Vermiculitas tratadas quimicamente na obtenção de sólidos microporosos como precursores para híbridos inorgânico-orgânicos com aplicações adsortivas

ALVES, Ana paula Melo. Vermiculitas tratadas quimicamente na obtenção de sólidos microporosos como precursores para híbridos inorgânico-orgânicos com aplicações adsortivas. 2009. 124 f. Tese (Doutorado em Quimica) - Centro de Ciências Exatas e da Natureza, Universidade Federal da Paraíba, João Pessoa, PB, 2009.

Influência do uso de combustíveis alternativos na síntese por combustão via microondas para a produção de materiais cerâmicos com estrutura espinélio

The development and study of detectors sensitive to flammable combustible and toxic gases at low cost is a crucial technology challenge to enable marketable versions to the market in general. Solid state sensors are attractive for commercial purposes by the strength and lifetime, because it isn t consumed in the reaction with the gas. In parallel, the use of synthesis techniques more viable for the applicability on an industrial scale are more attractive to produce commercial products. In this context ceramics with spinel structure were obtained by microwave-assisted combustion for application to flammable fuel gas detectors. Additionally, alternatives organic-reducers were employed to study the influence of those in the synthesis process and the differences in performance and properties of the powders obtained. The organic- reducers were characterized by Thermogravimetry (TG) and Derivative Thermogravimetry (DTG). After synthesis, the samples were heat treated and characterized by Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), analysis by specific area by BET Method and Scanning Electron Microscopy (SEM). Quantification of phases and structural parameters were carried through Rietveld method. The methodology was effective to obtain Ni-Mn mixed oxides. The fuels influenced in obtaining spinel phase and morphology of the samples, however samples calcined at 950 °C there is just the spinel phase in the material regardless of the organic-reducer. Therefore, differences in performance are expected in technological applications when sample equal in phase but with different morphologies are tested

Desenvolvimento de uma rota química alternativa de síntese de SrCo0,8Fe0,2O3- e LaNi0,3Co0,7O3- para aplicação na reação de oxidação do CO

This thesis focuses on the coprecipitation synthesis method for preparation of ceramic materials with perovskite structure, their characterization and application as catalytic material in the reaction of converting CO to CO2 developing a methodological alternative route of synthesis from the middle via oxalate coprecipitation material SrCo0,8Fe0,2O3-d. In order to check the influence of this method, it was also synthesized using a combined citrate - EDTA complexing method. The material was characterized by: X-ray diffraction (XRD), Rietveld refinement method, thermogravimetry and differential thermo analysis (TG / DTA), scanning (SEM) and transmission (TEM) electron microscopy, particle size distribution and surface analysis method BET. Both methods led to post-phase synthesis, with pH as a relevant parameter. The synthesis based on the method via oxalate coprecipitation among particles led to the crystalline phase as those obtained using a combined citrate - EDTA complexing method under the same conditions of heat treatment. The nature of the reagent used via oxalate coprecipitation method produced a material with approximately 80 % lower than the average size of crystallites. Moreover, the via oxalate coprecipitation method precursors obtained in the solid state at low temperature (~ 26 oC), shorter synthesis, greater thermal stability and a higher yield of around 90-95 %, maintaining the same order of magnitude the crystallite size that the combined citrate - EDTA complexing method. For purposes of comparing the catalytic properties of the material was also synthesized by the using a combined citrate - EDTA complexing method. The evaluation of catalytic materials SrCo0,8Fe0,2O3-d LaNi0,3Co0,7O3-d was accompanied on the oxidation of CO to CO2 using a stainless steel tubular reactor in the temperature range of 75-300 oC. The conversion CO gas was evaluated in both materials on the results shaved that the firm conversion was loves for the material LaNi0,3Co0,7O3-d

Vermiculitas tratadas quimicamente na obtenção de sólidos microporosos como precursores para híbridos inorgânico-orgânicos com aplicações adsortivas

ALVES, Ana paula Melo. Vermiculitas tratadas quimicamente na obtenção de sólidos microporosos como precursores para híbridos inorgânico-orgânicos com aplicações adsortivas. 2009. 124 f. Tese (Doutorado em Quimica) - Centro de Ciências Exatas e da Natureza, Universidade Federal da Paraíba, João Pessoa, PB, 2009.

Influência do uso de combustíveis alternativos na síntese por combustão via microondas para a produção de materiais cerâmicos com estrutura espinélio

The development and study of detectors sensitive to flammable combustible and toxic gases at low cost is a crucial technology challenge to enable marketable versions to the market in general. Solid state sensors are attractive for commercial purposes by the strength and lifetime, because it isn t consumed in the reaction with the gas. In parallel, the use of synthesis techniques more viable for the applicability on an industrial scale are more attractive to produce commercial products. In this context ceramics with spinel structure were obtained by microwave-assisted combustion for application to flammable fuel gas detectors. Additionally, alternatives organic-reducers were employed to study the influence of those in the synthesis process and the differences in performance and properties of the powders obtained. The organic- reducers were characterized by Thermogravimetry (TG) and Derivative Thermogravimetry (DTG). After synthesis, the samples were heat treated and characterized by Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), analysis by specific area by BET Method and Scanning Electron Microscopy (SEM). Quantification of phases and structural parameters were carried through Rietveld method. The methodology was effective to obtain Ni-Mn mixed oxides. The fuels influenced in obtaining spinel phase and morphology of the samples, however samples calcined at 950 °C there is just the spinel phase in the material regardless of the organic-reducer. Therefore, differences in performance are expected in technological applications when sample equal in phase but with different morphologies are tested

Estudo da viabilidade do sistema LZAS para uso como selante de PaCOS

Cells the solid oxide fuel are systems capable to directly convert energy of a chemical reaction into electric energy in clean, quiet way and if its components in the solid state differentiate of excessively the techniques for having all. Its more common geometric configurations are: the tubular one and to glide. Geometry to glide beyond the usual components (anode, cathode and electrolyte) needs interconnect and sealant. E the search for materials adjusted for these components is currently the biggest challenge found for the production of the cells. The sealants need to present chemical stability in high temperatures, to provoke electric isolation, to have coefficient of compatible thermal expansion with the excessively component ones. For presenting these characteristics the glass-ceramics materials are recommended for the application. In this work the study of the partial substitution of the ZrO2 for the Al2O3 in system LZS became it aiming at the formation of system LZAS, this with the addition of natural spodumene with 10, 20 and 30% in mass. The compositions had been casting to a temperature of 1500°C and later quickly cooled with the objective to continue amorphous. Each composition was worn out for attainment of a dust with average diameter of approximately 3μm and characterized by the techniques of DRX, FRX, MEV, dilatometric analysis and particle size analysis. Later the samples had been conformed and treated thermally with temperatures in the interval between 700-1000 °C, with platform of 10 minutes and 1 hour. The analyses for the treated samples had been: dilatometric analysis, DRX, FRX, electrical conductivity and tack. The results point with respect to the viability of the use of system LZAS for use as sealant a time that had presented good results as isolating electric, they had adhered to a material with similar α of the components of a SOFC and had presented steady crystalline phases

Preparação de óxidos mistos de níquel e zinco nanoparticulados a partir de combustíveis alternativos

The field of "Materials Chemistry" has been developing in recent years and there has been a great increase of interest in the synthesis and chemical and physical properties of new inorganic solids. New routes of synthesis and synthesis modified has been developed with the aim not only to optimize the processes in laboratory scale, but also on an industrial scale, and make them acceptable by current environmental legislation. The phenomenology of current solid state chemistry properties coupled with the high temperature superconductivity, ferromagnetism, porosity molecular and colors are evidence affected by the synthesis method, which in turn can influence the technological application of these materials. From this understanding, mixed oxides of nickel and zinc nanoparticulate were synthesized by microwave-assisted combustion route using three specific types of organic fuels employing the weight ratios 1:1/2 and 1:1 of cation metallic/fuel, in order to investigate the influence of such proportions to obtain the solids. The new fuels were chosen to replace, for example, urea or glycine that are the fuels most commonly preferred in this kind of synthesis. The powders without heat treatment were studied by Thermogravimetric analysis (TGA), X-Ray Diffraction (XRD) and then calcined at 900°C. After heat treatment, the samples were characterized by analysis of X Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The modified synthesis route porposed was effective for obtaining powders. Both the alternative fuels chosen as the different weight ratios employed, influenced in the morphology and obtaining oxides

Caracterização térmica (TG/DTG, DTA, DSC, DSC-fotovisual) de Hormônios bioidênticos (estriol estradiol)

Bioidentical hormones are defined as compounds that have exactly the same chemical and molecular structure as hormones that are produced in the human body. It is believed that the use of hormones may be safer and more effective than the non-bioidentical hormones, because binding to receptors in the organism would be similar to the endogenous hormone. Bioidentical estrogens have been used in menopausal women, as an alternative to traditional hormone replacement therapy. Thermal data of these hormones are scarce in literature. Thermal analysis comprises a group of techniques that allows evaluating the physical-chemistry properties of a drug, while the drug is subjected to a controlled temperature programming. The thermal techniques are used in pharmaceutical studies for characterization of drugs, purity determination, polymorphism identification, compatibility and evaluation of stability. This study aims to characterize the bioidentical hormones estradiol and estriol through thermal techniques TG/DTG, DTA, DSC, DSC-photovisual. By the TG curves analysis was possible to calculated kinetic parameters for the samples. The kinetic data showed that there is good correlation in the different models used. For both estradiol and estriol, was found zero order reaction, which enabled the construction of the vapor pressure curves. Data from DTA and DSC curves of melting point and purity are the same of literature, showed relation with DSC-photovisual results. The analysis DTA curves showed the fusion event had the best linearity for both hormones. In the evaluation of possible degradation products, the analysis of the infrared shows no degradation products in the solid state

Adsorção dos gases NH3, NO e H2S em fosfato de vanadila, hidrogeno fosfato de vanadila e fosfatos de vanadila dopados por Al, Co, Mn e Cr

In this work were synthesized the materials called vanadyl phosphate, hydrogen vanadyl phosphate and vanadyl phosphate doped by transition metals with the aim in adsorption the following compounds: ammonia, hydrogen sulfide and nitrogen oxide. To characterize the starting compounds was used DRX, FTIR, FRX and TG analysis. After the characterization of substrates, proceeded de adsorption of NH3 and H2S gases in reactor, passing the gases with continuous flow for 30 min and room temperature. Gravimetric data indicate that the matrices of higher performance in adsorption of ammonia was those doped by aluminum and manganese, obtaining results of 216,77 mgNH3/g and 200,40 mgNH3/g of matrix, respectively. The matrice of higher performance in adsorption of hydrogen sulfide was that doped by manganese, obtaining results of 86,94 mgH2S/g of matrix. The synthesis of substrates VOPO4.2H2O and MnVOPO4.2H2O with nitrogen oxide was made in solution, aiming the final products VOPO4.G.nH2O and MnVOPO4.G.nH2O (G = NO and n = number of water molecules). The thermo analytical behavior and the infrared spectroscopy are indicative of formation of VOPO4.2,5NO.3H2O compound. Results of scanning electron microscopy (SEM) and Energy dispersive spectroscopy (EDS) of materials vanadyl phosphate and vanadyl phosphate modified after reaction in solid state or in solution with the gases show morphology changes in substrates, beyond the formation of orthorhombic sulfur crystals over their respective hosts when these adsorb hydrogen sulfide

Síntese e caracterização de pós Ba(x)Sr(1-x)Co0,8Fe0,2O3- através do método de coprecipitação via oxalato

Ceramic powders based on oxides of perovskite-type structure is of fundamental interest nowadays, since they have important ionic-electronic conductivity in the use of materials with technological applications such as gas sensors, oxygen permeation membranes, catalysts and electrolytes for solid oxide fuel cells (SOFC). The main objective of the project is to develop nanostructured ceramic compounds quaternary-based oxide Barium (Br), Strontium (Sr), Cobalt (Co) and Iron (Fe). In this project were synthesized compounds BaxSr(1-x)Co0, 8Fe0,2O3- (x = 0.2, 0.5 and 0.8) through the oxalate co-precipitation method. The synthesized powders were characterized by thermogravimetric analysis and differential thermal analysis (TGADTA), X-ray diffraction (XRD) with the Rietveld refinement using the software MAUD and scanning electron microscopy (SEM). The results showed that the synthesis technique used was suitable for production of nanostructured ceramic solid solutions. The powders obtained had a crystalline phase with perovskite-type structure. The TGA-DTA results showed that the homogeneous phase of interest was obtained temperature above 1034°C. It was also observed that the heating rate of the calcination process did not affect the elimination of impurities present in the ceramic powder. The variation in the addition of barium dopant promoted changes in the average crystallite size in the nanometer range, the composition being BSCF(5582) obtained the lowest value (179.0nm). The results obtained by oxalate co-precipitation method were compared with those synthesis methods in solid state and EDTA-citrate method

Estudo da deposição de filmes finos de BaTi(1-X)Zr(X)O3 por meio de planejamento Box-Behnken

Ferroelectric ceramics with perovskite structure (ABO3) are widely used in solid state memories (FeRAM’s and DRAM's) as well as multilayered capacitors, especially as a thin films. When doped with zirconium ions, BaTiO3-based materials form a solid solution known as barium zirconate titanate (BaTi1-xZrxO3). Also called BZT, this material can undergo significant changes in their electrical properties for a small variation of zirconium content in the crystal lattice. The present work is the study of the effects of deposition parameters of BaTi0,75Zr0,25O3 thin films by spin-coating method on their morphology and physical properties, through an experimental design of the Box-Behnken type. The resin used in the process has been synthesized by the polymeric precursor method (Pechini) and subsequently split into three portions each of which has its viscosity adjusted to 10, 20 and 30 mPa∙s by means of a rotary viscometer. The resins were then deposited on Pt/Ti/SiO2/Si substrates by spin-coating method on 15 different combinations of viscosity, spin speed (3000, 5500 and 8000 rpm) and the number of deposited layers (5, 8 and 11 layers) and then calcined at 800 ° C for 1 h. The phase composition of the films was analyzed by X-ray diffraction (XRD) and indexed with the JCPDS 36-0019. Surface morphology and grain size were observed by atomic force microscopy (AFM) indicating uniform films and average grain size around 40 nm. Images of the cross section of the films were obtained by scanning electron microscopy field emission (SEM-FEG), indicating very uniform thicknesses ranging from 140-700 nm between samples. Capacitance measurements were performed at room temperature using an impedance analyzer. The films presented dielectric constant values of 55-305 at 100kHz and low dielectric loss. The design indicated no significant interaction effects between the deposition parameters on the thickness of the films. The response surface methodology enabled better observes the simultaneous effect of variables.

Estudo da viabilidade do sistema LZAS para uso como selante de PaCOS

Cells the solid oxide fuel are systems capable to directly convert energy of a chemical reaction into electric energy in clean, quiet way and if its components in the solid state differentiate of excessively the techniques for having all. Its more common geometric configurations are: the tubular one and to glide. Geometry to glide beyond the usual components (anode, cathode and electrolyte) needs interconnect and sealant. E the search for materials adjusted for these components is currently the biggest challenge found for the production of the cells. The sealants need to present chemical stability in high temperatures, to provoke electric isolation, to have coefficient of compatible thermal expansion with the excessively component ones. For presenting these characteristics the glass-ceramics materials are recommended for the application. In this work the study of the partial substitution of the ZrO2 for the Al2O3 in system LZS became it aiming at the formation of system LZAS, this with the addition of natural spodumene with 10, 20 and 30% in mass. The compositions had been casting to a temperature of 1500°C and later quickly cooled with the objective to continue amorphous. Each composition was worn out for attainment of a dust with average diameter of approximately 3μm and characterized by the techniques of DRX, FRX, MEV, dilatometric analysis and particle size analysis. Later the samples had been conformed and treated thermally with temperatures in the interval between 700-1000 °C, with platform of 10 minutes and 1 hour. The analyses for the treated samples had been: dilatometric analysis, DRX, FRX, electrical conductivity and tack. The results point with respect to the viability of the use of system LZAS for use as sealant a time that had presented good results as isolating electric, they had adhered to a material with similar α of the components of a SOFC and had presented steady crystalline phases

Preparação de óxidos mistos de níquel e zinco nanoparticulados a partir de combustíveis alternativos

The field of "Materials Chemistry" has been developing in recent years and there has been a great increase of interest in the synthesis and chemical and physical properties of new inorganic solids. New routes of synthesis and synthesis modified has been developed with the aim not only to optimize the processes in laboratory scale, but also on an industrial scale, and make them acceptable by current environmental legislation. The phenomenology of current solid state chemistry properties coupled with the high temperature superconductivity, ferromagnetism, porosity molecular and colors are evidence affected by the synthesis method, which in turn can influence the technological application of these materials. From this understanding, mixed oxides of nickel and zinc nanoparticulate were synthesized by microwave-assisted combustion route using three specific types of organic fuels employing the weight ratios 1:1/2 and 1:1 of cation metallic/fuel, in order to investigate the influence of such proportions to obtain the solids. The new fuels were chosen to replace, for example, urea or glycine that are the fuels most commonly preferred in this kind of synthesis. The powders without heat treatment were studied by Thermogravimetric analysis (TGA), X-Ray Diffraction (XRD) and then calcined at 900°C. After heat treatment, the samples were characterized by analysis of X Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The modified synthesis route porposed was effective for obtaining powders. Both the alternative fuels chosen as the different weight ratios employed, influenced in the morphology and obtaining oxides