The effect of Eu3+ concentration on the Y2O3 host lattice obtained from citrate precursors

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

Luminescent and morphological study of Sr2CeO4 blue phosphor prepared from oxalate precursors

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

Activity of Mo(II) allylic complexes supported in MCM-41 as oxidation catalysts precursors

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

Effect of magnesium on structure and properties of LiNbO3 prepared from polymeric precursors

The effect of magnesium addition on the phase formation and electric properties of LiNbO3 powder prepared from polymeric precursor was analyzed. It was shown that the unit-cell volume of the rhombohedral phase decreased with increasing magnesium concentration. Small amounts of secondary phases were observed in LiNbO3 powder doped with 5 and 10 mol% Mg+2. These results indicated that the Mg+2 ion was substituted for niobium ion in the rhombohedral phase. The addition of Mg+2 promotes densification of LiNbO3 ceramics. It was noticed that the increase in additive concentration leads to a decrease of electric properties, K-p and d(33). This is due to formation of LiNb3O8 and MgNb2O6 phases at the grain boundaries. (C) 2002 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

Synthesis and characterization of antimony tartrate for ceramic precursors

Synthesis and characterization of antimony tartrate used as a precursor of ceramic powders obtained by Pechini's method were carried out. Antimony tartrate was chosen as a substitute for the antimony citrate commonly used in this chemical processing, because of difficulties in preparing the citrate. FTIR and TGA/DTA analysis showed that antimony tartrate, H-2[Sb-2(C4H2O6)(2)]. forms a polymeric structure. The procedure described indicates that the antimony chelate obtained is adequate for Pechini's method.

Attainment of lead titanate - Through the thermal decomposition of coprecipitated 8-hydroxyquinolinate precursors

Crystalline PbTiO3 was obtained through the thermal decomposition of 8-hydroxyquinolinate of lead(II) and that of titanium(IV), which was monitored by TG/DTG/DTA under different atmospheric conditions and with varying heating rates. The compound was prepared from adding 8-hydroxyquinoline solution in the solution of metallic ions Pb(II):Ti(IV) (1:1) Linder constant stirring at 3degreesC, having the pH adjusted to 10. The results of these investigations show that different thermal behavior related to the precursor occurred and also the consequent formation of residues which have different crystallinities. No carbonate residues from the thermal decomposition could be determined by XRD and IR. Only PbTiO3 was observed and confirmed by DSC at 470degreesC, temperature lower than the tetragonal-cubic transition.

Electrosynthesis of binuclear ruthenium complexes from [RuCl3(dppb)(L)] precursors [L = pyridine, 4-methylpyridine or dimethyl sulfoxide; dppb=1,4-bis(diphenylphosphino)butane]

Electrolysis has been examined as a method of synthesis for [(L)(dppb)Ru(mu-Cl)(3)RuCl(dppb)] complexes, where dppb = 1,4-bis(diphenylphosphino)butane and L = pyridine (py), 4-methylpyridine (4-pic) or dimethyl sulfoxide (DMSO), by using [RuCl3(dppb)(L)] as precursors. The products of the electrolysis were characterized by P-31-{H-1} NMR, cyclic voltammetry and near infrared spectroscopy. The presence of the [Ru2Cl5(dppb)(2)] complex in the electrochemical cell suggests a mechanism by which the starting original species from the bulk solution reacts with the reduced form [RuCl2(dppb)(L)] generated at the surface of the electrode. The crystal structure of the precursor mer-[RuCl3(dppb)(4-pic)] was determined by X-ray diffraction.

Local Er(III) environment in luminescent titanosilicates prepared from microporous precursors

The local environment of Er3+ ions in microporous titanosilicate ETS-10 and in synthetic narsarsukite and glassy materials obtained by calcination of ETS-10 has been investigated by EXAFS, Raman and photoluminescence spectroscopies. Er L-III-edge EXAFS studies of Er3+-doped ETS-10 support the view that the exchanged Er3+ ions reside close to the (negatively charged) TiO6 octahedra. In ETS-10, Er3+ is partially bonded to framework oxygen atoms and hydration water molecules. The Er...Ti distance (3.3 Angstrom) is similar to the Na...Ti distances (3.15-3.20 Angstrom) reported previously for Na-ETS-10. Although the exact location of the ErO6 units within the host structure of Er3+-doped synthetic narsarsukite is still an open question, it is most likely that Er3+ substitutes Ti4+ rather than Na+ ions. EXAFS spectroscopy indicates that no significant clustering of erbium atoms occurs in the titanosilicate samples studied. Evidence for the insertion of Er3+ ions in the framework of narsarsukite has been obtained by Raman spectroscopy. This is indicated by the increasing full-width at half-maximum (FWHM) of the 775 cm(-1) peak and the increasing intensity of the anatase peaks as the erbium content increases. In addition, as the narsarsukite Er3+ content increases a band at ca. 515 cm(-1) firstly broadens and subsequently a new peak appears at ca. 507 cm(-1).Er3+-doped narsarsukite exhibits a characteristic local vibrational frequency, (h) over bar omega ca. 330 cm(-1), with an electron-phonon coupling, g ca. 0.2, which constitutes additional evidence for framework Er3+ insertion. The number of lines in the infrared emission spectrum of synthetic narsarsukite indicates the presence of two optically-active erbium centres with very similar local environments and an average I-4(13/2) lifetime of 7.8 +/- 0.2 ms.

BaTiO3 obtained through metallic stearate precursors

Metallic stearates were used as precursors to obtain BaTiO3. Barium and titanium stearate mixtures were homogenized in ball mill containing some amount of ammonium stearate. The mixture of the precursors was evaluated by simultaneous TG/ DTA and TMA, and residues from thermal decomposition were characterized by XRD and SEM. It could be verified that the residues from the thermal decomposition in both oxidant and inert atmospheres were the BaTiO3 but with characteristic morphological and crystalline aspects depending on the experimental conditions in which the mixtures of precursors were obtained. (C) 2002 Elsevier B.V. B.V. All rights reserved.

The influence of crystallization route on the properties of lanthanum-doped Bi4Ti3O12 thin films prepared from polymeric precursors

Pure and lanthanum-doped Bi4Ti3O12 thin films were deposited on Pt/Ti/SiO2/Si substrate using a polymeric precursor solution. The spin-coated films were specular and crack-free and crystalline after annealing at 700 degreesC for 2 h. Crystallinity and morphological evaluation were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). Multilayered films obtained using the intermediate-crystalline layer route present a dense microstructure with spherical grains. Films obtained using the intermediate-amorphous layer, present elongated grains around 250 nm in size. The dielectric and ferroelectric properties of the lanthanum-doped Bi4Ti3O12 films are strongly affected by the crystallization route. The hysteresis loops are fully saturated with a remnant polarization and drive voltage of the films, heat-treated by the intermediate-crystalline (P-r = 20.2 muC/cm(2) and V = 1.35 V) and for the film heat-treated by amorphous route (P-r = 22.4 muC/cm(2) and V = 2.99 V). (C) 2004 Elsevier B.V. All rights reserved.

Cracks developed during SrTiO3 thin-film preparation from polymeric precursors

Strontium titanate (SrTiO3) thin films were prepared by dip-coating Si(111) single-crystal substrates in citrate solutions of ethylene glycol, considering several citric acid/ethylene glycol (CA/EG) ratios. Measurements of intrinsic viscosity indicate that increasing the amount of EG increases the precursors' polymeric chains and increases the weight loss. After deposition the substrates were dried on a hotplate (approximate to 150 degrees C); this was followed by heat treatment at temperatures ranging from 500 to 700 degrees C using heating and cooling rates of 1 degrees C min(-1). SEM and optical microscopy investigations of the sintered films obtained from different CA/EG ratios indicate that there is a critical thickness above which the films present cracks. This critical thickness for SrTiO3 films deposited on the Si(111) substrate is about 150 nm, Measurements of crack spacing as a function of film thickness indicate that the origin of cracks cannot be explained by the elastic behavior of the film but rather by the viscoelastic relaxation of the film during pyrolysis and sintering. Copyright (C) 1999 John Wiley & Sons, Ltd.

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.

Synthesis and characterization of 9.5/65/35 PLZT prepared from the polymeric precursors

The 9.5/65/35 PLZT was prepared from the polymeric precursors (the Pechini and partial oxalate process) and by sintering in two stages in an oxygen atmosphere. After thermal treatment at 400 degreesC, the powders were calcinated and sintered at 1200 degreesC with slow heating and cooling rates. The second stage of sintering consisted of hot pressing at the same temperature in oxygen atmosphere. After calcination of PLZT powders obtained by both methods, as well as after sintering of PLZT obtained by Pechini process, the paraelectric cubic phase was formed. After sintering of PLZT obtained by partial oxalate procedure, small tetragonality of crystal structure was observed. After hot pressing PLZT was pseudocubic. SEM microstructural analyses were carried out of the sintering and hot pressed samples and indicated the small grain size less than 2 mum. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Preparation of zinc sodium polyphosphates glasses from coacervates precursors. Characterisation of the obtained glasses, and their applications

A soft chemistry route is described to obtain glasses in the P2O5-Na2O-ZnO-H2O. It is based on the addition of zinc salts to coacervates prepared from sodium polyphosphate. The processing of these coacervates leads to polyphosphate glasses with the same properties as those of glasses prepared in the classical way. So far, little work has been implemented in this system using 'coacervate route'. However, it makes an attractive method for coating and joining processes on the industrial scale. As the anion associated to zinc may take part in the adhesion mechanism, coacervate formation has been studied using zinc chloride, nitrate and sulphate as starting materials. The physical properties of the glasses obtained by this method are reported and potential applications of zinc and silver coacervate are described. (C) 2002 Academie des sciences / Editions scientifiques et medicales Elsevier SAS.

Thermal properties of fluoride glasses and their gel precursors

Xerogels were prepared from zirconium, barium, aluminum, lanthanum and lithium acetates, corresponding to a Li containing ZBLA composition. The study of their thermal properties (DSC, TG/DTG, FT-IR) showed that they might be used as chemically stable precursors in the preparation of fluoride glasses. Hydrofluoric acid in solution was chosen as a mild fluorinating agent. This newly proposed technique of fluorinating allowed to obtain high quality ZBLALi glass which presents the advantage of higher thermal stability and homogeneity in comparison with the glass obtained using individual commercial fluorides.