Síntesis de óxidos de estaño con adiciones de óxidos de Cu, Co y Mn mediante el método Pechini para uso potencial en capacitores electroquímicos.

Tesis (Doctor en Ciencias con Orientación en Química de los Materiales) UANL, 2013.

Obtenção de nanopartículas de hexaferrita de bário pelo método pechini

In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

Síntese, estudo cinético e análise microestrutural do sistema cério-níquel obtido pelo método pechini

The cerium oxide has a high potential for use in removing pollutants after combustion, removal of organic matter in waste water and the fuel-cell technology. The nickel oxide is an attractive material due to its excellent chemical stability and their optical properties, electrical and magnetic. In this work, CeO2-NiO- systems on molars reasons 1:1(I), 1:2(II) e 1:3(III) metal-citric acid were synthesized using the Pechini method. We used techniques of TG / DTG and ATD to monitor the degradation process of organic matter to the formation of the oxide. By thermogravimetric analysis and applying the dynamic method proposed by Coats-Redfern, it was possible to study the reactions of thermal decomposition in order to propose the possible mechanism by which the reaction takes place, as well as the determination of kinetic parameters as activation energy, Ea, pre-exponential factor and parameters of activation. It was observed that both variables exert a significant influence on the formation of complex polymeric precursor. The model that best fitted the experimental data in the dynamic mode was R3, which consists of nuclear growth, which formed the nuclei grow to a continuous reaction interface, it proposes a spherical symmetry (order 2 / 3). The values of enthalpy of activation of the system showed that the reaction in the state of transition is exothermic. The variables of composition, together with the variable temperature of calcination were studied by different techniques such as XRD, IV and SEM. Also a study was conducted microstructure by the Rietveld method, the calculation routine was developed to run the package program FullProf Suite, and analyzed by pseudo-Voigt function. It was found that the molar ratio of variable metal-citric acid in the system CeO2-NiO (I), (II), (III) has strong influence on the microstructural properties, size of crystallites and microstrain network, and can be used to control these properties

Síntese pelo método pechini e caracterização da zircônia dopada com cério e neodímio

In this study five compositions were synthesized zirconia doped with cerium and neodymium ions in the system Ce10-xNdx Zr90O2 with 0,5 ≤ x ≤ 4,0 using the Pechini method. The powders were characterized by thermogravimetric analysis, differential thermal analysis, infrared spectroscopy and X-ray diffraction, with application of Rietveld refinement of the calcination temperatures of 350ºC/3h and 30 minutes at 900ºC/3h. All compositions stabilized with a mixture of cubic and tetragonal phase zirconia. The samples were pressed into bars and sintered at 1500°C/3h and 1500°C/6h, being characterized by Xray diffraction, with application of the Rietveld refinement, density and porosity using Archimedes method, scanning electron microscopy and resistance the three point bending. It has been observed the increase in strength with increasing sintering temperature for the compositions x = 2,0 and x = 4,0. For x = 2,0 the main phase was the cubic with 92,56% with crystallite size of 0,56 μm, density and porosity of 96,82% from 1,36%. For x = 4,0 was a mixture of cubic and tetragonal phase with 21% and 37,98%, respectively. The crystallite size was 54,21 nm and 49,64 nm with a density porosity of 97,45% and 1,32% respectively. In the analysis of the fracture surface was observed a greater amount of grain fracture intragranular type, which contribute to increase the mechanical strength of the ceramic. Increased addition of the neodymium ion in the crystal lattice of the zirconium showed a nearly linear behavior with increasing mechanical strength of the zirconia ceramic. Was obtained a bending resistance of 537 ± 38 MPa for the composition x = 2,0 predominantly attributed to cubic phase with 92,56%

Óxido de zinco dopado com gálio preparado pelo método Pechini

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Influência do oxalato de amônio na formação do precursor columbita obtido pelo método Pechini

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Respuesta eléctrica de películas gruesas del sistema SnO2-TiO2, conformadas con polvos cerámicos obtenidos a través del método pechini

Tin oxide is the compound more used in the gas sensor production, mainly to reduce gases like CO and H2. Their electrical properties are strongly dependent of its surface. For this is of great importance to synthesize nanoscale tin oxide particles to use they later in the films conformation. The synthesis of SnO2-TiO2 nanoparticles by polymeric precursor method is reported in this work. The particles were characterized by DTA/TG, FT-IR, XRD and SEM. Also, the electrical response of thick films measured under oxygen and carbon monoxide atmospheres is was analyzed.

Influencia del TiO2 y Al2O3 sobre las propiedades eléctricas y microestructurales de cerámicas de SnO2 obtenidas por el método Pechini

Tin oxide has wakened up great scientific and technological interest for its potential use in varistors production and as gas sensor. In order to improve the microstructural and electrical properties in SnO varistor ceramics, the influence of differents dopants used, like TiO2 and Al2O3, is under research. The effect of TiO2 and Al2O3 on the properties of Sn-Co-Nb varistor Systems obtained by the Pechini method has been investigated in this work. Characterization of synthesized raw material was performed by X-Ray Diffraction (XRD) and Scanning Electronic Microscopy (SEM). The microstructural and electrical characterization of sintered samples show that the TiO2 favors the grain growth and the Al2O3, contributes to the decrease it, effect that is manifested in the Sn-Co-Nb varistor systems. Breakdown field increase up to 6300V/cm with increasing Al2O3 content and non-linear coefficients with α=22 were obtained.

Otimização das condições de síntese de amostras cerâmicas do composto Y'Ba IND. 2''Cu IND. 3''O IND. 7'-δ através do Método Pechini

Pós-graduação em Ciência e Tecnologia de Materiais - FC

Síntese de supercondutores cerâmicos à base de bismuto produzidos pelo método Pechini associado ao processo de hidrotermalização assistido por micro-ondas

Pós-graduação em Ciência dos Materiais - FEIS

Obtenção de nanopartículas de hexaferrita de bário pelo método pechini

In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

Síntese, estudo cinético e análise microestrutural do sistema cério-níquel obtido pelo método pechini

The cerium oxide has a high potential for use in removing pollutants after combustion, removal of organic matter in waste water and the fuel-cell technology. The nickel oxide is an attractive material due to its excellent chemical stability and their optical properties, electrical and magnetic. In this work, CeO2-NiO- systems on molars reasons 1:1(I), 1:2(II) e 1:3(III) metal-citric acid were synthesized using the Pechini method. We used techniques of TG / DTG and ATD to monitor the degradation process of organic matter to the formation of the oxide. By thermogravimetric analysis and applying the dynamic method proposed by Coats-Redfern, it was possible to study the reactions of thermal decomposition in order to propose the possible mechanism by which the reaction takes place, as well as the determination of kinetic parameters as activation energy, Ea, pre-exponential factor and parameters of activation. It was observed that both variables exert a significant influence on the formation of complex polymeric precursor. The model that best fitted the experimental data in the dynamic mode was R3, which consists of nuclear growth, which formed the nuclei grow to a continuous reaction interface, it proposes a spherical symmetry (order 2 / 3). The values of enthalpy of activation of the system showed that the reaction in the state of transition is exothermic. The variables of composition, together with the variable temperature of calcination were studied by different techniques such as XRD, IV and SEM. Also a study was conducted microstructure by the Rietveld method, the calculation routine was developed to run the package program FullProf Suite, and analyzed by pseudo-Voigt function. It was found that the molar ratio of variable metal-citric acid in the system CeO2-NiO (I), (II), (III) has strong influence on the microstructural properties, size of crystallites and microstrain network, and can be used to control these properties

Analysis of Ca-PZT powder obtained by the Pechini and partial oxalate methods

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Cerâmica condutora à base de 'SN''O IND.2' obtida pelo método dos precursores poliméricos e sinterização por micro-ondas

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Síntese e caracterização estrutural de pigmentos cerâmicos a base de cromita por método químico

The ceramic pigments are colored inorganic substances that during the process of dispersion in the ceramic glazes and subsequent calcination, are stable against physical and chemical attack. Therefore, they are crystalline compounds applied in the ceramic industry for coloring vitreous base. In this study, the Pechini method was used for obtaining the pigment CuCr2O4 with heat treatment at the temperatures of 800, 900 and 1000 ° C. The powder pigments were characterized on their structural, morphological and colorimetric aspects. The thermal analysis conducted on an amorphous precursor in a TG / DTA indicates the weight loss in the entire temperature range investigated, with characteristic exothermic peak of the elimination of the organic composition of the precursor around 300°C. The development of the crystalline phases were investigated by XRD, using a diffractometer with Cu Ka radiation and graphite monochromator, where it was observed the presence of crystalline phases corresponding to Cr2O3 and CuCr2O4.The measurements of the specific surface area of the powders pigments were carried out in an equipment Micromeritcs, model ASAP 2000, using N2 as gas of adsorption/desorption. The colorimetric measurements of the pigments were made in a colorimeter Gretac Macbeth Color-eye spectrophotometer 2180 / 2180UV in CIELAB standards. Based on the obtained results, it can be verified the thermal stability of the powder pigments of green coloration, which enables it as an alternative to the materials currently used in the manufacture of ceramic tiles.