Orientador: Eudes Borges de Araújo / Banca: Newton Luiz Dias Filho / Banca: Marcelo Rubens Barsi Andreeta / Banca: Fábio Simões de Vicente / Banca: Emerson Marcelo Girotto / 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: Materiais ferroelétricos do sistema Pb('Mg IND. 1/3'Nb IND.2/3')'O IND. 3'-xPbTi'O IND. 3'(PMN-xPT), possuem potencial efetivo para aplicações em dispositivos eletromecânicos, tais como, transdutores e sensores. Porém, a obtenção de cerâmica de PMN-xPT livre de fase pirocloro (paraelétrica) exige rigoroso controle durante a síntese. Neste trabalho, as condições destinadas a supressão de fase pirocloro em cerâmicas de PMN e PMN-xPT (para x = 0,33, 0,35 e 0,37), foram estudadas a partir de uma nova rota de preparação em função do excesso de MgO e PbO. Paralelamente, cerâmicas de PMN e PMN-PT obtidas pela rota convencional de mistura de óxidos, foram preparadas e os resultados comparados. Os resultados obtidos revelaram valores mais elevados de permissividade para as cerâmicas preparadas pela nova rota. Os valores da polarização remanescente das cerâmicas de PMN-xPT mostraram-se comparáveis com monocristais. Medidas dielétricas realizadas nas cerâmicas de PMN-xPT apontam um significante aumento nos valores de permissividade dielétrica em função do aumento do campo elétrico AC. Condutividade AC e impedância nas cerâmicas de PMN-xT foram estudadaas na região de frequência de 100Hz-1MHz e temperatura 325 - 50ºC. Uma anomalia no espectro de condutividade foi observada para todas as composições, próximo ao ponto de transição de fase ferroelétrica-paraelétrica. / Abstract: Ferroelectric materials of Pb('Mg IND. 1/3'Nb IND.2/3')'O IND. 3'-xPbTi'O IND. 3'(PMN-xPT) system have effective potential for applications in electromechanical devices such as transducers and sensors. However, to obtain free pyrochlore phase (paraelectric) ceramics of PMN-xPT requires control during the synthesis. In this work, the conditions for the removal of pyrochlore phase of PMN and PMN-xPT (for x = 0.33, 0,35 and 0.37) ceramics, were studied using a new route of preparation with the excess MgO and PbO. The obtained results were compared with the ceramics of PMN and PMN-xPT prepared by the conventional route of mixed oxides. The results showed higher values of permittivity for the ceramics prepared by the new route. The remnant polarization values of PMN-xPT ceramics shown to be comparable with single crystal. Dielectric of PMN-xPT ceramics showed a significant increase in the values of dielectric permittivity due to the increase of the AC electric field. Conductivity AC and impedance of PMN-xPT ceramics were studied in the frequency range of 100Hz - 1MHz and temperature 325 - 50ºC. An anomaly was observed in the spectrum of conductivity for all the compositions, which is close to the point of ferroelectric-paraelectric phase transition. / Doutor

Made available in DSpace on 2014-06-11T19:32:10Z (GMT). No. of bitstreams: 0 Previous issue date: 2009-04-24Bitstream added on 2014-06-13T19:47:11Z : No. of bitstreams: 1 reis_rn_dr_bauru.pdf: 4426846 bytes, checksum: 0832ad71536929474c2efea40b48c449 (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Materiais ferroelétricos do sistema Pb('Mg IND. 1/3''Nb IND.2/3')'O IND. 3'-xPbTi'O IND. 3'(PMN-xPT), possuem potencial efetivo para aplicações em dispositivos eletromecânicos, tais como, transdutores e sensores. Porém, a obtenção de cerâmica de PMN-xPT livre de fase pirocloro (paraelétrica) exige rigoroso controle durante a síntese. Neste trabalho, as condições destinadas a supressão de fase pirocloro em cerâmicas de PMN e PMN-xPT (para x = 0,33, 0,35 e 0,37), foram estudadas a partir de uma nova rota de preparação em função do excesso de MgO e PbO. Paralelamente, cerâmicas de PMN e PMN-PT obtidas pela rota convencional de mistura de óxidos, foram preparadas e os resultados comparados. Os resultados obtidos revelaram valores mais elevados de permissividade para as cerâmicas preparadas pela nova rota. Os valores da polarização remanescente das cerâmicas de PMN-xPT mostraram-se comparáveis com monocristais. Medidas dielétricas realizadas nas cerâmicas de PMN-xPT apontam um significante aumento nos valores de permissividade dielétrica em função do aumento do campo elétrico AC. Condutividade AC e impedância nas cerâmicas de PMN-xT foram estudadaas na região de frequência de 100Hz-1MHz e temperatura 325 - 50ºC. Uma anomalia no espectro de condutividade foi observada para todas as composições, próximo ao ponto de transição de fase ferroelétrica-paraelétrica. / Ferroelectric materials of Pb('Mg IND. 1/3''Nb IND.2/3')'O IND. 3'-xPbTi'O IND. 3'(PMN-xPT) system have effective potential for applications in electromechanical devices such as transducers and sensors. However, to obtain free pyrochlore phase (paraelectric) ceramics of PMN-xPT requires control during the synthesis. In this work, the conditions for the removal of pyrochlore phase of PMN and PMN-xPT (for x = 0.33, 0,35 and 0.37) ceramics, were studied using a new route of preparation with the excess MgO and PbO. The obtained results were compared with the ceramics of PMN and PMN-xPT prepared by the conventional route of mixed oxides. The results showed higher values of permittivity for the ceramics prepared by the new route. The remnant polarization values of PMN-xPT ceramics shown to be comparable with single crystal. Dielectric of PMN-xPT ceramics showed a significant increase in the values of dielectric permittivity due to the increase of the AC electric field. Conductivity AC and impedance of PMN-xPT ceramics were studied in the frequency range of 100Hz - 1MHz and temperature 325 - 50ºC. An anomaly was observed in the spectrum of conductivity for all the compositions, which is close to the point of ferroelectric-paraelectric phase transition.

The aim of this study is to produce Nb doped PZT thin films and then investigate the effects of Nb+5 ion on the structural, dielectric and ferroelectric properties. Niobium (Nb) doped lead zirconate titanate thin films (PNZT) were produced by solution deposition with nominal compositions, Pb(1-0.5x)(Zr0.53Ti0.47)1-xNbxO3 where x = 0.00 - 0.07. Single and multi-layered films were deposited onto (111)-Pt/Ti/SiO2/Si-(100) substrates by spin coating. PZT compositions near the morphotropic phase boundary (MPB) was chosen because excellent ferroelectric and dielectric properties were achieved in this area. The effects of sintering temperature, sintering time, variation of thickness in the films and change of niobium content were investigated with regard to phase development, microstructure, and ferroelectric and dielectric characteristics. The best results were obtained in double layered films (390 nm) which were sintered at 600 &deg / C for 1 h. Grain size of the films decreases with increasing Nb content except for 1 at % Nb doped films. The average grain size of 1 at % Nb doped thin films was calculated as 130 nm by using FESEM. Optimum doping level was found in 1 at % Nb doped films. For 1 at % Nb doped [Pb0.995(Zr0.53Ti0.47)0.99Nb0.01O3] films, remnant polarization (Pr) of 35.75 &amp / #956 / C/cm2 and coercive field (Ec) of 75.65 kV/cm have been obtained. The maximum dielectric constant was achieved in 1 at % Nb doped films which was 689. Tangent loss values were found between 2-4 % and these values were independent of Nb concentrations. Ferroelectric and dielectric properties were decreased at higher Nb doping levels because of the changes in the grain size, distortion of the crystal structure and pinning of the domains.

In the presented thesis, lead-free Ba(Ti0.8Zr0.2)O3-(Ba0.7Ca0.3)TiO3 (BZT-BCT) thin films were deposited on Pt/TiO2/SiO2/Si substrates using chemical solution deposition method and then the effect of process parameters were investigated to obtain optimum parameters of these lead-free thin films. The phase was selected near to the morphotropic phase boundary (MPH) to increase the number of polarization directions where rhombohedral and tetragonal phases exist together. In this study, the effect of sintering temperatures on microstructure, dielectric and ferroelectric properties were studied systematically. Among the various high-quality BZT-BCT thin films with uniform thickness, the optimum dielectric and ferroelectric responses were observed for films annealed at 800 oC for 1 h sintering time. The thickness was kept constant for all measurements as 500 nm (triple layered films). Therefore, the average grain sizes were found around 60 nm for samples sintered at 700,750 and 800 oC. BZT-BCT thin films sintered at 800 oC showed effective remnant polarization and coercive field values of 2.9 &micro / C/cm2 and 49.4 kV/cm, together with a high dielectric constant and low loss tangent of 365.6 and 3.52 %, respectively, at a frequency of 600 kHz due to pure perovskite phase showing full crystallization and minimum surface porosity obtained at this temperature.