Des nuances d’aciers à moyen carbone, microalliés au vanadium, ont été élaborées avec l’objectif d’obtenir de nouvelles microstructures, majoritairement constituées de ferrite aciculaire (FA). Le contrôle de la composition chimique (0.1-0.3 % V) et la vitesse de refroidissement (2.0 °Cs-1) conduit à des fractions de FA atteignant 80 %. Un paramètre empirique, le pouvoir ferritisant, P, a été introduit pour évaluer l’effet combiné de la composition chimique et de la vitesse de refroidissement sur la fraction de FA. Les caractérisations par MEB et MET montrent que la FA se développe à partir de la ferrite proeutectoïde recouvrant les inclusions de MnS. Une précipitation interphase de carbonitrures de vanadium, V(C,N), serait à l’origine d’un appauvrissement local en carbone de la matrice austénitique autour des aiguilles de FA, favorisant une germination autocatalytique. Le caractère fractal de la FA a été mis en évidence par des caractérisations morphologiques. Les dimensions fractales, D, et les longueurs de coupure ont été déterminées par la méthode de comptage de boîtes à partir d’images MEB. Des essais mécaniques isothermes-quasistatiques révèlent des propriétés mécaniques équivalentes à celles des microstructures bainitiques. Les courbes contrainte-déformation montrent un comportement mécanique de type Hollomon. Les structures de ces aciers présentent des taux de consolidation qui augmentent avec l’accroissement de la fraction de FA. Une corrélation entre les propriétés mécaniques et la dimension fractale a été établie. Ce lien s’exprime par des relations de type exponentiel : [delta]M = c exp [[alpha](D -2)] où M représente? les propriétés mécaniques (Re, Rm, etc.) et c? et ?[alpha] des constantes / Medium carbon vanadium microalloyed steels have been developed to obtain new microstructures, mainly formed of acicular ferrite (AF). Controlling the chemical composition and (0.1-0.3 % V) and the cooling rates (2.0 °Cs-1) lead to AF fractions up to 80 %. An empirical parameter, the ferritisant power, P, has been introduced to evaluate the combined effect of chemical composition and cooling conditions. Scanning (SEM) and transmission (TEM) electron microscopy investigations indicate that AF develops from proeutectoid ferrite enveloping MnS inclusions. An interphase precipitation of vanadium carbo-nitrides, V(C,N) has been identified. It is suggested that this precipitation is at the origin of carbon depletion in the austenitic matrix surrounding the AF plates. The formation of the AF is then enhanced by an autocatalytic effect. The fractal nature of AF has been determined by SEM and TEM characterisations. Fractal dimensions, D, and cut off lengths have been derived by the counting box method applied to SEM images. Mechanical tests conducted in isothermal and quasistatic conditions reveal that mechanical properties of AF are of the same grade of that of bainitic microstructures. Experimental strain-stress curves are described by the Hollomon law. The work hardening of the studied microstructures increases with the AF fraction. The mechanical properties have been linked to the fractal dimension by the following exponential relation : [delta]M = c exp [[alpha] (D -2)], where M represents the mechanical property (Re, Rm, etc.) and c and [alpha] are constants parameters

En perspective de la prolongation de la durée de vie en service des REPs, il est de plus en plus important d’obtenir une évaluation fiable de l’évolution de la microstructure des aciers constituant la cuve des REPs et de leurs propriétés correspondantes. Un mécanisme de fragilisation non-durcissante, dû à la ségrégation intergranulaire du P qui affaiblirait la cohésion des joints de grains, pourrait contribuer à la fragilisation et doit donc être étudié. Les présents travaux ont pour objectifs d’étudier la ségrégation intergranulaire du P dans un acier de cuve de réacteur afin (i) de connaître l’influence du type de joint de grain sur la ségrégation du P, (ii) de clarifier l’influence des conditions de vieillissement (vieillissement thermique et irradiation ionique) sur la ségrégation du P et (iii) de faire une comparaison avec les modèles disponibles et proposés ici.Pour cela, une méthodologie corrélative -Diffraction des Électrons Rétrodiffusés (EBSD), Diffraction de Kikuchi en Transmission (TKD) et Sonde Atomique Tomographique (APT) -a été adoptée pour étudier la ségrégation intergranulaire. Les informations cristallographiques (5 paramètres) et la composition chimique ont été collectées et systématiquement corrélées. Les aciers ont une microstructure complexe de ferrite aciculaire et de carbures intergranulaires. La ségrégation des solutés aux joints des grains (joints des grains faiblement désorientés (LAGB), joints des grains fortement désorientés généraux (HAGB) et Σ3HAGBs) et aux interfaces (interfaces carbure-ferrite M2.0-3.2C et interfaces cémentite-ferrite) a été quantifiée. Il existe une ségrégation évidente d'un élément ou de plusieurs espèces chimiques (C, P, Mn, Mo, Cr, Si et Ni) pour tous ces types de défauts plans. Tenant compte de la nature des éléments ségrégants et de la cristallographie du joint de grain, les ségrégations interstitielles et substitutionnelles ont été quantifiées et discutées. Sur la base d’un grand nombre de données, il apparaît que les niveaux moyens des segrégations en P sont plus élevés dans les HAGBs généraux ou les LAGBs que les autres types d'interfaces quel que soit le vieillissement envisagé. Par ailleurs, les résultats expérimentaux ont été comparés avec les résultats prévus par des modèles analytiques pour des systèmes binaires, ternaires et multi-composants. Bien qu'ayant un niveau de ségrégation du P prédit plus élevé, le modèle ternaire Fe-P-C se rapproche le plus des résultats expérimentaux. / With expectations for extending the service lifespans of PWRs, it is of great importance to get a reliable evaluation of the microstructural evolution and the corresponding property changes of RPV steels. A non-hardening mechanism, due to intergranular P segregation that impairs the grain boundary (GB) cohesion, may contribute to the embrittlement and thus needs to be studied. The present work aims to investigate the intergranular P segregation behavior in a RPV steel in order to (i) determine the influence of GB type on P segregation behavior, (ii) clarify the influence of ageing conditions (thermal ageing and ion irradiation) on P segregation behavior and (iii) make a comparison with the existing analytical models. To reach these objectives, a correlative - Electron Backscatter Diffraction (EBSD), Transmission Kikuchi Diffraction (TKD) and Atom Probe Tomography (APT) - methodology was adopted to study the GB segregation behavior. The crystallographic information (5 parameters) and chemical composition were collected simultaneously. The steels have a complex microstructure of acicular ferrite and intergranular carbides. The solute segregation at GBs (Low Angle Grain Boundaries (LAGBs), general High Angle Grain Boundaries (HAGBs) and Σ3 HAGBs) and interfaces (M2.0-3.2C carbide-ferrite interfaces and cementite-ferrite interfaces) were quantified. There is an obvious segregation of one element or several chemical species (C, P, Mn, Mo, Cr, Si and Ni) at all boundary types. Taking into account the nature of segregants and the five-parameter GB crystallography, both interstitial and substitutional segregation behaviors were discussed. Based on a large dataset, it appears that the average P segregation levels are higher in general HAGBs or LAGBs than in other boundary types. Besides, the experimental results were compared to the predicted ones from analytical models for binary, ternary and multicomponent systems. Though with a higher predicted P segregation level, the Fe-P-C ternary model seems to better fit the experimental results in all ageing conditions.

<p>У овој докторској дисертацији приказани су резултати синтеза и карактеризација нано-композитних честица са језгро-омотач структуром. Нанокомпозитне честице су синтетисане у течној фази, електростатичком депозицијом in situ синтетисаних SiO2, Fe3O4, ZnFe2O4 или NiFe2O4 наночестица на површину монодисперзних и сферичних силика језгро честица (средњег пречника ~ 0,4 &mu;m). Силика језгро честице су синтетисане хидролизом и кондезацијом TEOS-a у базној средини. Силика наночестице су добијене неутрализацијом јако базног воденог раствора натријум силиката, док су феритне наночестице синтетисане копреципитацијом из воденог раствора одговарајућих нитратних соли. Да би се омогућила електростатичка депозиција нано-честица, силика језгра су функционализована са 3-аминопропилтриетоксисилан (APTES) или поли(диалилдиметиламонијум хлорид) (PDDA) чиме се повећава изоелектрична тачка силика честица. На овај начин су око силика језгро честица синтетисани једнослојни омотачи на бази SiO2, Fe3O4, ZnFe2O4 или NiFe2O4.<br />Резултати су потврдили да се униформан силика слој може депоновати на функцијонализованим силика честицама. Формиран силика омотач је имао дебљину ~ 30 nm, мезопорозну структуру са средњом величином пора од ~ 8 nm и значајном укупном запремином пора. Због тога су тако добијене силика језгро-омотач наноструктуре погодне за имобилизацију ензима али и неких других активних материја. Такође је потврђено да је оптимална pH вредност за синтезу хомогеног Fe3O4 омотача на нефункционализованим силика језгрима ~ 5,4. Добијени Fe3O4 омотач је суперпа-рамагнетан са температуром блокирања ~ 25 К. Уградња никла и цинка у феритну структуру омотача није било могуће на нижим pH вредностима. Међутим, показано је и да је на вишим pH вредностима велика брзина формирања феритних честица и њихова самоагрегација доминира над конкурентном реакцијом депозиције феритних честица на функционализована силика језгра. У циљу спречавања самоагрегације, депо-зиција ZnFe2O4 и NiFe2O4 наночестица на PDDA-функционализованим силика језгрима је обављена у присуству цитратне киселине на pH &gt; 7. Цитратна киселина пасивизира површину феритних наночестица и на тај начин инхибира самоагрегацију, омогућавајући депозицију ових честица на површину PDDA-функционализованих силика језгара.<br />У овој тези су синтетисане честице са двослојним омотачем, који се састоје од унутрашњег Fe3O4 и спољашњег силика слоја. На PDDA-функцио-нализованим SiO2-језгро/Fe3O4-омотач честицама, обављена је депозиција силика наночестица чиме је формиран спољни мезопорозни силика омотач. Добијене су композитне честице са два различита функционална слоја: унутрашњим који омогућава магнетну сепарацију честице из реакционог медијума и спољним који омогућава имобили-зацију активних материја. Добијени резултати су указали да се ове нанокомпозитне честице могу употребити у биоинжењерству и областима хертерогене катализе.</p> / <p>U ovoj doktorskoj disertaciji prikazani su rezultati sinteza i karakterizacija nano-kompozitnih čestica sa jezgro-omotač strukturom. Nanokompozitne čestice su sintetisane u tečnoj fazi, elektrostatičkom depozicijom in situ sintetisanih SiO2, Fe3O4, ZnFe2O4 ili NiFe2O4 nanočestica na površinu monodisperznih i sferičnih silika jezgro čestica (srednjeg prečnika ~ 0,4 &mu;m). Silika jezgro čestice su sintetisane hidrolizom i kondezacijom TEOS-a u baznoj sredini. Silika nanočestice su dobijene neutralizacijom jako baznog vodenog rastvora natrijum silikata, dok su feritne nanočestice sintetisane koprecipitacijom iz vodenog rastvora odgovarajućih nitratnih soli. Da bi se omogućila elektrostatička depozicija nano-čestica, silika jezgra su funkcionalizovana sa 3-aminopropiltrietoksisilan (APTES) ili poli(dialildimetilamonijum hlorid) (PDDA) čime se povećava izoelektrična tačka silika čestica. Na ovaj način su oko silika jezgro čestica sintetisani jednoslojni omotači na bazi SiO2, Fe3O4, ZnFe2O4 ili NiFe2O4.<br />Rezultati su potvrdili da se uniforman silika sloj može deponovati na funkcijonalizovanim silika česticama. Formiran silika omotač je imao debljinu ~ 30 nm, mezoporoznu strukturu sa srednjom veličinom pora od ~ 8 nm i značajnom ukupnom zapreminom pora. Zbog toga su tako dobijene silika jezgro-omotač nanostrukture pogodne za imobilizaciju enzima ali i nekih drugih aktivnih materija. Takođe je potvrđeno da je optimalna pH vrednost za sintezu homogenog Fe3O4 omotača na nefunkcionalizovanim silika jezgrima ~ 5,4. Dobijeni Fe3O4 omotač je superpa-ramagnetan sa temperaturom blokiranja ~ 25 K. Ugradnja nikla i cinka u feritnu strukturu omotača nije bilo moguće na nižim pH vrednostima. Međutim, pokazano je i da je na višim pH vrednostima velika brzina formiranja feritnih čestica i njihova samoagregacija dominira nad konkurentnom reakcijom depozicije feritnih čestica na funkcionalizovana silika jezgra. U cilju sprečavanja samoagregacije, depo-zicija ZnFe2O4 i NiFe2O4 nanočestica na PDDA-funkcionalizovanim silika jezgrima je obavljena u prisustvu citratne kiseline na pH &gt; 7. Citratna kiselina pasivizira površinu feritnih nanočestica i na taj način inhibira samoagregaciju, omogućavajući depoziciju ovih čestica na površinu PDDA-funkcionalizovanih silika jezgara.<br />U ovoj tezi su sintetisane čestice sa dvoslojnim omotačem, koji se sastoje od unutrašnjeg Fe3O4 i spoljašnjeg silika sloja. Na PDDA-funkcio-nalizovanim SiO2-jezgro/Fe3O4-omotač česticama, obavljena je depozicija silika nanočestica čime je formiran spoljni mezoporozni silika omotač. Dobijene su kompozitne čestice sa dva različita funkcionalna sloja: unutrašnjim koji omogućava magnetnu separaciju čestice iz reakcionog medijuma i spoljnim koji omogućava imobili-zaciju aktivnih materija. Dobijeni rezultati su ukazali da se ove nanokompozitne čestice mogu upotrebiti u bioinženjerstvu i oblastima herterogene katalize.</p> / <p>This thesis presents the results of the synthesis and characterization of the nanocomposite particles with core-shell structure. Nanocomposite particles were synthesized by liquid-phase technique through electrostatic deposition of in situ synthesized SiO2, Fe3O4, ZnFe2O4 or NiFe2O4 nanoparticles on the surface of spherical and monodispersed silica core particles (average size ~ 0.4 &mu;m). Silica core particles were prepared by hydrolysis and condensation of tetraethylorthosilicate in basic conditions. Silica nanoparticles were obtained by neutralization of highly basic sodium silicate solution while ferrite nanoparticles were obtained by coprecipitation from solutions of the corresponding nitrate salts. To improve electrostatic assembling of nanoparticles on the surface of silica core particles, the latter were functionalized with 3-amino-propyltriethoxysilane (APTES) or poly(diallyldimethylammonium chloride) (PDDA) which increases the isoelectric point of the silica core particles. In this way SiO2, Fe3O4 , ZnFe2O4 or NiFe2O4 shells were synthesized around the silica core particles, respectively.<br />The results confirmed that uniform silica layer can be deposited at the functionalized silica core particles. The formed silica layer had thickness of ~ 30 nm, mesoporous structure with average pore size of ~ 8 nm and high total pore volume. This makes silica shell suitable for immobilization of enzymes. Optimal conditions for synthesis of homogenous and thin Fe3O4 shell around non-functionalized silica core particles were found at pH ~ 5.4. Obtained Fe3O4 shell was superparamagnetic with blocking temperature at ~25 К. Incorporation of nickel and zinc into ferrite structure was impossible at lower pH values. However at higher pH the formation rate of Ni- and Zn-ferrite particles becomes very fast and the self-aggregation dominates the competing formation of the ferrite shell around functionalized silica cores. Because of that the self-aggregation was prevented by surface modify-cation of ZnFe2O4 and NiFe2O4 nanoparticles with citric acid before their deposition on the PDDA-functionalized silica core and homogenous and continuous shells were finally obtained at pH &gt; 7.<br />In addition, bilayered shell composed of internal Fe3O4 layer and external SiO2 layer, were also prepared. Silica nanoparticles were deposited on the surface of PDDA-functionalized SiO2-core/Fe3O4-shell particles which induced formation of external mesoporous silica shell. Obtained composite particles had two different functional layers: internal which would allow its magnetic separation from reaction mixture and external which could allow imobilization of various molecules and nanoparticles such as enzymes inside its pores. Based on these results, obtained nanoparticles could be used in bioengineering and heterogenous catalysis.</p>

This thesis work deals with the volume changes during the solidification of cast irons and peritectic steels. The volume changes in casting metals are related to the expansion and/or contraction of the molten metal during solidification. Often, different types of shrinkage, namely macro- and micro-shrinkage, affect the casting quality. In addition to that, exposure of the metal casting to higher contraction or expansion during the solidification might also be related to internal strain development in samples, which eventually leads to surface crack propagation in some types of steel alloys during continuous casting. In consequence, a deep understanding of the mechanisms and control of the solidification will improve casting quality and production. All of the experiments during the entire work were carried out on laboratory scale samples. Displacement changes during solidification were measured with the help of a Linear Variable Displacement Transformer (LVDT). All of the LVDT experiments were performed on samples inside a sand mould. Simultaneously, the cooling curves of the respective samples during solidification were recorded with a thermocouple. By combining the displacement and cooling curves, the volume changes was evaluated and later used to explain the influence of inoculants, carbon and cooling rates on volume shrinkages of the casting. Hypoeutectic grey cast iron (GCI) and nodular cast iron (NCI) with hypo-, hyper- and eutectic carbon compositions were considered in the experiments from cast iron group. High nickel alloy steel (Sandvik Sanbar 64) was also used from peritectic steel type. These materials were melted inside an induction furnace and treated with different types of inoculants before and during pouring in order to modify the composition. Samples that were taken from the LVDT experiments were investigated using a number of different  methods in order to support the observations from the displacement measurements:  Differential Thermal Analysis (DTA), to evaluate the different phase present; Dilatometry, to see the effect of cooling rates on contraction for the various types of alloys; metallographic studies with optical microscopy; Backscattered electrons (BSE) analysis on SEM S-3700N, to investigate the different types of oxide and sulphide nuclei; and bulk density measurements  by applying Archimedes' principle. Furthermore, the experimental volume expansion during solidification was compared with the theoretically calculated values for GCI and NCI. It was found that the casting shows hardly any shrinkage during early solidification in GCI, but in the eutectic region the casting expands until the end of solidification. The measured and the calculated volume changes are close to one another, but the former shows more expansion. The addition of MBZCAS (Si, Ca, Zr, Ba, Mn and Al) promotes more flake graphite, and ASSC (Si, Ca, Sr and Al) does not increase the number of eutectic cells by much. In addition to that, it lowers the primary austenite fraction, promotes more eutectic growth and decreases undercooled graphite and secondary dendritic arm spacing (SDAS). As a result, the volume expansion changes in the eutectic region. The expansion during the eutectic growth increase with an increase in the inoculant weight percentage. At the same time, the eutectic cells become smaller and increase in number. The effect of the inoculant and the superheat temperature shows a variation in the degree of expansion/contraction and the cooling rates for the experiments. Effective inoculation tends to homogenize the eutectic structure, reducing the undercooled and interdendritic graphite throughout the structure. In NCI experiments, it was found that the samples showed no expansion in the transversal direction due to higher micro-shrinkages in the centre, whereas in the longitudinal direction the samples shows expansion until solidification was complete.   The theoretical and measured volume changes agreed with each other. The austenite fraction and number of micro-shrinkage pores decreased with increase in carbon content. The nodule count and distribution changes with carbon content. The thermal contraction of NCI is not influenced by the variation in carbon content at lower cooling rates. The structural analysis and solidification simulation results for NCI show that the nodule size and count distribution along the cross-sections at various locations are different due to the variation in cooling rates and carbon concentration. Finer nodule graphite appears in the thinner sections and close to the mold walls. A coarser structure is distributed mostly in the last solidified location. The simulation result indicates that finer nodules are associated with higher cooling rate and a lower degree of microsegregation, whereas the coarser nodules are related to lower cooling rate and a higher degree of microsegregation. As a result, this structural variation influences the micro-shrinkage in different parts. The displacement change measurements show that the peritectic steel expands and/or contracts during the solidification. The primary austenite precipitation during the solidification in the metastable region is accompanied by gradual expansion on the casting sides. Primary δ-ferrite precipitation under stable phase diagram is complemented by a severe contraction during solidification. The microstructural analysis reveals that the only difference between the samples is grain refinement with Ti addition. Moreover, the severe contraction in solidification region might be the source for the crack formation due to strain development, and further theoretical analysis is required in the future to verify this observation. / <p>QC 20170228</p>

In this age of wireless technology, Body Area networks (BAN) is revolutionising the concept of patient care and health monitoring. BAN provides people good assessment of their health status at any time, wherever they are physically. The increased interest in developing effective body (in, on &amp; off) communication systems made phantoms which can mimic the electrical properties of an actual human body necessary. Wearable antennas which are the indispensable part of BAN got to be low pro file and above all influences that human body can make. There should also be a way to reduce the effect of antennas on human body namely specific absorption rate (SAR). In this work effort has been made to develop phantoms suitable for both On body and In body communications. The base materials which are selected for the study are of biological origin (bio ceramics and biopolymers) whose behaviour is closer to that of human tissues. As these phantoms are biocompatible they are essentially non toxic where the conventionally available phantoms are toxic in nature. Different kinds of low profile conformal wearable antennas working at 2.4GHz ISM band were developed and studied in the BAN perspective. Antennas suffer much in terms of matching and efficiency when they are in contact or in the premises of human body. This is a major hurdle in the way to setting up a good body communication network. This work encompasses various techniques adopted to limit the body interferences to an acceptable level. The techniques adopted (Such as Backing Ground Plane, High Impedance Surface &amp; Polymeric Ferrite Sheets) proved to be effective in reducing the sway in antenna characteristics when they are mounted on body. Specific absorption rate is also brought to acceptable levels and thus avoiding the formation of hot spots due to microwave absorption. A safer and cost effective BAN can be set up using this work which will lead to a safer, mobile and healthy future. / Les réseaux BAN (Body Area Network) révolutionnent le concept de la surveillance et de la prise en charge à distance de la santé du patient. Le BAN fournit des informations sur l’état de santé du patient en temps réel quelque soit l’endroit où il se trouve. Dans le « télé monitoring », des capteurs de mouvement, de respiration ou du rythme cardiaque placés à l’intérieur ou sur le corps humain transmettent des données via le réseau sans fil constituant le BAN, une antenne étant associée à chaque nœud du réseau. La communication peut être in/on, on/on ou on/off selon que les antennes sont placées à l’intérieur, sur ou à l’extérieur du corps. Le développement des BAN nécessite la réalisation de modèles (ou fantômes) simulant au mieux les propriétés électromagnétiques du corps humain. Des antennes portables, miniaturisées doivent être réalisées avec des contraintes d’intégration d’une part (aux vêtements, à des objets type montre ou badge), des contraintes de résistance ou de prise en compte de l’influence du corps d’autre part. La réduction de l’impact des antennes sur les tissus en terme de SAR (Specific Absorption Rate) doit également être considérée. Dans ce travail, l’objectif est de développer des fantômes valables pour les communications dans et sur le corps. Les matériaux de base sélectionnés sont d’origine biologique (biocéramiques et biopolymères) avec des propriétés proches de celles des tissus humains. Ces fantômes étant biocompatibles, ils sont essentiellement non toxiques alors que les fantômes usuels le sont en général. D’autre part, différents types d’antennes conformables, fonctionnant dans la bande ISM 2.4 GHz ont été développées et étudiées dans la perspective du BAN. Les antennes voient leur adaptation et leur efficacité chuter au contact ou à proximité du corps, ce qui constitue un écueil majeur pour établir une bonne communication. Différentes méthodes permettant de réduire l’influence du corps (plan de masse à l’arrière, surface haute impédance, feuille de ferrite polymère) sont testés et leurs avantages et inconvénients développés. Des mesures de SAR permettent aussi de démontrer l’efficacité de ces méthodes sur la réduction de la puissance absorbée par les tissus. Au final, ce travail apporte une contribution à l’étude théorique et expérimentale de l’interaction entre corps humain et antenne dans le cadre des réseaux BAN appliqués à la télésurveillance de la santé.

Submitted by Samira Prince (prince@ufpa.br) on 2012-09-26T14:39:27Z No. of bitstreams: 2 license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) Tese_SuperficiesEletromagneticasMicroondas.pdf: 1321427 bytes, checksum: 32abfb3810d0b4ac8c23d53ce7e3a5bf (MD5) / Approved for entry into archive by Ana Rosa Silva(arosa@ufpa.br) on 2012-10-01T12:24:22Z (GMT) No. of bitstreams: 2 license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) Tese_SuperficiesEletromagneticasMicroondas.pdf: 1321427 bytes, checksum: 32abfb3810d0b4ac8c23d53ce7e3a5bf (MD5) / Made available in DSpace on 2012-10-01T12:24:22Z (GMT). No. of bitstreams: 2 license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) Tese_SuperficiesEletromagneticasMicroondas.pdf: 1321427 bytes, checksum: 32abfb3810d0b4ac8c23d53ce7e3a5bf (MD5) Previous issue date: 2012 / CAPES - Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Neste trabalho foram investigadas (FSSs) com ressonância de alto fator de qualidade (fator Q) e independência da polarização para uma onda plana com incidência normal. Estas FSSs são baseadas em um arranjo planar de metalizações sobre um substrato. Um alto fator Q é obtido por meio da excitação do trapped-mode e a independência da polarização, por meio da alta simetria rotacional dos elementos que compõe o arranjo. Para o projeto de FSSs com controle do regime de trapped-mode, foram utilizados substratos feitos de materiais com possibilidade de controle de suas propriedades elétricas ou magnéticas (ferrite magnetizada ou silício ativado oticamente). O arranjo de dois anéis concêntricos em um substrato dielétrico analisado neste trabalho apresenta uma ressonância de trapped-mode com fator Q em torno de 12 e transmitância máxima de 70 %. Com a utilização de um substrato de ferrite magnetizada nesse arranjo, é mostrado que é possível deslocar a frequência de ressonância do trappedmode em torno de 20 %, sem degradação significativa da ressonância de transmisão. Com o emprego de um substrato de silício ativado opticamente, é demonstrado que é possível realizar um chaveamento praticamente completo da banda de transmissão desse arranjo. Para realização das simulações computacionais foram utilizados o método dos momentos no domínio espectral (SDMM) e os programas comerciais Ansoft Designer 5 Planar EM e CST 2009. / In this work frequency selective surfaces (FSSs) with high quality factor (Q-factor) resonance and polarization independence for a normally incident plane wave were investigated. These FSSs are based on a planar array of metallization on a substrate. A high Q-factor is obtained by excitation of trapped-mode and polarization independence by means of high rotational symmetry of the elements that compose the array. For the design of FSSs with trapped-mode regime control, substrates made of materials with the possibility of controlling their electric or magnetic properties (magnetized ferrite or optically activated silicon) were used. The two concentric rings array on a dielectric substrate analyzed in this work presents a trapped-mode resonance with a Q-factor around 12 and maximum transmittance of 70 %. With the utilization of a magnetized ferrite substrate in this array, it is shown that we can shift the resonance frequency of the trappedmode around 20 % without significant degradation of the transmission resonance. With the use of an optically activated silicon substrate, it is demonstrated the possibility of an almost complete switching of the transmission band in that array. To perform the computer simulations the spectral domain moment method (SDMM) and the commercial programs Ansoft Designer 5 PlanarEM and CST 2009 were used.

Nous explorons les propriétés structurales de nanoparticules cœur-coquille, avec un cœur de ferrite MFe2O4 (M = Mn et Co) ou de ferrite mixte Mn-Zn. Ces nanoparticules sont obtenues par co-précipitation hydrothermique et sont dispersées en milieu acide par un traitement de surface empirique au nitrate ferrique, protégeant les nanograins contre une dissociation chimique par une fine couche superficielle de maghémite. La fraction volumique du cœur, de la coquille et l’épaisseur de la couche superficielle sont déterminées par dosage chimique. Nous suivons les changements structurels des nanocristaux de MnFe2O4 et CoFe2O4, pendant la durée du traitement de surface, tandis que ceux des nanoparticules de ferrite mixte Mn-Zn sont étudiés en fonction de leur teneur en zinc. Diffraction de rayons-x et de neutrons sont utilisées pour déterminer les paramètres de structure, en particulier la diffusion de cations dans les interstices de la ferrite spinelle. Pour un haut degré de fiabilité, des raffinements de Rietveld sont réalisés. Les distances inter-atomiques, l’état d’oxydation moyen et le degré d’inversion sont déterminés par spectroscopie d’absorption des rayons-x. Morphologie, cristallinité et taille des nanoparticules de ferrite mixte Mn-Zn sont étudiées par TEM/HRTEM et par diffraction des électrons. Dans les nanoparticules MnFe2O4 et de ferrite mixte Mn-Zn, on constate la présence de cations Mn3+ en environnement octaédrique, responsables de déformations anisotropes (effet Jahn-Teller). Le degré d’inversion obtenu ici diffère de celui du bulk en raison de la réduction à l’échelle nanométrique et de l'augmentation du rapport surface/volume pendant le processus de synthèse. / Structural properties of core-shell ferrite nanoparticles MFe2O4 (M = Mn and Co) and Mn-Zn ferrite nanoparticles are here investigated. The nanoparticles are synthesized by hydrothermal co-precipitation and are dispersed in acid medium thanks to an empirical surface treatment by ferric nitrate, which prevents the chemical dissociation by a thin maghemite layer incorporated at the surface of the nano-grains. Chemical titrations allow us to calculate volume fractions of core and shell, as well as the surface-layer thickness. Structural changes induced by the surface treatment are followed as a function of treatment duration in MnFe2O4 and CoFe2O4 nanocrystals. Whereas structural changes in Mn-Zn ferrite nanoparticles are investigated as a function of zinc content. X-ray and Neutron diffractions are used to determine the structural parameters, in particular cationic distribution in the spinel ferrite sites. Precise structural information with high degree of reliability is obtained by Rietveld refinements. To investigate the local structure of these materials, X-ray Absorption Spectroscopy measurements are performed, allowing determining interatomic distances, mean oxidation state and inversion degree. Morphology, crystallinity and size of mixed-ferrite nanoparticles are investigated by TEM/HRTEM and electron diffraction. In Mn-Zn ferrite nanoparticles, the presence of Mn3+ in octahedral environment is responsible for anisotropic distortions, known as Jahn-Teller effect. The inversion degree obtained in this work diverges from the bulk values due to the reduction to nanoscale and to the increase of the surface/volume ratio, associated to the synthesis process.

Multiferroic materials exhibit unique properties such as simultaneous existence of two or more of coupled ferroic order parameters (ferromagnetism, ferroelectricity, ferroelasticity or their anti-ferroic counterparts) in a single material. Recent years have seen a huge research interest in multiferroic materials for their potential application as high density non-volatile memory devices. However, the scarcity of these materials in single phase and the weak coupling of their ferroic components have directed the research towards multiferroic heterostructures. These systems operate by coupling the magnetic and electric properties of two materials, generally a ferromagnetic material and a ferroelectric material via strain. In this work, horizontal heterostructures of composite multiferroic materials were grown and characterized using pulsed laser ablation technique. Alternate magnetic and ferroelectric layers of cobalt ferrite and lead zirconium titanate, respectively, were fabricated and the coupling effect was studied by X-ray stress analysis. It was observed that the interfacial stress played an important role in the coupling effect between the phases. Doped zinc oxide (ZnO) heterostructures were also studied where the ferromagnetic phase was a layer of manganese doped ZnO and the ferroelectric phase was a layer of vanadium doped ZnO. For the first time, a clear evidence of possible room temperature magneto-elastic coupling was observed in these heterostructures. This work provides new insight into the stress mediated coupling mechanisms in composite multiferroics.

Non-metallic inclusions in steels are generally considered to be detrimental for mechanical properties. However, it has been recognized that certain inclusions, such as Ti-oxide and TiN, can serve as potent nucleation sites for the formation of intragranular ferrite (IGF) in low-alloy steels. The formation of IGF could improve the toughness of the coarse grained heat affected zone (CGHAZ) of weld metals. Thus, the present thesis mainly focuses on the effect of size of nucleation sites on the IGF formation. Quantitative studies on the composition, size distribution and nucleation probability for each size of the inclusions as well as the area fraction, starting temperature and morphology of an IGF have been carried out. In the present work, the Ti-oxide and TiN powders were mixed with metallic powders. The mixed powders were heated up to the liquid state and cooled with a slow cooling rate of 3.6 ºC/min. These as-cast steels with Ti-oxide and TiN additions were used to simulate the IGF formation in the CGHAZ of weld metals. Specifically, the inclusion and microstructure characteristics in as-cast steels have been investigated. The results show that the nucleant inclusion was identified as a TiOx+MnS phase in steels with Ti2O3 additions and as a TiN+Mn-Al-Si-Ti-O+MnS phase in steels with TiN additions. In addition, the TiOx and TiN phases are detected to be the effective nucleation sites for IGF formation. It is clearly shown that an increased inclusion size leads to an increased probability of IGF nucleation. This probability of IGF nucleation for each inclusion size of the TiOx+MnS inclusions is clearly higher than that of the complex TiN+Mn-Al-Si-Ti-O+MnS inclusions. In addition, the area fraction of IGF in the steels with Ti2O3 additions is larger than that of the steels with TiN additions. This result agrees with the predicted tendency of the probability of IGF nucleation for each inclusion size in the steels with Ti2O3 and TiN additions. In order to predict the effective inclusion size for IGF formation, the critical diameters of the TiO, TiN and VN inclusions, which acted as the nucleation sites of IGF formation, were also calculated based on the classical nucleation theory. The critical diameters of TiO, TiN and VN inclusions for IGF formation were found to be 0.192, 0.355 and 0.810 μm in the present steels. The calculation results were found to be in agreement with the experiment data of an effective inclusion size. Moreover, the effects of the S, Mn and C contents on the critical diameters of inclusions were also calculated. It was found that the critical diameter of the TiO, TiN and VN inclusions increases with an increased content of Mn or C. However, the S content doesn’t have a direct effect on the critical diameter of the inclusions for IGF formation. The probability of IGF nucleation for each inclusion size slightly decreases in the steel containing a higher S content. This fact is due to that an increased amount of MnS precipitation covers the nucleant inclusion surface. In the as-cast experiment, it was noted that an IGF can be formed in steels with Ti2O3 and TiN additions with a cooling rate of 3.6 ºC/min. In order to control the microstructure characteristics, such as the area fraction and the morphology of an IGF, and to investigate the starting temperature of IGF and grain boundary ferrite (GBF) formation, the dynamic transformation behavior of IGF and GBF was studied in-situ by a high temperature confocal laser scanning microscope (CLSM). Furthermore, the chemical compositions of the inclusions and the morphology of IGF after the in-situ observations were investigated by using scanning electron microscopy (SEM), electron backscatter diffraction (EBSD) and electron probe microanalysis (EPMA) which equipped wavelength dispersive spectrometer (WDS). The results show that the area fraction of IGF is larger in the steels with Ti2O3 additions compared to the steels with TiN additions, after the same thermal cycle has been imposed. This is due to that the TiOx phase provides more potent nucleation sites for IGF than the TiN phase does. Also, the area fraction of IGF in the steels is highest after at an intermediate cooling rate of 70 ºC/min, since the competing phase transformations are avoided. This fact has been detected by using a hybrid methodology in combination with CLSM and differential scanning calorimetry (DSC). In addition, it is noted that the morphology of an IGF is refined with an increased cooling rate. / <p>QC 20150325</p>

The concept for a novel new antenna design is presented and investigated for application to ground penetrating radar (GPR). The proposed new antenna design is called the shielded magnetic bowtie antenna (MBA). As the name suggests, it is predominately constructed from a bowtie-shaped volume of magnetic material that is fed from the centre of the structure by a small magnetic loop antenna. This thesis develops the magnetic antenna concept and investigates its potential for GPR predominately through numerical modelling. However, a significant part of the investigation concentrates on validating the numerical modelling technique developed to study the shielded MBA by comparing the results with measurements obtained from a scale model constructed to operate in the watertank antenna test facility, a controlled environment for GPR antenna research. The broadband properties required for GPR antennas are achieved uniquely with the shielded MBA design by a combination of the antenna shape being defined in terms of angles and an inherent magnetic loss mechanism within the antenna material structure. The design also affords an intrinsically placed antenna shield that has the potential for mitigating problems typically experienced with shielding electric dipole antennas. Antenna shielding is an important consideration for GPR antenna designers, especially given the recent US government (FCC) changes that restrict radiated energy emissions within the regulated spectrum used by GPR systems. In addition to providing the intended directional radiation properties, the magnetic antenna shield also provides an elegant solution for a low-loss wideband balun, allowing the antenna to be effectively fed from an unbalanced coaxial transmission line. Other important aspects of the proposed design are discussed in relation to the requirements for GPR antennas. Numerical models of the magnetic antenna concept show encouraging bandwidth results. For example, from a simple comparison with an equivalent sized electric bowtie antenna model, the effective gain bandwidth of the magnetic antenna is found to be at least 3-octaves compared to approximately 2-octaves for the electric bowtie. The shielded magnetic antenna achieves a gain of approximately 2 dB, compared to 5 dB for the unshielded electric bowtie antenna. However, it is noted that the magnetic antenna models contain significantly more loss compared to the electric bowtie model. The shielded MBA design emerged from a theoretical investigation of electrically small GPR antennas, given that the initial thesis objective was to investigate ways of improving low frequency GPR antennas. In general, GPR systems are operated with electric dipole antennas, such as the electric bowtie. Interestingly, the electrically small antenna investigation revealed that only the small magnetic loop (i.e., magnetic dipole) antenna can be constructed to approach, arbitrarily closely, the fundamental bandwidth limit for small antennas. This surprising and counter intuitive result is shown to be theoretically achievable with the use of magnetic materials. For the small loop antenna, energy stored within the antenna structure can be avoided by filling the antenna sphere with a perfect magnetic material. This theoretical argument is discussed and supported by numerically modelled results. The electrically small antenna investigation presented in this thesis extends to include the influence that proximity to a lossy dielectric half-space has, on improving the antenna impedance bandwidth. This investigation is of general interest for GPR; it is performed numerically and supported by measurements conducted on an experimental loop antenna situated at various heights above the ground. These results provide support for the hypothesis that a magnetic antenna may experience less influence from near-field changes in the dielectric properties of the ground compared to the equivalent sized electric field antenna.