Orientador: Elson Longo da Silva / Banca: Sonia Maria Zanetti / Banca: Alberthmeiry Teixeira Figueiredo / O Programa de Pós-Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi da Unesp / Resumo: Neste trabalho de dissertação de mestrado foram preparadas amostras do sistema 'Pb IND. 1-x-yCa IND. xSr IND.yTiO IND. 3' (PCST) com x = 0.05, 0,15, 0,35 e y = 0,05, 0.15, 0,35, utilizando-se o método dos precursores poliméricos e, a partir desse material, produzir amostras cerâmicas e filmes finos nanoestruturados e caracterizar suas propriedades estruturais, microestruturais e elétricas. A caracterização estrutural foi realizada utilizando as técnicas de difração de raios X, espectroscopia Raman e espectroscopia na região do infravermelho. Os filmes finos foram preparados pela técnica "spin-coating" sobre substrato de 'Si/SiO IND. 2/Ti/Pt'. A temperatura de cristalização foi de 600ºC. A cristalização de todos os filmes finos e pó apresentaram estrutura do tipo perovisquita sem a presença de uma segunda fase. Foi possível obter com sucesso um sistema complexo de incorporação de dois diferentes íons '(Ca POT. 2+ e Sr POT. 2+)' no sitio A, em substituição aos íons 'Pb POT. 2+' para o sistema 'Pb IND. 1-x-yCa IND. xSr IND.yTiO IND. 3' na forma de filme fino e pó, sem a separação de fases tais como 'PbTiO IND. 3, CaTiO IND. 3, SrTiO IND. 3', ou até mesmo fase complexas como '(Pb,Sr)TiO IND. 3' ou '(Pb,Ca)TiO IND. 3'. Os sítios A localizam-se dentro de um dodecaedro '(AO IND. 12)' de doze oxigênios enquanto o sitio B no interior de um octaedro regular '(BO IND.6)' constituído de oito oxigênios. Portanto, as distorções ocorridas nestas estruturas produzem importantes mudanças e surgimento de novas propriedades elétricas que encadeiam grande interesse tecnológico e cientifico. As propriedades ferroelétricas foram fortemente influenciadas pela presença desses dois íons '(Ca POT. 2+ e Sr POT. 2+)' em substituição aos íons 'Pb POT. 2+'. Levando o sistema a uma completa ausência de natureza ferroelétrica a temperatura ambiente. / Abstract: On this master's degree dissertation samples of the system 'Pb IND. 1-x-yCa IND. xSr IND.yTiO IND. 3' (PCST) with x = 0.05, 0.15, 0.35 and y = 0.05, 0.15, 0.35 were prepared through the polymeric precursors method. From this material, ceramic samples and thin films were produced and their structure, microstructure and electrical properties were assessed. The structural characterization was done using X-ray diffraction, Raman spectroscopy and spectroscopy techniques on the infrared region. The films were prepared through the spin-coating technique on 'Si/SiO IND. 2/Ti/Pt' substrate and its crystallization temperature was 600ºC. All thin films and powder showed structure like perovskite without a second phase. A complex incorporation system of two different ions '(Ca POT. 2+ e Sr POT. 2+)' at site A was successfully achieved, replacing the 'Pb POT. 2+' ions on the 'Pb IND. 1-x-yCa IND. xSr IND.yTiO IND. 3' system as thin film and powder with no partition of phases such as 'PbTiO IND. 3, CaTiO IND. 3, SrTiO IND. 3', or even more complex ones as '(Pb,Sr)TiO IND. 3' or '(Pb,Ca)TiO IND. 3'. The sites A were found in a '(AO IND. 12)' dodecahedron of twelve oxygens, and the site B was discovered in a regular octahedron formed by eight oxygens. Therefore the distortions on these structures triggered relevant changes and new electrical properties which promote great technological and scientific interest. It is noteworthy that the ferroelectric properties were heavily influenced by the presence of these two ions '(Ca POT. 2+ e Sr POT. 2+)' replacing the 'Pb POT. 2+' ions, leading the system to an absolute absence of ferroelectric nature at room temperature. / Mestre

Made available in DSpace on 2014-06-11T19:23:29Z (GMT). No. of bitstreams: 0 Previous issue date: 2008-07-07Bitstream added on 2014-06-13T19:29:34Z : No. of bitstreams: 1 pontes_dsl_me_bauru.pdf: 3995495 bytes, checksum: e77735073c68d26d0fbf6d4f3285874a (MD5) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / Neste trabalho de dissertação de mestrado foram preparadas amostras do sistema 'Pb IND. 1-x-yCa IND. xSr IND.yTiO IND. 3' (PCST) com x = 0.05, 0,15, 0,35 e y = 0,05, 0.15, 0,35, utilizando-se o método dos precursores poliméricos e, a partir desse material, produzir amostras cerâmicas e filmes finos nanoestruturados e caracterizar suas propriedades estruturais, microestruturais e elétricas. A caracterização estrutural foi realizada utilizando as técnicas de difração de raios X, espectroscopia Raman e espectroscopia na região do infravermelho. Os filmes finos foram preparados pela técnica “spin-coating” sobre substrato de 'Si/SiO IND. 2/Ti/Pt'. A temperatura de cristalização foi de 600ºC. A cristalização de todos os filmes finos e pó apresentaram estrutura do tipo perovisquita sem a presença de uma segunda fase. Foi possível obter com sucesso um sistema complexo de incorporação de dois diferentes íons '(Ca POT. 2+ e Sr POT. 2+)' no sitio A, em substituição aos íons 'Pb POT. 2+' para o sistema 'Pb IND. 1-x-yCa IND. xSr IND.yTiO IND. 3' na forma de filme fino e pó, sem a separação de fases tais como 'PbTiO IND. 3, CaTiO IND. 3, SrTiO IND. 3', ou até mesmo fase complexas como '(Pb,Sr)TiO IND. 3' ou '(Pb,Ca)TiO IND. 3'. Os sítios A localizam-se dentro de um dodecaedro '(AO IND. 12)' de doze oxigênios enquanto o sitio B no interior de um octaedro regular '(BO IND.6)' constituído de oito oxigênios. Portanto, as distorções ocorridas nestas estruturas produzem importantes mudanças e surgimento de novas propriedades elétricas que encadeiam grande interesse tecnológico e cientifico. As propriedades ferroelétricas foram fortemente influenciadas pela presença desses dois íons '(Ca POT. 2+ e Sr POT. 2+)' em substituição aos íons 'Pb POT. 2+'. Levando o sistema a uma completa ausência de natureza ferroelétrica a temperatura ambiente. / On this master’s degree dissertation samples of the system 'Pb IND. 1-x-yCa IND. xSr IND.yTiO IND. 3' (PCST) with x = 0.05, 0.15, 0.35 and y = 0.05, 0.15, 0.35 were prepared through the polymeric precursors method. From this material, ceramic samples and thin films were produced and their structure, microstructure and electrical properties were assessed. The structural characterization was done using X-ray diffraction, Raman spectroscopy and spectroscopy techniques on the infrared region. The films were prepared through the spin-coating technique on 'Si/SiO IND. 2/Ti/Pt' substrate and its crystallization temperature was 600ºC. All thin films and powder showed structure like perovskite without a second phase. A complex incorporation system of two different ions '(Ca POT. 2+ e Sr POT. 2+)' at site A was successfully achieved, replacing the 'Pb POT. 2+' ions on the 'Pb IND. 1-x-yCa IND. xSr IND.yTiO IND. 3' system as thin film and powder with no partition of phases such as 'PbTiO IND. 3, CaTiO IND. 3, SrTiO IND. 3', or even more complex ones as '(Pb,Sr)TiO IND. 3' or '(Pb,Ca)TiO IND. 3'. The sites A were found in a '(AO IND. 12)' dodecahedron of twelve oxygens, and the site B was discovered in a regular octahedron formed by eight oxygens. Therefore the distortions on these structures triggered relevant changes and new electrical properties which promote great technological and scientific interest. It is noteworthy that the ferroelectric properties were heavily influenced by the presence of these two ions '(Ca POT. 2+ e Sr POT. 2+)' replacing the 'Pb POT. 2+' ions, leading the system to an absolute absence of ferroelectric nature at room temperature.

The optical propagation losses resulting from the internal microstructure of ZnS thin films were investigated using a wavelength technique. Waveguide losses were determined by measuring the scattered light as a function of propagation distance along the film. Accurate measurements were obtained by using a technique we developed that employees a coherent fiber bundle to transfer the scattered light streak to a remote image plane that was scanned with an apertured photomultiplier tube. Microstructure effects on losses were found to dominate effects caused by substrate surface finish. The magnitude of the loss was found to depend upon two independent parameters: the average grain size of the polycrystalline films and the refractive index difference between ZnS and the interstitial material. Increasing the H₂O partial pressure led to lower losses as a result of reduced crystallite size, and a change in preferential crystallite orientation. A similar change in orientation was observed for films deposited onto heated substrates. Increasing the O₂ partial pressure during deposition also resulted in slightly lower waveguide losses, possibly as a result of void filling with ZnO. The modal dependence of the losses for ZnS films deposited at ambient temperature suggests that volume losses dominate surface losses for the lowest order mode while the ratio of surface to volume losses increases for higher order modes. By depositing ZnS onto substrates cooled with liquid nitrogen, adatom surface mobility was reduced which resulted in amorphous films. Losses were minimized (≤0.5 dB/cm at λ = 633 nm) for a substrate temperature of -50°C. These losses are lower than any previously reported for ZnS. However, further reduction of the substrate temperature resulted in an increase in tensile stress which eventually led to higher waveguide losses and crazing. The films deposited onto cooled substrates exhibited a low refractive index which indicates a low packing density and increased porosity. Differential water desorption, which is further evidence of increased porosity, was most noticeable in films with lower refractive indices when nonlinear prism coupling was attempted.

Title: NMR in magnetic systems Author: Petr Křišťan Department: Department of Low Temperature Physics Supervisor: prof. RNDr. Helena Štěpánková, CSc. Abstract: Magnetically ordered iron oxides, namely magnetite, maghemite, hexagonal ferrite M or system Fe-B, with nano or submicron dimensions of particles are the main subject of study of the presented thesis. The materials were investigated mainly by 57 Fe nuclear magnetic resonance (NMR). The results were thoroughly analyzed and compared with the results obtained by other methods (Mössbauer spectroscopy, ZFC/FC magnetic measurement, X-ray diffraction or TEM). In case of the maghemite nanoparticles a regular distribution of vacancies in octahedral positions was verified by the help of NMR in external magnetic fields and at various temperatures. The experi- mental results were also compared with ab-initio calculations. In thin layers of barium M type hexaferrite, effects of reduced particle size on 57 Fe NMR spectra were observed. The NMR methods were also successfully applied to investigation of system FeMoCuB of amorphous and nanocrystalline ribbons, where 57 Fe NMR was able to resolve formation of different phases in depen- dence on the process of preparation. Due to different NMR excitation condi- tions of signal from strontium M type hexaferrite and maghemite,...