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Study on conduction mechanismes of mediun voltage cable XLPE insulation in the melting range of temperatures.Orrit Prat, Jordi 07 March 2012 (has links)
D’ençà que el polietilè reticulat (XLPE) es va començar a utilitzar com aïllament elèctric per cables de subministrament elèctric, s’han destinat molts esforços a l’estudi de les propietats dielèctriques del polietilè i l’efecte que la càrrega d’espai té sobre el seu comportament. En aquest sentit, les corrents de despolarització estimulades tèrmicament (TSDC) s’han utilitzat extensament per estudiar les relaxacions de càrrega d’espai. Aquesta tècnica ha demostrat tenir prou resolució per distingir diferències en aïllaments de XLPE amb composicions o processos de fabricació diferents. En aquesta tesi, els mecanismes de conducció dels aïllaments XLPE de cables de mitjana tensió (MV) han estat estudiats per TSDC i diverses tècniques complementàries, com l’anàlisi dinàmica elèctrica (DEA), les corrents d’absorció/resorció (ARC), el pols electroacústic (PEA) i les corrents de despolarització isotèrmiques (IDC). Altres tècniques, com l’espectroscòpia d’infrarojos (FTIR) o la difracció de raigs X, han estat també utilitzades per caracteritzar el material. S’han obtingut espectres TSDC per diferents mostres de cable, les quals en condicions de servei treballen en un rang de tensió AC de 12 a 20kV i a temperatures al voltant dels 90ºC. D’altra banda, s’han realitzat mesures de la conductivitat per ARC i DEA en mostres de cable, en cilindres de XLPE i en films. Les mesures s’han dut a terme a temperatures pertanyents al rang de fusió del XLPE (50–110ºC), en mostres sotmeses a aquestes temperatures durant diferents períodes de temps. Els resultats mostren diferències importants entre el comportament de les propietats conductives de les mostres de cable amb pantalles semiconductores (SC) i sense (cilindres de XLPE). El comportament observat ha estat explicat mitjançant la coexistència de dos mecanismes de conducció. La difusió d’impureses des de les pantalles SC determina el comportament d’una d’aquestes contribucions a mig i llarg termini. Els resultats obtinguts per FTIR són consistents amb aquest model. Respecte la microestructura, tant les mesures DSC com la difracció per raigs X mostren que existeixen processos de recristal•lització quan les mostres són sotmeses a temperatures ubicades dins del rang de fusió. Els electrets formats mitjançant el mètode de la polarització per finestres (WP) mostren una descàrrega TSDC amb un ample pic heteropolar en el rang de fusió, amb el màxim al voltant dels 105ºC. En treballs previs, aquest pic es va associar a la fusió de la fracció cristal•lina. Tanmateix, en lloc de decréixer quan la temperatura de polarització augmenta, el pic presenta una temperatura de polarització òptima al voltant de 90-95ºC. Aquest comportament ha estat explicat tenint en compte els processos de recristal•lització que es produeixen quan el material es polaritza isotèrmicament. Durant la recristal•lització, una nova fracció cristal•lina creix en un estat polaritzat degut el camp aplicat, i origina una corrent de despolarització quan es fon durant la mesura TSDC. Amb l’objectiu de determinar l’origen d’altres pics que apareixen en l’espectre TSDC del XLPE, s’han emprat les IDC com a tècnica complementària. Les corrents IDC obtingudes de mostres no tractades es poden representar com la combinació de dues contribucions diferenciades: un terme que és una funció potencial del temps i un d’exponencial. La segona relaxació es correspon amb un pic TSDC que apareix a 95ºC. D’aquesta manera s’ha pogut determinar l’origen dipolar del pic. Finalment, mitjançant la tècnica PEA s’ha obtingut la distribució de la càrrega d’espai en mostres polaritzades que havien estat sotmeses a diferents tractaments tèrmics. S’ha observat un comportament transitori tant per PEA com per TSDC. Tanmateix no s’ha pogut establir cap relació directa entre les descàrregues TSDC i mesures PEA. En conseqüència, s’ha proposat una explicació per les corbes TSDC que considera mecanismes que no són detectables en els perfils de càrrega obtinguts per PEA / Since cross-linked polyethylene (XLPE) started to be used as electrical insulation for power cables, much research has been focused on polyethylene dielectric properties and the effect of the space charge on its behavior. In this sense, thermally stimulated depolarization currents (TSDC) have been widely used to study space charge relaxation. This technique has proved to have enough resolution to determine differences in charge trapping properties among XLPE insulations with different composition and manufacturing processes. In this thesis work, the conduction mechanisms of medium voltage (MV) cable XLPE insulation have been studied by TSDC and several complementary techniques, such as dynamic electrical analysis (DEA), absorption/resorption currents (ARC), pulsed electroacoustic (PEA) and isothermal depolarization currents (IDC). Other techniques, like Fourier transform infrared (FTIR) spectroscopy or X-ray diffractometry, have been used to characterize the material. TSDC spectra have been obtained for different cable samples, which in service conditions work under AC voltages ranging from 12 to 20kV and at temperatures around 90ºC. On the other hand, conductivity measurements by ARC and DEA have been performed in cable samples and in XLPE cylinders, as well as XLPE films. Measurements have been carried out at temperatures within the melting temperature range of XLPE (50–110ºC) on samples annealed at such temperatures during several annealing times. Results show significant differences in the behavior of the conductive properties of XLPE cable samples with semiconducting (SC) screens and without them (XLPE cylinders). The observed behavior has been explained by the coexistence of two conduction mechanisms. Diffusion of impurities from SC screens determines the medium and long-term behavior of one of these contributions and, hence, of cable conductivity. FTIR results are consistent with this model. With respect to microstructure, DSC and X-ray diffractometry results show that recrystallization processes exist when samples are annealed in the melting range of temperatures. Electrets formed by means of the windowing polarization method (WP) showed a TSDC discharge with a wide heteropolar peak in the melting temperature range, and with the maximum at about 105ºC. This peak was associated with the melting of the crystalline fraction in previous works. However, in spite of decreasing with the temperature of polarization, an optimal polarization temperature around 90–95ºC is found. This behavior has been explained by taking into account recrystallization processes when the insulation is isothermally polarized. During recrystallization, the new crystalline fraction grows in a polarized state due to the applied electric field, and it causes the depolarization current when it melts during the TSDC measurement. Results obtained from different experiments are consistent with this assumption. With the aim to find out the origin of other TSDC peaks present in the spectrum of XLPE cable samples, IDC has been used as complementary technique. IDC currents obtained from as-received cable samples at temperatures close to service conditions can be considered as the combination of two different contributions: a power law current and a stretched exponential contribution. The last relaxation process has been successfully associated with with a TSDC peak found at 95ºC. By this way the dipolar origin of the peak has been determined. Finally, PEA measurements have provided the space charge distribution profiles of polarized samples with different annealings. A transient behavior has been observed in both PEA and TSDC measurements. However, no straightforward relation between TSDC discharges and space charge detected by PEA can be established. Therefore, an explanation for TSDC curves has been proposed, which considers mechanisms that are not noticeable in charge profiles obtained by PEA.
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Imagerie polarimétrique de speckle statique pour l’étude de matériaux et dynamique pour la détection de micro-vascularisation tumorale / Static speckle polarimetric imaging for material study, and dynamic for the detection of tumoral micro-vascularlzationDupont, Jan 03 February 2017 (has links)
Lors de la diffusion d’une onde électromagnétique sur une surface de rugosité aléatoire ou dans un volume, un champ de speckle, dont les caractéristiques dépendent du diffuseur considéré, se forme. Les diffusions au sein de matériaux impactent l’état de polarisation d’une lumière incidente. Ainsi, la polarisation est un paramètre sensible pour la caractérisation et l’étude de matériaux. Une technique de polarimétrie résolue spatialement, permettant une mesure de précision en champs de speckle, est proposée. Cette technique est utilisée pour étudier l’impact de différents paramètres d’imagerie sur la mesure polarimétrique, notamment les phénomènes de dépolarisation des champs dus au mode d’observation. Un modèle de simulation de champs de speckle polarisés, validé par comparaison avec l'expérimentation pour différents régimes de diffusions, est développé. Par ailleurs, les propriétés dynamiques de l’échantillon peuvent être mesurées par une analyse de contraste du speckle qu’il diffuse. Un dispositif d’imagerie de micro-vascularisation par mesure de contraste de speckle dynamique polarisé est optimisé, puis appliqué à l’étude in-vivo de l’angiogenèse tumorale du mélanome murin, ainsi que l’évolution de la vascularisation après traitement des tumeurs par électrochimiothérapie. Le potentiel de la technique pour la détection et l'étude du mélanome murin, sans contact ni marqueur, est démontré, avec comme perspective la détection et l'étude du mélanome humain, dont l'efficacité reste à être caractérisée pour une utilisation en imagerie biomédicale. / When an electromagnetic wave is scattered by a rough surface or in a volume, a speckle field is observed, with characterlstlcs depending on the consldered scatterer. Multiple scattering in samples immpact the State of polarizatlon of an incident light. Thus, polarization Is a sensitive parameter for material characterization and study. A spatially resolved polarlmetry method, allowing accurate measurements in speckle fields is proposed. That method is used to study the Impact of various parameters on polarimétrie measurements, especially the depolarization phenomenon due to the observation setup. A polarlzed speskle simulation model is proposed, validated by comparison with expérimentation for various scattering régime. Besides, dynamlc properties of samples can be measured by an analysis of the scattered speckle contrast. A method allowing microvascularization imaging based on dynamic polarized light scattering imaging is optlmlzed, then applied to in-vivo study of the tumor angiogenesis occuring on murine melanoma, as well as the vascularization évolution after a treatment called electrochemotherapy. Potentlal of the method for non invasive détection and study of the murine melanoma is demonstrated, its efflciency on human melanoma for biomédical applications remaning to be characterized.
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Detection of carious lesions utilizing depolarization imaging by polarization sensitive optical coherence tomographyGolde, Jonas, Tetschke, Florian, Walther, Julia, Rosenauer, Tobias, Hempel, Franz, Hannig, Christian, Koch, Edmund, Kirsten, Lars 27 August 2020 (has links)
As dental caries is one of the most common diseases, the early and noninvasive detection of carious lesions plays an important role in public health care. Optical coherence tomography (OCT) with its ability of depth-resolved, high-resolution, noninvasive, fast imaging has been previously recognized as a promising tool in dentistry. Additionally, polarization sensitive imaging provides quantitative measures on the birefringent tissue properties and can be utilized for imaging dental tissue, especially enamel and dentin. By imaging three exemplary tooth samples ex vivo with proximal white spot, brown spot, and cavity, we show that the combination of polarization sensitive OCT and the degree of polarization uniformity (DOPU) algorithm is a promising approach for the detection of proximal carious lesions due to the depolarization contrast of demineralized tissue. Furthermore, we investigate different sizes of the DOPU evaluation kernel on the resulting contrast and conclude a suitable value for this application. We propose that DOPU provides an easy to interpret image representation and appropriate contrast for possible future screening applications in early caries diagnostics.
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Model fibrilace síní / Atrial fibrillation modelŘedina, Richard January 2021 (has links)
The aim of this master thesis is to create a 3D electroanatomical model of a heart atria, which would be able to perform atrial fibrillation. To control the model, the differential equations of the FitzHugh-Nagumo model were chosen. These equations describe the change of voltage on the cell membrane. The equations have established parameters. The modification of them leads to changes in the behavior of the model. The simulations were performed in the COMSOL Multiphysics environment. In the first step, the simulations were performed on 2D models. Simulations of healthy heart, atrial flutter and atrial fibrillation were created. The acquired knowledge served as a basis for the creation of a 3D model on which atrial fibrillation was simulated on the basis of ectopic activity and reentry mechanism. Convincing results were obtained in accordance with the used literature. The advantages of computational modeling are its availability, zero ethical burden and the ability to simulate even rarer arrhythmias. The disadvantage of the procedure is the need to compromise between accuracy and computational complexity of simulations.
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Studium dielektrické relaxace v základních materiálech DPS a v izolacích kabelů / Study of dielectric relaxation in PCB substrates and cable insulationJežík, Jan January 2011 (has links)
This study investigates relaxation polarization in some dielectric components of tester UNISPOT S40 developed by company UNITES Systems a.s. Relaxation polarization in the PCB substrates and in tester’s cable insulation causes undesirable deceleration of some test steps. Relaxation polarization in selected PCB substrates and various cables are examined by method of dielectric relaxation spectroscopy in the frequency domain and by measurement of polarization or depolarization current.
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Měření parametrů piezoelektrických aktivních prvků snímačů akustické emise / Measurement of Parameters of Piezoelectric Active Elements for Acoustic Emission SensorsFialka, Jiří January 2015 (has links)
The doctoral thesis discusses the measurement of parameters of piezoelectric (PZT) materials and the influence of temperature on their stability. In the introductory sections, the author briefly explains the piezoelectric effect and its use; simultaneously, methods for the preparation of piezoelectric materials and the measurement of their properties are presented to illustrate the analyzed problem. The experimental part of the thesis describes the procedure of measuring and calculating the complete matrix of material coefficients from samples of PZT ceramics. The applied set of piezoelectric samples complying with relevant European and world standards was made in the form of thin plates, thin discs and cylinders, via gradual modification of the large disc. The NCE51 and/or the older PCM51 ceramics obtained from the company Noliac Ceramics were used in determining the complete matrix and describing the measurement method. Both these types are soft piezoceramics composed from a solid solution of lead zirconate and lead titanate with the general chemical formula of Pb(Zr1-x,Tix)O3. The real crystallographic structure and chemical composition of the samples were confirmed by X-ray diffraction spectroscopy and energy dispersive spectroscopy (EDS), respectively. The frequency method was used for the measurement and calculation of all material coefficients. An Agilent 4294A impedance analyzer and a set of measuring tweezers marketed as “Tweezers Contact Test Fixture 16334A” were used in the process. Fast determination of the entire matrix of coefficients without any special requirement for the preparation of the samples to be measured was tested and verified. The charge coefficients of the piezoelectric material were confirmed by direct methods including the laser interferometer technique, the vibrometric method, and the procedure utilizing changes of the force applied to the sample. The advantages and disadvantages of the methods were compared and defined based on measurements and their results. The main part of thesis was focused on the behavior of piezoelectric material at high temperatures near the Curie point. Depolarization performed by means of a high temperature approaching the Curie point constitutes a significant yet hardly measurable material property of PZT ceramics. Commonly available vibrometric methods (d33-meters) do not appear to be suitable for the measurement of temperature dependencies, and for that reason the frequency technique was used. The piezoelectric charge coefficient, whose value can be effectively measured via the above-discussed frequency method, was selected as the indicator showing the depolarization state in the applied piezoelectric ceramics. The accuracy of the procedure was verified via comparison of the vibrometric method in cylinders of the NCE51 ceramics with different sizes, which are designed for the longitudinal length mode. The result is an optimized measurement methodology which facilitates accurate determination of the Curie temperature, namely phase transition to the cubic crystallographic structure. The experiment also proved the applicability of progressive, controlled depolarization of PZT ceramics via high temperature, and it also enabled us to define the temperature limits at which there occur irreversible changes of the piezoelectric properties of piezoceramics. In the measured NCE51 and PCM51 materials, the limit for the irreversible changes was equal to 95% of the Curie temperature.
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Estudos das propriedades estruturais e ópticas de vidros teluritos / Studies of the structural and optical properties of the tellurite glassesGiehl, Júlia Maria 25 February 2011 (has links)
Vidros teluritos são considerados fortes candidatos para aplicações em lasers e óptica não linear devido a importantes características, como o elevado índice de refração, baixa energia de fônons, baixa temperatura de transição vítrea e sua fácil preparação. Neste trabalho foram produzidas amostras dos sistemas vítreos TeO2- ZnO-Na2O, TeO2-Nb2O5-Na2O e Te2O-Na2O incluindo ou não dopagens de AgNO3 para estudos estruturais e ópticos. As propriedades estruturais e os mecanismos de recombinação destes vidros foram estudados por meio das técnicas de ressonância paramagnética eletrônica, termoluminescência e correntes de despolarização termicamente estimuladas. Já as propriedades ópticas como o coeficiente de absorção linear, índice de refração linear e não linear foram estudadas por meio das técnicas de absorção óptica, acoplamento de prismas e varredura Z. Foram ainda desenvolvidos estudos da precipitação de nanopartículas de prata para o sistema TeO2-ZnO-Na2O com dopagens de AgNO3 com diferentes temperaturas de tratamento térmico. A caracterização das nanopartículas metálicas foi realizada por meio da técnica de absorção óptica auxiliada por microscopia eletrônica de transmissão e espectrometria de energia dispersiva. Foram observadas por ressonância paramagnética eletrônica quatro respostas paramagnéticas dos vidros irradiados com raio , sendo uma de natureza desconhecida e as outras três identificadas como g¹, g² e g³ atribuídas respectivamente ao centro de buraco do telúrio e do oxigênio, centro de buraco do oxigênio terminal e centro de elétron do telúrio. Foi proposto ainda um modelo para explicar os mecanismos de formação destes centros. A partir dos resultados de termoluminescência observou-se que os processos de recombinação destes centros de defeitos são não radioativos. Neste projeto foram estudados pela primeira vez na literatura os fenômenos de polarização e despolarização em vidros teluritos, com e sem irradiação gama, por meio da técnica de correntes de despolarização termicamente estimuladas. Quanto às propriedades ópticas, foi investigada a influência da adição de prata dos sistemas vítreos TeO2-ZnO-Na2O e TeO2-Nb2O5-Na2O em relação à energia do gap, a cauda de Urbach, índice de refração linear e não linear.Nos resultados de varredura Z do sistema vítreo TeO2-Nb2O5-Na2O foi observado o aumento da assimetria na curva com aumento da adição de AgNO3 Este fenômeno foi explicado por meio de uma adaptação do modelo de Sumi para processos não radiativos, responsáveis pelo aumento do caráter térmico do índice de refração não linear. Por fim um modelo foi criado para explicar a precipitação de nanopartículas de prata na matriz vítrea TeO2-ZnO-Na2O mediante tratamento térmico. / Tellurite glasses are considered powerful candidates for applications in lasers and nonlinear optics due to their important properties such as high refractive index, low phonon energy, relatively low glass transition temperature and easy glass production at room atmosphere. In this work glass samples of the systems ZnO-Na2O, TeO2-Nb2O5-Na2O and Te2O-Na2O were produced, including or not the AgNO3 doping for the structural and optical study purposes. The structural properties and the recombination mechanisms of these glasses were studied by means of the techniques of electron paramagnetic resonance, thermoluminescence and thermally stimulated depolarization currents. The optical properties such as the optical linear absorption coefficient, linear and nonlinear refractive index were studied by means of the optical absorption techniques, prism coupling and Z-scan. Further studies were developed on the precipitation of silver nanoparticles embedded in the glass system TeO2-ZnO-Na2O doped with AgNO3, by means of thermal treatments at different temperatures. The characterization of the metallic nanoparticles was carried out by optical absorption aided by transmission electron microscopy and dispersive energy spectroscopy. Four paramagnetic responses were observed by electron paramagnetic resonance of the -irradiated glasses, one not yet identified and the other three identified as g0, g1 and g3 attributed respectively to the tellurium-oxygen hole center, non-bridging oxygen hole center and tellurium electron center. A model to explain the formation mechanisms of these centers was proposed. The thermoluminescence results indicated that the recombination processes of these centers are non-radiative. This is the first study that deals with polarization and depolarization phenomena in tellurite glasses with and without gamma irradiation, by the technique of thermally stimulated depolarization currents. In what regards the optical properties of the glass systems TeO2-ZnONa2O and TeO2-Nb2O5-Na2O, the effect of the silver doping on the gap energy, Urbach tail, linear and nonlinear refractive indices were investigated. Through the Z-scan technique results of the glass system TeO2-Nb2O5-Na2O, an increasing asymmetry of the curve, with increasing AgNO3 content was observed. This phenomenon was explained through an adaptation of Sumi´s model for non-radiative processes, applied to a silver doped insulating glass, to explain the thermal character of the nonlinear refractive index. Finally, a model was developed to explain the silver nanoparticles precipitation in the TeO2-ZnO-Na2O glass matrix submitted to thermal treatment.
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Investigation of magnetic order in nickel-5d transition metal systemsPapadopoulos, Konstantinos January 2019 (has links)
Double perovskite materials exhibit alterations in magnetic order through manipulation oftheir crystal structure. Certain ultra thin metallic bilayers can create an exotic magnetic stateof confined spin textures called skyrmions. In both cases, new atomic arrangements leadto new electrical and magnetic properties. The following work comprises two studies, bothof which examine the magnetic properties of transition metals in either powder or thin filmsamples. The first part is dedicated to a series of muon spin rotation and relaxation (muSR)experiments on a LaSrNiReO6, double perovskite, powder sample. In the muSR technique, aspin polarized muon beam is focused onto a powder envelope in low pressure and temperatureconditions. The spins of the implanted muons evolve depending on the intrinsic or externallyapplied magnetic field according to Larmor precession. The measurement is based onthe detection of decay positrons that carry this precession information on their preferreddecay directions. Measurements that were realized in wTF, ZF and LF setups, reveal asecond transition to magnetic order at Tc ≃ 22K, below a transition that was observed at T =261K from magnetic susceptibility measurements. The experimental results point to threemagnetic phases, paramagnetic for T > 261K, dilute ferrimagnetic for 22 < T < 261K and amagnetically ordered state for T < 22K, that may implicate ferro- and antiferromagnetismfrom Ni sublattices and Ni-Re interactions. The second part follows an attempt to produce and characterize ultra thin bilayer filmsfor the observation of interfacial chiral structures and skyrmions. Co/Fe/MgO (100) andW/Ni/Cu (100) bilayers were grown with magnetron sputter deposition in various layerthicknesses and their structure was determined by X-ray reflectometry (XRR). The XRRscans presented a relatively thick-layered Co/Fe/MgO film, while extremely thin and roughW/Ni/Cu bilayers, for the purposes of studying films with broken interfacial inversionsymmetry. This study was concluded with indicative magneto-transport measurements thatalso point to the reconfiguration of the growth procedure.
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Estudos das propriedades estruturais e ópticas de vidros teluritos / Studies of the structural and optical properties of the tellurite glassesJúlia Maria Giehl 25 February 2011 (has links)
Vidros teluritos são considerados fortes candidatos para aplicações em lasers e óptica não linear devido a importantes características, como o elevado índice de refração, baixa energia de fônons, baixa temperatura de transição vítrea e sua fácil preparação. Neste trabalho foram produzidas amostras dos sistemas vítreos TeO2- ZnO-Na2O, TeO2-Nb2O5-Na2O e Te2O-Na2O incluindo ou não dopagens de AgNO3 para estudos estruturais e ópticos. As propriedades estruturais e os mecanismos de recombinação destes vidros foram estudados por meio das técnicas de ressonância paramagnética eletrônica, termoluminescência e correntes de despolarização termicamente estimuladas. Já as propriedades ópticas como o coeficiente de absorção linear, índice de refração linear e não linear foram estudadas por meio das técnicas de absorção óptica, acoplamento de prismas e varredura Z. Foram ainda desenvolvidos estudos da precipitação de nanopartículas de prata para o sistema TeO2-ZnO-Na2O com dopagens de AgNO3 com diferentes temperaturas de tratamento térmico. A caracterização das nanopartículas metálicas foi realizada por meio da técnica de absorção óptica auxiliada por microscopia eletrônica de transmissão e espectrometria de energia dispersiva. Foram observadas por ressonância paramagnética eletrônica quatro respostas paramagnéticas dos vidros irradiados com raio , sendo uma de natureza desconhecida e as outras três identificadas como g¹, g² e g³ atribuídas respectivamente ao centro de buraco do telúrio e do oxigênio, centro de buraco do oxigênio terminal e centro de elétron do telúrio. Foi proposto ainda um modelo para explicar os mecanismos de formação destes centros. A partir dos resultados de termoluminescência observou-se que os processos de recombinação destes centros de defeitos são não radioativos. Neste projeto foram estudados pela primeira vez na literatura os fenômenos de polarização e despolarização em vidros teluritos, com e sem irradiação gama, por meio da técnica de correntes de despolarização termicamente estimuladas. Quanto às propriedades ópticas, foi investigada a influência da adição de prata dos sistemas vítreos TeO2-ZnO-Na2O e TeO2-Nb2O5-Na2O em relação à energia do gap, a cauda de Urbach, índice de refração linear e não linear.Nos resultados de varredura Z do sistema vítreo TeO2-Nb2O5-Na2O foi observado o aumento da assimetria na curva com aumento da adição de AgNO3 Este fenômeno foi explicado por meio de uma adaptação do modelo de Sumi para processos não radiativos, responsáveis pelo aumento do caráter térmico do índice de refração não linear. Por fim um modelo foi criado para explicar a precipitação de nanopartículas de prata na matriz vítrea TeO2-ZnO-Na2O mediante tratamento térmico. / Tellurite glasses are considered powerful candidates for applications in lasers and nonlinear optics due to their important properties such as high refractive index, low phonon energy, relatively low glass transition temperature and easy glass production at room atmosphere. In this work glass samples of the systems ZnO-Na2O, TeO2-Nb2O5-Na2O and Te2O-Na2O were produced, including or not the AgNO3 doping for the structural and optical study purposes. The structural properties and the recombination mechanisms of these glasses were studied by means of the techniques of electron paramagnetic resonance, thermoluminescence and thermally stimulated depolarization currents. The optical properties such as the optical linear absorption coefficient, linear and nonlinear refractive index were studied by means of the optical absorption techniques, prism coupling and Z-scan. Further studies were developed on the precipitation of silver nanoparticles embedded in the glass system TeO2-ZnO-Na2O doped with AgNO3, by means of thermal treatments at different temperatures. The characterization of the metallic nanoparticles was carried out by optical absorption aided by transmission electron microscopy and dispersive energy spectroscopy. Four paramagnetic responses were observed by electron paramagnetic resonance of the -irradiated glasses, one not yet identified and the other three identified as g0, g1 and g3 attributed respectively to the tellurium-oxygen hole center, non-bridging oxygen hole center and tellurium electron center. A model to explain the formation mechanisms of these centers was proposed. The thermoluminescence results indicated that the recombination processes of these centers are non-radiative. This is the first study that deals with polarization and depolarization phenomena in tellurite glasses with and without gamma irradiation, by the technique of thermally stimulated depolarization currents. In what regards the optical properties of the glass systems TeO2-ZnONa2O and TeO2-Nb2O5-Na2O, the effect of the silver doping on the gap energy, Urbach tail, linear and nonlinear refractive indices were investigated. Through the Z-scan technique results of the glass system TeO2-Nb2O5-Na2O, an increasing asymmetry of the curve, with increasing AgNO3 content was observed. This phenomenon was explained through an adaptation of Sumi´s model for non-radiative processes, applied to a silver doped insulating glass, to explain the thermal character of the nonlinear refractive index. Finally, a model was developed to explain the silver nanoparticles precipitation in the TeO2-ZnO-Na2O glass matrix submitted to thermal treatment.
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Síntese e caracterização estrutural e magnética das perovskitas complexas ReFe0:5M0:5O3 (Re = Dy, Gd, Sm, Eu,Nd ; M= Mn,Al)Santana, Marcos Cleison Silva 26 February 2015 (has links)
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Samples of Bi 2Fe4O9 mullite and ReFe 0.5M0.5O3 (Re = Nd, Sm, Eu, Gd, Dy; M = Mn, Al) complex perovskites were successfully synthesized by using the combustion synthesis method.
While the mullite was obtained after thermal treatment at temperatures below 1000ºC, complex perovskites are produced after thermal treatments between 1250ºC and 1500ºC for at most 24 h. The X-ray diffraction data analysis suggests the formation of single phase orthorhombic structure, after suitable heat treatment. Scanning electron microscopy (SEM) revealed the formation of micrometric grain size, giving to the sample the relative density. EDS spectra confirmed the homogeneity and purity of complex perovskites. Magnetization measurements as a function of field and temperature showed the diversity of magnetic behavior of the samples. Among the behaviors we can highlight the reorientation of spin for ortoferritas ReFe0.5Mn0.5O3 (Re = Dy, Gd, Eu, Sm, Eu) and ReFe0.5Al0.5O3 (Re = Dy, Nd). Another interesting finding was the effect of magnetic reversal of the samples ReFe0.5Al0.5O3 (Re = Nd, Gd) and EuFe0.5Mn0.5O3. Raman spectra show anomalous bands of second order in the perovskite DyFe0.5Al0.5O3 with
characteristics of resonant effects. The evolution of the band associated with the symmetric vibrational mode of the octahedron shows hardening at the temperature range of ordered magnetic phase, thus suggesting a possible spin-phonon coupling. Depolarization current measurements highlights a relaxation process due to charge carriers in the samples ReFe0.5Mn0.5O3 (Re = Dy, Gd). The application of magnetic field profoundly influences the depolarization current behavior
of DyFe0.5Mn0.5O3. Dielectric permittivity measurements showed no anomalies between 10 K and 300 K, that could can be associated to a ferroelectric phase. / Amostras da mulita Bi2Fe4O9 e das perovskitas complexas ReFe0.5M0.5O3 (Re= Nd, Sm, Eu, Gd, Dy; M = Mn, Al) foram sintetizadas com sucesso utilizando o método de síntese por reação de combustão. Enquanto a mulita foi obtida após tratamento térmico com temperaturas abaixo de 1000ºC, as perovskitas complexas foram produzidas após tratamentos térmicos entre 1250ºC e 1500ºC por, no máximo, 24 h. A análise de dados de difração de raios X sugerem a
formação de estruturas ortorrômbicas de fase única, após os tratamento térmico apropriado. Medidas de microscopia evidenciaram formação de grãos micrométricos conferindo às amostras relativa densidade. Os espectros EDS confirmaram a homogeneidade e pureza das perovskitas complexas. As medidas de magnetização em função do campo e da temperatura evidenciaram a diversidade de comportamentos magnéticos das amostras estudadas. Entre os comportamentos destacamos reorientação de spin para as ortoferritas ReFe0.5Mn0.5O3 (Re = Dy, Gd, Eu, Sm, Eu) e ReFe0.5Al0.5O3 (Re = Dy,Nd). Outro interessante achado foi o efeito de inversão magnética das amostras ReFe0.5Al0.5O3 (Re = Nd, Gd) e EuFe0.5Mn0.5O3. Espectros Raman demonstram
bandas anômalas de segunda ordem na perovskita DyFe0.5Al0.5O3 com características de efeitos ressonantes. A evolução da banda associada ao modo vibracional simétrico do octaedro apresenta endurecimento em temperaturas na faixa da fase magnética ordenada, sugerindo assim,
um possível acoplamento spin-f onon. Medidas de corrente de despolarização destaca um processo de relaxação devido aos portadores de cargas nas amostras ReFe0.5Mn0.5O3 (Re=Dy,Gd). A aplicação de campo magnético influencia profundamente o comportamento da corrente de
despolarização do DyFe0.5Mn0.5O3. Medidas de permissividade dielétrica não exibiram anomalias entre 10 K e 300 K que possam a ser associadas a uma fase ferroelétrica.
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