the sample, which was found to fully recrystallize between 720 and 740 °C for 1 hour anneals. No significant change in measured properties were found when annealing time was increased to 2 hours. Full recrystallization was observed for samples annealed for as short of times as 10 minutes at 800 °C.
Master of Science

Introduction There is a pressing clinical need to treat patients with acute coronary syndrome (ACS) timely and efficiently in order to improve their prognosis. Standard tools available in ED, while useful, do not comprehensively characterize ACS for either diagnosis or risk stratification. The role of CMR in ACS is emerging because it allows assessment of both myocardial composition and function. Newer CMR techniques such as: a) T2 W imaging for assessing myocardial oedema and area at risk B) pre contrast T1 mapping techniques for quantitative characterization of the tissue composition, are adding further utility for CMR in ACS. At present the clinical use of these techniques is still limited and further investigations are needed to assess their clinical applicability in ACS patients. Aims The aims of this thesis were several. Firstly we sought to establish a CMR protocol for imaging ACS patients on a 3T CMR scanner. In order to do so, we validated a novel T2 W technique for oedema imaging (T2 prep SSFP) at 3T. Second, we aimed to perform a detailed study of the time course of oedema in ACS patients in order to establish the appropriate imaging time for the assessment of area at risk. Third, by applying T2W acute oedema imaging, we sought to investigate the functional and pathological meaning of complicated remote plaques in patients with multivessel disease. Finally, we aimed to establish whether, in comparison to standard CMR techniques, novel precontrast Tl mapping allows better characterisation of the acutely injured myocardium and whether it can predict long-term functional recovery. Methods The research studies were all performed on a 3T Trio Siemens scanner. In the initial stage of the research, we validated the T2 W technique performing phantom work and scanning both volunteers and patients to assess the uniformity of signal intensity in the myocardium and to establish a threshold based method to post process the images. We then established a CMR protocol for ACS including oedema imaging, T1 mapping imaging, perfusion, functional and late gadolinium enhancement imaging. Patients with acute myocardial infarction (both ST elevation myocardial infarction (STEMI) and non STEMI) were scanned at 4 different time points after the acute event (3 scans within 2 weeks and one at 6 months). All STEMI patients underwent primary percutaneous coronary intervention (PCI) while the non-STEMI patients underwent coronary angiography and for PCI. Results We validated the T2prep SSFP technique at 3T, highlighting its limitations and establishing a threshold of mean ± 2SD to assess myocardial oedema. We found that the optimal imaging window to assess the maximal expression of myocardial oedema was within 1 week from the acute event in patients with ST elevation MI. Also, our results showed a reduction of LGE over time (from acute to chronic) in segments which also showed improvement in contractile function indicating that even segments with transmural LGE assessed in the early hours post event could be viable. By applying these techniques in acute patients with bystander disease undergoing percutaneous coronary intervention, we found that: l) T2W imaging can detect myocardial injury downstream from a vessel identified as "non culprit" 2) in 20% of NSTEMI patients, the angiographic assessment alone failed to identify the culprit vessel. Finally, we found that the diagnostic performance of acute pre-contrast Tl-mapping was at least as good as that ofT2W CMR for detecting myocardial injury. There was a significant relationship between the segmental damaged fraction assessed by either by LGE or T2W, and mean segmental Tl values and the likelihood of improvement of segmental function at 6 months decreased progressively as acute Tl values increased. Conclusions In summary, we defined a stable imaging window for the retrospective evaluation of area at risk and we also indicated that acutely detected LGE does not necessarily equate with irreversible injury and may severely underestimate salvaged myocardium. Furthermore, in NSTEMI patients with multivessel disease, by revealing acute myocardial damage in territories pertaining to vessels not treated acutely, we raised the issue of the need for better tools for the correct identification of the culprit vessel and to stratify patients rather than by angiographic assessment alone. Finally, we demonstrated how pre-contrast Tl mapping allows for assessment of the extent of myocardial damage and how Tl mapping might become an important complementary technique to LGE and T2W for the identification of reversible myocardial injury and the prediction of functional recovery in acute MI.

Many Co-based Heusler alloys with the stoichometric composition X2YZ are ideal candidates for the spintronics applications. So, they have been extensively studied theoretically and experimentally. The aim of this work was to investigate the effect heat treatment on phase stability and magnetic properties for quaternary Co2FeSi1-xGax Heusler alloys with varying Si concentration. The Co2FeSi1-xGax alloy samples were prepared by conventional arc melting technique. The structure of Co2FeSi1-xGax bulk alloys were examined by powder x-ray diffraction and differential scanning calorimetry. It was confirmed that Co2FeSi1-xGax alloys display the L21 type structure for all x compositions based on the annealing temperature. The magnetic ordering transition temperature, Tc, was measured by differential scanning calorimetry. It was found that the order-disorder phase transition temperature from the L21 to the B2 structure, T , decreases while the Curie temperature, Tc, increases with increasing x
however, the value of these temperatures were not influenced by changing heat treatment process. The magnetic properties of Co2FeSi1-xGax alloy were investigated by using vibrating sample magnetometer. Higher saturation value was obtained at the L21 phase than the value obtained at the B2 phase. It was concluded that the Co2FeSi0.2Ga0.8 alloy was chosen optimum composition for spintronics applications because of its highest Curie temperature and phase stability of L21.

The feasibility of using hydrochloric acid (HCl), heat, dilution and magnetic stirring for the pre-treatment of palm oil mill Effluent (POME) before the primary anaerobic treatment was investigated in this study. The theoretical background of oily water emulsion which is the characteristic of POME was reviewed. A range of experiments was performed on samples made up of different combinations of the three major components of POME namely, palm oil, solid from decanter and water. The results suggest that the development of a pre-treatment system to remove the 0.5- 1.2% residue oil and 3-4% solid matter from the fresh POME is feasible thus it could improve the efficiency of further downstream POME treatment.Experiments were conducted to examine the rate of oil flotation from the mixtures of different ratios of palm oil and water treated with different concentrations of HCl, and temperatures and magnetic stirring. Similarly, a series of experiments were performed to determine the rate of solid settlement from palm oil-solid mixture, solid-water mixture and palm oil-solid-water mixture of different ratios treated with different concentrations of HCl and different temperatures. The data obtained from the experiments were used to determine the optimum dosage of HCl used and the temperature required for best oil recovery and solid settlement.From the kinetic studies, the models of the kinetic rate of palm oil flotation and solid settlement were derived. A macro kinetic modeling was adapted to the oil flotation while a power model was used for solid settling. The results showed that treatment with 0.5% HCl was sufficient to increase the rate of oil flotation significantly in Palm oil-water mixture. However, the effect was dependent on the oil-water ratio. An increase in temperature gave higher rate of oil flotation but not as great as that of HCl treatment. Dilution was found to be the two other factors that affected the rate of flotation. The solid settling rates in all tested samples were not significantly affected when they were treated with HCl. The rate of solid settlement was found to be temperature dependent. The optimum temperature for the rate of solid sedimentation was found to be in the region of 800C. Similar positive effect was also observed for a more diluted sample of Solid-Palm oil-Water mixture.

На сучасному етапі розвитку магнітоелектроніки велика увага дослідників приділяється вивченню впливу різних фізичних полів на стабільність робочих характеристик матеріалів чутливих елементів датчиків магнітного поля. Дана робота присвячена встановленню загальних закономірностей впливу температури термообробки на магнітні властивості мультишарів на основі Со і Gd при зміні їх орієнтації у зовнішньому магнітному полі.

Les ultrasons focalisés de hautes intensités ont la capacité de déposer de l'énergie ultrasonore localement et de façon non invasive dans les tissus biologiques. Il est possible d'exploiter les effets mécaniques et/ou thermiques en fonction des paramètres ultrasonores utilisés. Guidée par un système d'Imagerie de Résonance Magnétique, cette technologie se voit dotée d'une modalité de planification et le suivi en temps réel de la procédure. Les applications actuelles des ultrasons focalisés guidés par IRM sont sur des organes fixes, notamment le cerveau et l'os ou le fibrome utérin. Dans le cas du cœur, d'une part la présence de mouvements cardiaques et respiratoires constitue une difficulté importante, tant pour le traitement ultrasonore (balistique) que pour l'IRM de température (artéfacts sur les images). D'autre part, la cage thoracique joue le rôle de barrière pour la propagation des ultrasons. Dans ce travail de thèse, un ensemble de techniques nouvelles pour l'ablation et la stimulation cardiaque non invasive par ultrasons focalisés guidés par IRM a été développé. Une première étude montre la faisabilité technique de contrôler le rythme cardiaque par des impulsions ultrasonores brèves dirigées vers le myocarde. L'influence des paramètres des impulsions a été étudiée quantitativement sur cœur isolé battant puis in vivo sur un modèle préclinique. Pour cela, un dispositif original a été développé. Une seconde étude présente de nouvelles méthodes rapides d'IRM permettant de cartographier simultanément la température et le déplacement local induit par les ultrasons focalisés. La méthode est validée sur le foie sur un modèle préclinique, et démontre qu'il est possible de corréler la dose thermique obtenue par thermométrie IRM à un changement des propriétés mécaniques des tissus traités mesurés simultanément. Une troisième étude a consisté à développer une technique de mesure de position de la cible en 3D temps réel par quelques éléments de l'émetteur ultrasonore opérant en réception. Cette mesure permet de corriger dynamiquement la position du foyer ultrasonore pour maximiser le dépôt d'énergie au point ciblé, le tout monitoré par thermométrie IRM temps réel à une cadence de 10 images par seconde. Là encore, une validation préclinique est présentée. Ce travail de thèse propose donc des avancées importantes pour lever les verrous actuels de la technologie permettant d'envisager des traitements non invasifs des pathologies cardiaques par voie non invasive, le tout guidé par IRM en temps réel
High intensity focused ultrasound has the ability to deposit ultrasonic energy locally and non-invasively into biological tissues. It is possible to exploit the mechanical and/or thermal effects according to the ultrasonic parameters used. Guided by a Magnetic Resonance Imaging (MRI) scanner, this technology is equipped with a planning modality and real-time monitoring of the procedure. As of now, applications of MRI-guided focused ultrasound are on fixed organs, including brain and bone or uterine fibroid. For the heart, the presence of cardiac and respiratory movements constitutes an important difficulty, both for the ultrasonic (ballistic) treatment and for the temperature monitoring under MRI (artefacts on images). In addition, the rib cage acts as a barrier for the propagation of ultrasounds. In this thesis work, a set of new technological development have been developed for ablation and non-invasive cardiac stimulation using focused MRI-guided ultrasound. A first study shows the technical feasibility of controlling heart rhythm by short ultrasound pulses targeted to the myocardium. The influence of the parameters of the pulses (duration, amplitude, emission time in the cardiac cycle) were studied quantitatively on isolated beating heart then in vivo on a preclinical model. For this, an original device was developed. A second study presents new rapid MRI methods for simultaneously mapping the temperature and local displacement induced by focused ultrasound. The method is validated on the liver on a preclinical model and demonstrates that it is possible to correlate the thermal dose obtained by MR-thermometry with a change in the mechanical properties of the treated tissues measured simultaneously. A third study consisted in developing a technique for measuring the position of the target in 3D real-time using some elements of the ultrasonic transmitter as receivers. This measure allows to dynamically correct the position of the ultrasonic focus to maximize energy deposition at the targeted point. In addition, we monitored in real-time the procedure using MR-thermometry at a rate of 10 images per second. Here again a preclinical validation is presented. This thesis work proposes important advances to remove the current locks of the technology allowing to envision noninvasive treatments of cardiac pathologies, all guided by MRI in real-time

Cardiac Resynchronization Therapy (CRT) is a treatment option for heart failure patients with ventricular dyssynchrony. CRT corrects for dyssynchrony by electrically stimulating the septal and lateral walls of the left ventricle (LV), forcing synchronous con- traction and improving cardiac output. Current selection criteria for CRT rely upon the QRS duration, measured from a surface electrocardiogram, as a marker of electrical dyssynchrony. Unfortunately, 30-40% of patients undergoing CRT fail to benefit from the treatment. A multitude of studies have shown that presence of mechanical dyssynchrony in the LV is an important factor in determining if a patient will benefit from CRT. Furthermore, recent evidence suggests that patient response can be improved by placing the LV pacing lead in the most dyssynchronous or latest contracting segment. The overall goal of this project was to develop methods that allow for accurate assessment and display of regional mechanical dyssynchrony throughout the LV and at the site of the LV pacing lead. To accomplish this goal, we developed a method for quantifying regional dyssynchrony from standard short-axis cine magnetic resonance (MR) images. To assess the effects of LV lead placement, we developed a registration method that allows us to project the LV lead location from dual-plane fluoroscopy onto MR measurements of cardiac function. By applying these techniques in patients undergoing CRT, we were able to investigate the relationship between regional dyssynchrony, LV pacing lead location, and CRT response.

Thesis (Ph.D.)--Biomedical Engineering, Georgia Institute of Technology, 2008.
Committee Chair: Oshinski, John N.; Committee Member: Fyfe, Derek A.; Committee Member: León, Angel R.; Committee Member: Skrinjar, Oskar; Committee Member: Taylor, W. Robert.

The potentially most important challenges today are related to energy and the environment. New materials and methods are needed in order to, in a sustainable way, convert and store energy, reduce pollution, and clean the air and water from contaminations. In this, nanomaterials and nanocomposites play a key role, and hence knowledge about the relation between synthesis, structure, and properties of nanosystems is paramount. This thesis demonstrates that solution-chemical synthesis, using amine-modified acetates and nitrates, can be used to prepare widely different nanostructured films. By adjusting the synthesis parameters, metals, oxides, and metal–oxide or oxide–oxide nanocomposites were prepared for two systems based on Co and Zn:Fe, respectively, and the films were characterised using diffraction, spectroscopy, and microscopy techniques, and SQUID magnetometry. A variety of crystalline cobalt films—Co metal, CoO, Co3O4, and composites with different metal:oxide ratios—were synthesised. Heat-treatment parameters and control of the film thickness enabled tuning of the phase ratios. Random and layered Co–CoO composites were prepared by utilising different heating rates and gas flow rates together with a morphology effect associated with the furnace tube. The Co–CoO films exhibited exchange bias due to the ferromagnetic–antiferromagnetic interaction between the Co and CoO, whereas variations in e.g. coercivity and exchange bias field were attributed to differences in the structure and phase distribution. Ordered structures of wurtzite ZnO surrounded by amorphous ZnxFeyO were prepared through controlled phase segregation during the heating, which after multiple coating and heating cycles yielded ZnO–ZnxFeyO superlattices. The amorphous ZnxFeyO was a prerequisite for superlattice formation, and it profoundly affected the ZnO phase, inhibiting grain growth and texture, already from 1% Fe. In addition, ZnO–ZnxFeyO exhibited a photocatalytic activity for the oxidation of water that was higher than results reported for pure ZnO, and comparable to recent results reported for graphene-modified ZnO.

Made available in DSpace on 2016-12-08T17:19:37Z (GMT). No. of bitstreams: 1 Resumo.pdf: 10956 bytes, checksum: b3ab8ff2ededda1434fbc70325d132f4 (MD5) Previous issue date: 2010-12-07
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior
Semi-processed electrical steels require annealing after processing in the motors manufactures to improve motors efficiency by reducing losses and increasing permeability. Annealing in fully processed electrical steel is performed to relax the residual stress and promote recovery or recrystallization of distorted parts. Commercial samples from different steels with different chemical compositions were selected to evaluate the influence of final annealing heat treatment temperature and dew point on the magnetic properties, the carbon content and grain size increase. Were performed with annealing atmosphere without steam and with dew point of 5, 10, 20 and 25°C at temperatures of 760 and 790°C. Magnetic losses, relative permeability, carbon content, grain size and mechanical properties measurements were made in addition to the evaluation of the microstructure to determine this influence. It was observed in the semi-processed steel with 300 ppm carbon content, which with dew point increase the carbon content reduce the grain size increase and improve magnetic properties. In the other steels studied, reducing the dew point improved the magnetic properties, but the atmosphere without steam has improved only fully processed steel with 2% silicon. It was found that in fully processed steels the best results were obtained with annealing temperature of 790°C.
Aços elétricos semiprocessados necessitam de recozimento após a sua manufatura para melhorar o rendimento dos motores com a redução das perdas magnéticas e aumento da permeabilidade. os aços totalmente processados o recozimento é realizado para relaxar as tensões residuais e promover a recuperação ou recristalização das partes deformadas. Amostras comerciais de diferentes aços com variadas composições químicas foram selecionadas para avaliar a influência do ponto de orvalho e temperatura de recozimento final nas propriedades magnéticas, no teor de carbono e no aumento do tamanho de grão. Foram realizados recozimentos com atmosfera sem vapor e com ponto de orvalho de 5, 10, 20 e 25°C, nas temperaturas de 760 e 790°C. Medições de perdas magnéticas, permeabilidade, teor de carbono, tamanho de grão e propriedades mecânicas, além da avaliação da microestrutura, foram efetuados para determinar esta influência. Foi verificado no aço com 300 ppm de carbono, que com aumento do ponto de orvalho reduziu o teor de carbono, aumentou o tamanho de grão e melhorou as propriedades magnéticas. Nos demais aços estudados, a redução do ponto de orvalho melhorou as propriedades magnéticas, porém com ausência de umidade somente houve melhora no aço totalmente processado com 2% de silício. Foi verificado ainda que nos aços totalmente processados os melhores resultados foram obtidos com a temperatura de recozimento de 790°C.

In this work we studied the magnetic properties referring to the MgFe2O4 nanoparticles precipitated in monocrystalline solid solution of [Mg, Fe]O, with 2.2% iron, obtained at different temperatures and times. These particles grow coherently with the matrix lattice and present shapes of small octahedrons whose diagonals are parallel to the [100] directions. The results presented here refer to samples treated in the temperature range between 400 and 900 º C for 2, 6 and 10 hours. They were analyzed by X-ray diffraction (XRD), magnetization as a function of field (hysteresis curves) and magnetization as a function of temperature (Zero Field Cooled e Field Cooled Warming). It was observed that in samples treated for 6 hours, the system shows increasing values of magnetization remanent and coercive field for temperatures of precipitation from 600 º C, which can be attributed to the precipitation and growth of nanoparticles magnesioferrite matrix. The variation of coercive field with temperature measurement was studied using two different theoretical models. By comparing the remanent magnetization and coercive field of the samples, it was found that the variation of the inversion parameter of magnesioferrite in the studied range of precipitation temperature decreases as reported by other authors.
Neste trabalho foram estudadas as propriedades magnéticas do sistema de nanopartículas de MgFe2O4 obtidas por precipitação em solução sólida monocristalina de [Mg;Fe]O, com 2,2% de ferro, em diferentes tempos e temperaturas de precipitação. Estas partículas crescem de forma coerente com a matriz, exibindo a forma de pequenos octaedros cujas diagonais são paralelas às direções [100] da rede cristalina da matriz, que possui simetria cúbica. Os resultados aqui apresentados são referentes a amostras tratadas no intervalo de temperaturas entre 400 e 900ºC durante 2, 6 e 10 horas. As mesmas foram analisadas por difração de raios X (DRX), magnetização em função do campo (curvas de histerese) e magnetização em função da temperatura (Zero Field Cooled e Field Cooled Warming). Observou-se que, em amostras tratadas durante 6 horas, o sistema apresenta valores crescentes de magnetização remanente e campo coercivo para temperaturas de precipitação a partir de 600ºC, fato que pode ser atribuído à precipitação e ao crescimento de nanopartículas de magnesioferrita na matriz. A variação do campo coercivo com a temperatura de medição foi estudada utilizando-se dois diferentes modelos teóricos e, a partir da comparação da magnetização remanente e do campo coercivo das amostras tratadas em diferentes temperaturas, verificou-se que a variação do parâmetro de inversão da magnesioferrita na faixa de temperaturas de precipitação estudada decresce como reportado por outros autores.

Made available in DSpace on 2014-10-09T12:34:08Z (GMT). No. of bitstreams: 0
Made available in DSpace on 2014-10-09T14:06:40Z (GMT). No. of bitstreams: 0
Dissertação (Mestrado)
IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Etude par rmn en phase solide et par analyses d'images de microscopie electronique. Evaluation du pourcentage des differentes especes, de la densite en hydroxyles et de leur evolution en fonction d'un traitement thermique determine. Etude de la structure geometrique des surfaces apres griffage de petites molecules (diols et alcools). Proposition d'un modele ou la surface des silices de precipitation est constitue d'une couche tres desorganisee d'epaisseur donnee. Caracterisation des projections bidimensionnelles des agregats de silice par des exposants fractals, a partir des micrographies electroniques

Caracterisation de couches minces cozr et co(zr,nb) deposes par pulverisation cathodique en radio-frequences. Etude de l'anisotropie developpee aux faibles et fortes pressions de depot. Discussion relative a l'origine de ces anisotropies. Etude du controle de la direction et de l'intensite du champ d'anisotropie par application de recuits sous champ magnetique tournant suivis de recuits sous champ magnetique fixe

Submitted by Claudinei Pracidelli (cpracide@ipen.br) on 2015-06-09T18:22:48Z No. of bitstreams: 0
Made available in DSpace on 2015-06-09T18:22:49Z (GMT). No. of bitstreams: 0
Tese (Doutorado em Tecnologia Nuclear)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Effets microstructuraux de l'oxygene dans l'alliage pour aimant permanent nd#1#5fe#7#7b#8 a l'etat brut de fonderie et apres traitement l'oxydation a l'air. Analyse des microstructures de rubans nd#1#5fe#7#7b#8 trempes des vitesses croissantes a partir du liquide, ainsi que celles de rubans cristallises depuis l'etat amorphe. Correlation entre microstructure et proprietes magnetiques. Etude de rubans microcristallises d'alliages a matrice sm(fe, ti)#1#2 obtenus par solidification rapide suivie de differents traitements thermiques provoquant la cristallisation de phases secondaires

La micro fusion laser d'un lit de poudre (SLM) permet la réalisation de pièces complexes avec des microstructuresfines. Cette technologie présente de nombreux avantages mais se heurte encore à une faible disponibilité des poudres d'alliages. En SLM, la pièce est d'abord conçue par CAO (conception assistée par ordinateur), puis construite couche par couche avec un faisceau laser commandé par un ordinateur. Dans ce cadre, le travail effectué dans cette thèse a consisté à étudier et à développer une nouvelle méthode pour réaliser des pièces en alliages et en composites à partir de mélanges de poudres élémentaires, ouvrant ainsi la voie à une grande variété de compositions.Au niveau expérimental le choix s'est porté sur le système aluminium-silicium avec différentes teneurs en silicium (12, 18 et 50% en poids). L'effet de l'ajout d'un champ magnétique statique a aussi été proposé comme un outil supplémentaire de contrôle de la microstructure.Dans le processus de fabrication de pièces par SLM la puissance du laser et la vitesse de balayage déterminent au premier chef la densité, la microstructure, la composition des phases et les propriétés mécaniques du produit. Une analyse systématique de l'effet de ces paramètres sur l'alliage Al - Si fabriqué par SLM à partir de mélanges de poudres est présentée. Des alliages ont été ainsi obtenus pour plusieurs domaines de composition visés correspondant à des applications pratiques (structures légères, système tribologique, emballage électronique, ...).Les microstructures fines obtenues grâce à la solidification rapide des matériaux fondus conduit à des propriétés quise comparent de façon favorable à celles obtenues avec les techniques classiques d'élaboration et de mise en oeuvre
As a new manufacturing technology, Selective laser melting (SLM) has a large potential in the manufacturing of complex parts with ultrafine microstructure.Selective laser melting has many significant advantages over traditional manufacturing methods but still faces a low availability of powder materials. With SLM, the part is firstly designed via 3D computer-aided design (CAD)), then built layer-by-layer with a high energy computer-controlled laser beam The work done in this study was therefore aiming at developing a new way to obtain alloys and composites directly from elemental powder mixtures with a large composition flexibility.Experimentally the choice was made of the aluminum-silicon system with several silicon contents (12, 18, 50 wt. %).Adding a static magnetic field was also considered as an additional way to control the microstructure. When parts are manufactured by SLM, laser power and scanning speed are the main parameters determining the density, microstructure, phase composition and mechanical properties. A systematic analysis of the role of these parameter on the manufacturing of Al - Si alloys by SLM from mixtures of powders was therefore conducted. Al - Si alloys with a very fine microstructure were thus obtained for several composition ranges corresponding to practical applications (lightweight structures, high wear resistance alloys, electronic packaging material, ...). The properties of the materials obtained in this way, according to the performed characterizations, compares favorably with those obtained via the conventional production technologies

Le traitement thermique (« torréfaction ») des graines de Coffea arabica L. détermine leur composition chimique et, de ce fait, la composition et les propriétés organoleptiques de la boisson qui en est issue (« café »). Dans cette étude, nous avons utilisé plusieurs techniques de spectroscopie de résonance magnétique nucléaire quantitative (q RMN) pour explorer les phénomènes qui ont lieu au cours de la torréfaction et de l’extraction en phase aqueuse des grains de café broyés. Des plans d'expériences ont été mis en œuvre, afin d’examiner l’influence de paramètres clés des torréfactions et, in fine, d'identifier les mécanismes des phénomènes que ces traitements provoquent. Contrairement aux études antérieures, nous avons appliqué des barèmes de torréfaction représentatifs des pratiques industrielles. Nous avons établi que les paramètres de commande et de contrôle utilisés par l’industrie ne suffisaient pas à caractériser les diverses torréfactions. Puis, par des analyses chimiométriques, nous avons identifié les composés dont les concentrations varient avec les cinétiques considérées. Des traitements thermiques plus poussés ont aussi été effectués afin (1) d'établir des corrélations entre ces composés et des changements de couleur et de pH et (2) d'identifier les mécanismes réactionnels qui interviennent au cours des torréfactions
The heat treatment (“roasting”) of Coffea arabica L. seeds determines their chemical composition and, as a result, the composition and organoleptic properties of the resulting beverage ("coffee"). In this study, we used several quantitative nuclear magnetic resonance (q NMR) spectroscopy techniques to explore the phenomena that occur during roasting and extraction of coffee beans in the aqueous phase. Experimental designs were implemented to examine the influence of key roasting parameters and, ultimately, to identify the mechanisms of the phenomena that these treatments cause. Unlike previous studies, we applied roasting kinetics that are in line with industry standards. We determined that the parameters used by the industry were not sufficient to characterize the various roasts. Then we used chemometrics in order to identify markers, i.e. compounds whose concentrations vary with the kinetics involved. More extensive heat treatments were also carried out to (1) establish correlations between these compounds and changes in colour and pH and (2) identify the reaction mechanisms that occur during roasting

I. Proprietes magnetiques et magnetomecaniques (magnetostriction) et leurs modifications (traitements thermiques, irradiation par ions lourds) sont etudiees dans deux alliages amorphes ferromagnetiques. Ii. Proprietes structurales et supraconductrices d'une nouvelle famille d'oxydes supraconducteurs a haute temperature tl-ba-ca-cu-o

Les composites ferromagnétiques, matrices polymères renforcées de particules ferromagnétiques présentent un potentiel intéressant dans de nombreuses applications médicales. Dans cette thèse, nous nous concentrons particulièrement autour du Chauffage par Induction Basse Fréquence (CIBF) de cathéters ferromagnétiques, une méthode alternative pour l'ablation des varices. L'effet CIBF apparaît dès lors que le composite est exposé à un champ magnétique alternatif. Ce phénomène est principalement dû aux courants de Foucault dits "microscopiques" générés par les mouvements des parois des domaines magnétiques. En introduisant le cathéter à travers la varice endommagée et en l'excitant par un champ magnétique basse fréquence, haute amplitude, il est concevable d'atteindre une température suffisamment élevée pour guérir correctement la zone endommagée sans perturber les zones saines environnantes. Par comparaison aux traitements existants, la méthode CIBF est précise, économique et simple. En transférant la chaleur sans conduction, l'encombrement du cathéter est réduit et le procédé semble applicable même pour des veines très sinueuses. Des composites ferromagnétiques de différentes formes et fractions volumiques ont été fabriqués et testés grâce à un dispositif expérimental dédié. Différents paramètres (fréquence, pourcentage de particules…) ont été analysés afin d’établir la combinaison présentant la meilleure réponse thermique. Les propriétés physiques (perméabilité, conductivités électrique et thermique) ont également été caractérisées. Un modèle Comsol® combinant comportement ferromagnétique et thermique a été conçu afin d’améliorer la compréhension des phénomènes. Pour améliorer la conversion, des échantillons anisotropes ont été développés en imposant un champ magnétique statique dans la phase de solidification. Finalement, une imprimante 3D de type extrusion a été utilisée pour imprimer des échantillons de formes proches de celle d’un cathéter. Des spécimens isotropes et anisotropes ont été imprimés. Les réponses CIBF distinctes et marquées entre les différentes directions testées chez les échantillons anisotropes ouvrent la voie à d’autres applications médicales comme le suivi électromagnétique (navigation chirurgicale)
Ferromagnetic composites, polymer matrix mixed with ferromagnetic particles show good potential in medical applications. In this thesis, we especially focus on the Low Frequency Induction Heating (LFIH) of ferromagnetic catheters as an alternative process for varicose veins ablation. The LFIH effect appears as soon as the composite is exposed to an alternating magnetic field. This phenomenon is mainly due to the so-called "microscopic" eddy currents generated by the magnetic domain wall motions. By inserting the catheter through a damaged varicose vein, and exciting it with a low frequency, high amplitude magnetic field, it is conceivable to reach a temperature high enough to properly heal the damaged area without injuring the surrounding healthy ones. Compared to the existing treatments, the LFIH method is accurate, cost competitive and simple. By transferring heat in a non-conductive way, the catheter bulkiness is reduced and the method is applicable even in tortuous veins. Ferromagnetic composites with different shapes and particle volume fractions were built and tested in a specific experimental bench. Different parameters (frequency, particle fraction …) were analyzed to reach the best thermal answer. The physical properties (permeability, electrical and thermal conductivities) were also characterized. A Comsol® model combining ferromagnetic behavior and thermal transfer properties was designed to improve the understanding of the phenomena. For a better efficiency, specimens with anisotropic magnetic behaviors were built by curing them under the influence of a static magnetic field. Finally, a commercial extrusion-type 3D printer was used to print samples with catheter shapes. Isotropic and anisotropic specimens were built. Interesting LFIH behavior were observed and for the later ones directional answers potentially interesting in alternative medical applications like the electromagnetic tracking (surgery navigation)

Mécanismes, caractéristiques et facteurs influant le dépôt électrolytique. Techniques d'élaboration et de dosage du fer dans les alliages NI-FE déposés. Influence des conditions opératoires sur la nature et composition des alliages élaborés. Étude des propriétés électriques magnétiques et de l'influence des traitements thermiques sur la structure des alliages

The majority of UK’s intermediate level radioactive waste is currently stored in 316L and 304L austenitic stainless steel containers in interim storage facilities for permanent disposal until a geological disposal facility has become available. The structural integrity of stainless steel canisters is required to persevere against environmental degradation for up to 500 years to assure a safe storage and disposal scheme. Hitherto existing severe localised corrosion observances on real waste storage containers after 10 years of exposure to an ambient atmosphere in an in-land warehouse in Culham at Oxfordshire, however, questioned the likelihood occurrence of stress corrosion cracking that may harm the canister’s functionality during long-term storage. The more corrosion resistant duplex stainless steel grade 2205, therefore, has been started to be manufactured as a replacement for the austenitic grades. Over decades, the threshold stress corrosion cracking temperature of austenitic stainless steels has been believed to be 50-60°C, but lab- and field-based research has shown that 304L and 316L may suffer from atmospheric stress corrosion cracking at ambient temperatures. Such an issue has not been reported to occur for the 2205 duplex steel, and its atmospheric stress corrosion cracking behaviour at low temperatures (40-50°C) has been sparsely studied which requires detailed investigations in this respect. Low temperature atmospheric stress corrosion cracking investigations on 2205 duplex stainless steel formed the framework of this PhD thesis with respect to the waste storage context. Long-term surface magnesium chloride deposition exposures at 50°C and 30% relative humidity for up to 15 months exhibited the occurrence of stress corrosion cracks, showing stress corrosion susceptibility of 2205 duplex stainless steel at 50°C.The amount of cold work increased the cracking susceptibility, with bending deformation being the most critical type of deformation mode among tensile and rolling type of cold work. The orientation of the microstructure deformation direction, i.e. whether the deformation occurred in transverse or rolling direction, played vital role in corrosion and cracking behaviour, as such that bending in transverse direction showed almost 3-times larger corrosion and stress corrosion cracking propensity. Welding simulation treatments by ageing processes at 750°C and 475°C exhibited substantial influences on the corrosion properties. It was shown that sensitisation ageing at 750°C can render the material enhanced susceptible to stress corrosion cracking at even low chloride deposition densities of ≤145 µm/cm². However, it could be shown that short-term heat treatments at 475°C can decrease corrosion and stress corrosion cracking susceptibility which may be used to improve the materials performance. Mechanistic understanding of stress corrosion cracking phenomena in light of a comprehensive microstructure characterisation was the main focus of this thesis.

In the foundation of this work is the issue for production of non-magnetic materials with predetermined weak magnetic properties. Preferable solution is to dope these materials with ferromagnetic impurities in low concentrations. One of the efficient ways to obtain such materials is the use of powder metallurgy which gives an opportunity to produce complex powder compositions with variety of components in precisely specified concentrations.

Tese de mestrado integrado em Engenharia Biomédica e Biofísica, apresentada à Universidade de Lisboa, através da Faculdade de Ciências, 2017
De acordo com os dados de 2017 da Organização Mundial da Saúde, as doenças cardiovasculares são a principal causa de morte a nível mundial. Se estes tipos de doenças não forem diagnosticadas e tratadas atempadamente, podem levar a insuficiências cardíacas ou outras complicações irreversíveis. As duas doenças cardiovasculares congénitas estudadas neste trabalho são a coarctação aórtica (CoA), caracterizada por uma estenose, habitualmente, na zona do arco da artéria aorta, e a doença da válvula aórtica (AvD), uma malformação ao nível da válvula aórtica. Estas doenças são responsáveis por cerca de 50,000 intervenções por ano. Deste modo, a melhoria métodos de diagnóstico e de intervenção adequados e eficientes é uma prioridade e pode levar ao decréscimo no número das intervenções, bem como reduzir a morbilidade e a mortalidade. A área de imagiologia médica de diagnóstico tem tido uma evolução significativa ao longo dos anos e é de extrema importância nas tentativas de substituição de métodos de diagnóstico invasivos. As imagens médicas são adquiridas e posteriormente processadas e analisadas, com recurso a programas adequados. Atualmente, é possível obter os valores de gradientes de pressão relativa a partir de Ecocardiografia Doppler e Ressonância Magnética. Contudo, os gradientes de pressão medidos no cateterismo cardíaco, o método gold standard para o diagnóstico de CoA e AvD, são gradientes de pressão absoluta. Nesta dissertação desenvolveu-se um método de diagnóstico de CoA e AvD, a partir dos mapas de pressão relativa no estreitamento da aorta e na válvula aórtica, respectivamente. O método matemático desenvolvido tem por base as equações de Poisson, resolvida com a condição de fronteira de Neumann utilizando os métodos de elementos finitos, e a de Navier Stokes para a conservação do momento. O método desenvolvido também tem em conta a informação proveniente da função de Windkessel da artéria aorta, uma artéria distensível. Esta função dá-nos o comportamento da propagação do pulso de pressão com uma velocidade de pulso de propagação. Deste modo, é observado um desfasamento temporal entre as curvas de fluxo da pressão e da velocidade, entre as duas regiões de interesse escolhidas. Deste modo, o método, denominado de Time-shift Corrected Pressure Maps (TCPM, sigla em inglês), permite obter os mapas de pressão absoluta, isto é, mapas de pressão que têm em conta o intervalo de tempo entre os picos de pressão na aorta descendente e ascendente, no caso do primeiro estudo, e antes e depois da válvula aórtica, no caso do segundo estudo. Os pacientes de ambos os estudos tinham indicação clínica para cateterismo cardíaco e foram submetidos a ressonância magnética cardiovascular de contraste de fase em tempo real (4D PC MRI, em inglês), para recolher as imagens ao nível da aorta e da válvula aórtica e os respectivos campos de velocidade da corrente sanguínea. O primeiro estudo tem como objetivo a aplicação do método TCPM a 27 pacientes de CoA (n=16 masculinos, n=11 femininos, faixa etária de 4 a 52 anos, idade média de 20±15 anos). Após aquisição das imagens, estas foram processadas usando programas específicos. Em primeiro lugar foi necessário segmentar a aorta, seguiu-se a seleção das regiões de interesse e, finalmente, a obtenção dos campos de velocidade e dos mapas de pressão relativa entre as duas regiões de interesse selecionadas. Após aplicação do método TCPM, foram aplicados testes estatísticos (correlação, teste t e Bland-Altman) para comparar os valores obtidos a partir de TCPM com os valores obtidos no cateterismo cardíaco. Após processamento das imagens dos 27 pacientes, 6 pacientes foram retirados do estudo. N=3 pacientes foram retirados porque a percentagem de fluxo que passa pelo estreitamento é insuficiente para calcular o gradiente de pressão a partir de TCPM e N=3 pacientes foram retirados porque a aorta não estava inserida por completo no FOV. As medições obtidas a partir de TPCM e cateterismo cardíaco têm uma correlação linear significante (R²=0,90; p<0,001). A partir dos gráficos Bland-Altman é possível verificar uma boa concordância entre as medições de ambos os métodos, com bias de -2,69 mmHg e os limites de concordância de ±4,74 mmHg. O teste de equivalência mostrou uma relação significante entre os métodos (p=0,007). O segundo estudo tem como objetivo a aplicação do método TPCM e o método da Área de Gorlin a 4 pacientes de AvD (n=4 masculinos, faixa etária 17 a 36 anos, idade média 27±7 anos). O método da Área de Gorlin permite obter o gradiente de pressão absoluta a partir da área geométrica da válvula e do fluxo total que passa nessa área. Após a aquisição das imagens, foi feito o processamento das mesmas. Numa primeira fase, as imagens foram segmentadas na região da válvula aórtica. Depois, as imagens segmentadas foram analisadas em dois programas distintos. O primeiro foi utilizado de forma a obter os campos de velocidade e os mapas de pressão relativa entre dois pontos antes e depois da válvula aórtica. O segundo permitiu definir a região da válvula como região de interesse e exportar os valores de velocidade, área, pressão relativa e fluxo absoluto nessa região. Os resultados mostram uma correlação linear significativa entre os valores de cateterismo cardíaco e de TCPM (R²=0,99; p<0,001). Os gráficos de Bland-Altman mostram uma boa concordância entre os valores de TCPM (24,75±22,50 mmHg) e de cateterismo (20,88±19,51 mmHg), com um bias de -3,87 mmHg e limites de concordância de ±3,64 mmHg. Os resultados também sugeriram uma ligeira subestimação dos valores do cateterismo cardíaco a partir do método da Área de Gorlin (14,47±13,00 mmHg), com um bias de 6,41 mmHg e limites de concordância de ±7,15 mmHg. Este estudo foi feito com uma amostra diminuta de 4 pacientes, o que não é suficiente para retirar conclusões com significância. Contudo, foi uma primeira abordagem positiva, que mostra a potencialidade que este método pode vir a apresentar. O método TCPM proposto neste projeto permite a medição não invasiva de gradientes de pressão absoluta a partir de mapas de pressão relativa em pacientes de CoA e AvD. Vários aspectos têm que ser tidos em conta de forma a garantir a eficácia deste método. Por exemplo, as regiões de interesse escolhidas têm que se cuidadosamente selecionadas de forma a serem perpendicular à direção do fluxo naquele local. Só desta maneira é possível obter o fluxo, os campos de velocidade e as pressões relativas corretas. Também, se o raio da estenose for menor que 2 voxéis, a relação sinal-ruído aumenta substancialmente, e a resolução especial da aquisição é insuficiente. Contudo, a aplicação do método TPCM a casos de grande estreitamento não é necessária visto que estes casos já são tipicamente identificados em imagens anatómicas de ressonância magnética e que o paciente segue automaticamente para intervenção quando a área do estreitamente representa cerca de 50% do valor de área típico da aorta. O método não invasivo TCPM apresenta uma boa concordância com o cateterismo cardíaco em termos da medição dos gradientes de pressão em CoA e AvD. Os bias e os limites de concordância entre cateterismo e TCPM foram substancialmente mais pequenos que os bias e os limites de concordância entre cateterismo e ecocardiografia Doppler e entre o cateterismo e o método da Área de Gorlin. Com os resultados apresentados já é possível ver o potencial desta técnica no processo de diagnóstico e decisão de intervenção em casos de CoA e AvD. Contudo, estudos com populações maiores será extremamente benéfico para validar clinicamente este método.
This dissertation aims to validate MRI-based time-shift corrected pressure mapping (TCPM) against cardiac catheterization in CoA and AvD patients. Also, in AvD patients, catheterization will be compared against Gorlin Area method. This project is divided in two independent studies: the first one for CoA patients and the second one for AvD patients, all with clinical indication for cardiac catheterization. In both CoA and AvD, clinical guidelines recommend treatment in the presence of a relevant pressure gradient. While reliable non-invasive measurement approaches would be crucial, the accuracy of currently available methods has been limited. In both studies, 4D PC-MRI was performed to compute relative pressure maps via Pressure-Poisson equation. To consider the patient-specific peak pressure time-shift from the ascending to the descending aorta and before and after the aortic valve, relative pressure gradient maps were corrected by the inertial term. Comparison between TCPM and invasive peak-to-peak measurements was performed using correlation, Bland-Altman plots and mean-equivalence t-test. In the first study, with a cohort of 21 patients with CoA, TCPM and catheter measurements showed significant linear correlation (R²=0.90; p<0.001). Bland-Altman plots demonstrated good agreement between TCPM and catheter derived pressure gradients with mean differences of -2.69 mmHg and 95% limits of agreement between -6.38 and 1.00 mmHg between methods. The mean-equivalence test was significant (p=0.007). In the second study, with a cohort of 4 patients with AvD, the catheterization measurements were compared against TPCM measurements. The results showed significant linear correlation (R²=0.99; p<0.001). Bland Altman plots showed a good agreement between TCPM (24.75±22.50 mmHg) and catheter derived peak-to-peak pressure gradients (20.88±19.51 mmHg), and suggested slight underestimation of the pressure gradients by the Gorlin Area method (14.47±13.00 mmHg). Non-invasive TCPM showed equivalence to pressure gradients from invasive heart catheterization in patients with CoA and AvD. However, in the AvD study, they were obtained for a very small cohort of patients and do not have sufficient statistical significance to validate the method for AvD patients.