Optimization of photo-polymerized sol gel monolithic stationary phases prepared in polyacrylate-coated fused-silica capillaries for capillary electrochromatography

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SrBi2Nb2O9 thin films crystallized using a low power microwave oven

SrBi2Nb2O9 thin films were produced by the polymeric precursor method using an aqueous solution. The crystallization of the films was carried out using a domestic microwave oven by means of a SiC susceptor in order to absorb the microwave energy and rapidly transfer the heat to the film. Low microwave power and short time have been used. The films obtained are well-adhered, homogeneous and with good specularity, even when treated at 600 degreesC for 10 min. The microstructure and the structure of the films can be tuned by adjusting the crystallization conditions. Depending on the direction of the heat flux it is possible to obtain preferential oriented or polycrystalline films in the microwave oven for 10 min. The microstructure presented a polycrystalline nature with spheroid small mean grain size when the susceptor is placed above the substrate. When the susceptor is placed below the substrate, the films presented platelet grains with mean grain size around 250 nm and a 001 orientation. For comparison, films were also prepared by the conventional method at 700 degreesC for 2 h. (C) 2003 Elsevier Ltd. All rights reserved.

Study of electrical, chemical and structural characteristics of superconductor thin film obtained by polymeric precursors method

Superconductor films of the BSCCO system have been grown by dip coating technique with good success. The chemical method allows us to grow high temperature superconductor thin films to get better control of stoichiometry, large areas and is cheaper than other methods. There is a great technological interest in growth oriented superconductor films due anisotropic characteristics of superconductor materials of high critical temperature, specifically the cuprates, as we know that the orientation may increase the electrical transport properties. Based on this, the polymeric precursor method has been used to obtain thin films of the BSCCO system. In this work we have applied that method together with the deposition technique known as dip coating to obtain Bi-based superconductor thin films, specifically, Bi1.6Pb0.4Sr2.0C2.0Cu3.0Ox+8, also known as 2223 phase with a critical temperature around 110 K. The films with multilayers have been grown on crystalline substrates of LaAlO3 and orientated (100) after being heat treated around 790 degrees C - 820 degrees C in lapse time of 1 hour in a controlled atmosphere. XRD measurements have shown the presence of a crystalline phase 2212 with a critical temperature around 85 K with (001) orientation, as well as a small fraction of 2223 phase. SEM has shown a low uniformity and some cracks that maybe related to the applied heat treatment. WDS has also been used to study the films composition. Different heat treatments have been used with the aim to increase the percentage of 2223 phase. Measurements of resistivity confirmed the presence of at least two crystalline phases, 2212 and 2223, with T-c around 85 K and 110 K, respectively.

Nanocoating of Al2O3 additive on ZrO2 powder and its effect on the sintering behaviour in ZrO2 ceramic

ZrO2 powder was coated with Al2O3 precursor generated by a polymeric precursor method in aqueous solution. The system of nanocoated particles formed a core shell-like structure in which the particle is the core and the nanocoating (additive) is the shell. A new approach is reported in order to control the superficial mass transport and the exaggerated grain growth during the sintering of zirconia powder. Transmission electron microscopy (TEM) observations clearly showed the formation of an alumina layer on the surface of the zirconia particles. This layer modifies the sintering process and retards the maximum shrinkage temperature of the pure zirconia.

Synthesis of nanocrystalline tetragonal zirconia by a polymeric organometallic method

A polymeric precursor method based on the Pechini process was successfully used to synthesize zirconia-12 mol% ceria ceramic powders, the influence of the main process variables (citric acid-ethylene glycol ratio, citric acid-total oxides ratio and calcination temperature) on phase formation and powder morphology (surface area and crystallite size) were investigated. The thermal decomposition behavior of the precursor is presented. X-ray diffraction (XRD) patterns of powders revealed a crystalline tetragonal zirconia single-phase, with crystallite diameter ranging from 6 to 15 nm. The BET surface areas were relatively high, reaching 95 m(2) g(-1) Nitrogen adsorption/desorption on the powders suggested that nonaggregated powders could be attained, depending on the synthesis conditions. Copyright (C) 1999 John Wiley & Sons, Ltd.

The effect of Nb doping on ferroelectric properties of PZT thin films prepared from polymeric precursors

Pure and Nb doped PbZr0.4Ti0.603 thin films was prepared by the polymeric precursor method and deposited by spin coating on Pt/Ti/SiO2/Si (100) substrates and annealed at 700 degreesC. The films are oriented in (1 1 0) and (1 0 0) direction. The electric properties of PZT thin films show strong dependence of the crystallographic orientation. The P-E hysteresis loops for the thin film with composition PbZr0.39Ti0.6Nb0.103 showed good saturation, with values for coercive field (E-c) equal to 60 KV cm(-1) and for remanent polarization (P-r) equal to 20 muC cm(-2). The measured dielectric constant (epsilon) is 1084 for this film. These results show good potential for application in FERAM. (C) 2004 Elsevier B.V. All rights reserved.

Influence of polymerization on the synthesis of SrTiO3: Part I. Characteristics of the polymeric precursors and their thermal decomposition

The influence of polymerization on the thermal decomposition of polymeric precursors and phase formation was investigated during synthesis of SrTiO3. The precipitation of polymeric precursor in acetone produced a more thermal stable precursor with lower weight loss during decomposition. This more stable precursor retarded the formation of the SrTiO3 phase. From thermal analysis, XRD and FT-IR the presence of an intermediate phase during decomposition of the precursors was observed. This is a mixed (Sr,Ti) carbonate phase with the proposed composition of Sr2Ti2O5.CO3. © 1995.

Particle growth during calcination of polycation oxides synthesized by the polymeric precursors method

The particle-growth kinetics of sodium niobate and zirconium titanate powders that were processed by the polymeric precursors method were studied. The growth kinetics that were studied for the particle, in the final stage of crystallization, showed that the growth process occurs in two different stages. For temperatures <800°C, the particle-growth mechanism is associated with surface diffusion, with an activation energy in the range of 40-80 KJ/mol. For temprratures >800°C, particle growth is controlled by densification of the nanometric particle cluster and by a neck-size-controlled particle-growth mechanism. The results suggest that this behavior was typical of the synthesis method, because two different polycation oxides presented the same behavior.

Synthesis of PbTiO3 by use of polymeric precursors

Lead titanate powders were synthesized through the use of polymeric precursors according to the Pechini Process. The polymeric precursor was calcined at temperatures ranging from 300 to 600°C for 1 or 2 h. X-ray diffraction (XRD) showed that lead titanate crystallizes from the precursor at temperatures as low as 400°C. No intermediate carbonate phase was detected by Fourier transform infrared spectroscopy (FTIR) or by XRD. A powder with mean particle size of 150 nm was obtained after calcination of the precursor at 600°C for 1 h. © 1998 Elsevier Science B.V. All rights reserved.

Temperature and stoichiometry effect on microstructural and ferroelectric properties of Pb(Zr1-xTix)O3 thin films prepared by chemical soulution deposition

Lead zirconate titanate (PZT) solutions were prepared using a polymeric precursor method, Zr n-propoxide and Ti i-propoxide were used as starting materials with ethylene glycol and water as solvents. The PZT solution was spin-coated on Pt/Ti/SiO2/Si substrates, baked on a hot plate, and finally heat-treated in a tube furnace between 400 and 800°C. The surface morphology and grain size of the films were characterized by atomic force microscopy (AFM), using a tapping mode with amplitude modulation. The films, thermal annealed at temperatures higher than 500°C, exhibited a dense microstructure, without noticeable cracks or voids. Electrical properties were investigated as a function of composition and annealing temperature.

Characterization of Zn0. 95Mn0.05O synthesized by polymeric precursors

This paper discusses the preparation and characterization of Zn 0.95Mn0.05O phase obtained by the polymeric precursor method for DMS applications. The as-obtained powders were calcined between 500 to 800°C and characterized by XRD, SEM and BET. The XRD analysis of the powder showed a crystalline material containing second phase. The crystallite sizes ranged from 20 to 51 nm. The micrographs showed that the powders consisted of soft and homogeneous agglomerations. The nitrogen adsorption/desorption curves of the Zn0.95Mn0.05O phases were type II curves, which is characteristic of mesoporous materials.

Lanthanum cobaltite black pigments with perovskite structure

In this work La1-xCaxCoO3 (x = 0-0.4) pigments were synthesized by the polymeric precursor method with heat treatments at 700, 800 and 900 C for 4 h. The powders were characterized by colorimetry, UV-vis spectroscopy and powder X-ray diffraction (XRD). The X-ray diffraction patterns showed the presence of a single phase perovskite, changing its structure from rhombohedral to cubic, when calcium was added to the lattice. All of the pigments had a black colour with a strong absorption over the whole of the visible spectrum as a consequence of the different oxidation states of cobalt and the high short-range disorder. The substitution of Ca2+ for La3+ did not influence the pigment colour but decreased its final cost. © 2013 Elsevier Ltd. All rights reserved.

Síntese e caracterização de nanoestruturas e filmes finos de 'BI' 'FE' 'OIND.3' modificado com samário visando aplicação em memórias de múltiplos estados

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Caracterização estrutural de pós de 'SRTIO IND.3' puro e dopado com samário

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Obtenção e caracterização de filmes finos de Bi3NbO7 pelo método dos precursores poliméricos

Pós-graduação em Engenharia Mecânica - FEG