Structure of nanoporous zirconia-based powders synthesized by different gel-combustion routes

Zirconia-based ceramics that retain their metastable tetragonal phase at room temperature are widely studied due to their excellent mechanical and electrical properties. When these materials are prepared from precursor nanopowders with high specific surface areas, this phase is retained in dense ceramic bodies. In this work, we present a morphological study of nanocrystalline ZrO2-2.8 mol% Y2O3 powders synthesized by the gel-combustion method, using different organic fuels - alanine, glycine, lysine and citric acid - and calcined at temperatures ranging from 873 to 1173 K. The nanopore structures were investigated by small-angle X-ray scattering. The experimental results indicate that nanopores in samples prepared with alanine, glycine and lysine have an essentially single-mode volume distribution for calcination temperatures up to 1073 K, while those calcined at 1173 K exhibit a more complex and wider volume distribution. The volume-weighted average of the nanopore radii monotonically increases with increasing calcination temperature. The samples prepared with citric acid exhibit a size distribution much wider than the others. The Brunauer-Emmett-Teller technique was used to determine specific surface area and X-ray diffraction, environmental scanning electron microscopy and transmission electron microscopy were also employed for a complete characterization of the samples.

Sintering of tin oxide processed by slip casting

Sintering of SnO 2 compacts, obtained through slip casting, was studied by means of dilatometry, Hg porosimetry, scanning electron microscopy, and density measurement (Archimedes method). Sintering is strongly influenced by the green microstructure. Moreover, the sintering mechanisms are not dependent on the slurries' solid content up to 50% of solids in volume. Above this value, agglomerates are formed, leading to differential sintering inside and among the agglomerates. Another important point is the reduction of the temperature of maximum shrinkage rate when compared to tin oxide processed by isostatic pressing. This reduction is more accentuated when ammonium hydroxide is added to the suspension. (C) 2000 Published by Elsevier Science Ltd. All rights reserved.

Magnetoelectric coefficient in strontium ruthenate buffered lanthanum modified bismuth ferrite thin films grown by chemical method

This paper focuses on the magnetoelectric coupling (ME) at room temperature in lanthanum modified bismuth ferrite thin film (BLFO) deposited on SrRuO 3-buffered Pt/TiO 2/SiO 2/Si(100) substrates by the soft chemical method. BLFO film was coherently grown at a temperature of 500 °C. The magnetoelectric coefficient measurement was performed to evidence magnetoelectric coupling behavior. Room temperature magnetic coercive field indicates that the film is magnetically soft. The maximum magnetoelectric coefficient in the longitudinal direction was close to 12 V/cmOe. Dielectric permittivity and dielectric loss demonstrated only slight dispersion with frequency due the less two-dimensional stress in the plane of the film. Polarization reversal was investigated by applying dc voltage through a conductive tip during the area scanning. We observed that various types of domain behavior such as 71 ° and 180° domain switching, and pinned domain formation occurred. Copyright © 2009 American Scientific Publishers All rights reserved.

Morphological and luminescent studies on nanosized Er, Yb-Yttrium oxide up-converter prepared from different precursors

In this paper, we report luminescent and morphological studies with yttrium oxide samples doped with ytterbium and erbium. The samples were prepared by the combustion method and also from different precursors: oxalate, basic carbonate and polymeric resin. All powders were identified Lis being an yttrium oxide with a C-form structure, independent of the employed precursor. From mean crystallite size measurements, it was verified that oxides prepared through the polymeric precursor and combustion methods lead to the smallest crystallite size. Particle shape and size were investigated by SEM and TEM, and showed that both the oxalate precursor and the combustion methods do not provide oxide materials of suitable shape or size, on the other hand. The basic carbonate and polymeric precursors resulted in spherically shaped particles with an average diameter of 90 and 15 run. respectively, Upon 980 run diode laser excitation, green and red emission lines were detected for all samples and were assigned to the H-2(11/2) S-4(3/2) -> I-4(15/2) and (4)Fg(9/2) -> 4I(15/12) transitions, respectively. Such transitions are characteristic for Er3+ and result from energy transfer from Yb3+ energy levels, F-2(7/2) -> F-2(5/2). A relationship between the decrease in the mean crystallite size and the enhancement in red emission was also established as well as the influence of the presence of a high percentage of Yb-3 Both factors promote ET from Yb3+ (F-2(5/2)) to Er3+ (I-4(11/2)). (c) 2004 Elsevier B.V. All rights reserved.

The synergistic effects of Nb/Mn and Sb/Mn on the microstructure and electrical characteristics of BaTiO3 based ceramics

The microstructure and dielectric properties of Nb-Mn or Sb-Mn codoped BaTiO3 compositions were investigated. Starting ceramics powders were prepared by Pechini method. The composites were sintered at 1310°C and 1330°C in an air atmosphere for two hours. The microstructure and compositional investigations were done with SEM equipped with EDS. Two distinguish microstructure regions are observed in Nb/0.05Mn doped BaTiO 3 ceramics sintered at low temperature. The first, large one, with grain sizes from 5-40 μm and the second region with small grain sizes from 1 to 5 μm. Sintering at higher temperature, independent of Mn content, enables to achieve a uniform microstructure with grains less than 6 μm. In Sb/Mn doped ceramics, for both sintering temperatures, bimodal microstructures with fine grained matrix and grains up to 10 μm is formed. The highest value of permittivity at room temperature and the greatest change of permittivity in function of temperature are observed in Nb/0.01Mn doped ceramics compared to the same ones in Sb/Mn doped ceramics. The greatest shift of Curie temperature towards lower temperature has been noticed in Sb/Mn BaTiO3 ceramics compared to others samples. In all investigated samples the dielectric loss after initially large values at low frequency maintains a constant value for f>3 kHz.

Análise estrutural e morfológica de ferrita NiFe2O4 dopada com cromo

This paper reports on the effect of the substitution of Fe3+ for Cr3+ ions in the spinel lattice of the powders was investigated. Nickel ferrite powders with a NiFe2-xCrxO4 nominal composition (x = 0.0; 0.5; 1.0 and 1.5 mol of the chromium) were synthesized by combustion reaction using urea as fuel. The powders resulting were characterized by XRD, nitrogen adsorption by BET, SEM and Mössbauer spectroscopy (57Fe Mössbauer spectra). The results show that the substitution of the Fe3+ for Cr3+ions increased the crystalline degree of the phase, reduced the superficial area and consequently increased the particle size. The Mössbauer spectra of the samples also confirm the distribution of the particles size by the magnetic properties. Analyze of the spectra Mössbauer gives an estimate of the superparamagnetic and ferromagnetic particles behavior in each sample for several chromium concentrations.

Characterization of silica-carbon mesoporous matrix with embedded nickel nanoparticles synthesized by the polymeric precursor method

Nickel nanoparticles into silica-carbon matrix composites were prepared by using the polymeric precursor method. The effects of the polyester type and the time of pyrolysis on the mesoporosity and nickel particle dispersion into non-aqueous amorphous silica-carbon matrix were investigated by thermogravimetric analysis, adsorption/desorption isotherms and TEM. A well-dispersed metallic phase could be only obtained by using ethylene glycol. Weightier polyesters affected the pyrolysis process due to a combination of more amounts of carbonaceous residues and delaying of pyrolysis process. The post-pyrolyzed composites were successfully cleaned at 200 degrees C for I h in oxygen atmosphere leading to an increase in the surface area and without the occurrence of carbon combustion or nickel nanoparticles oxidation. The matrix composites presented predominantly mesoporous with pore size well defined in 38 angstrom, mainly when tetraethylene glycol was used as polymerizing agent. (C) 2007 Elsevier B.V. All rights reserved.

X-ray diffraction and mossbauer spectra of nickel ferrite prepared by combustion reaction

Nickel ferrite powders with a nominal NiFe2O4 composition were synthesized by combustion reaction using urea as fuel. The powder was obtained using a vitreous silica basin heated directly on a hot plate at 480 degrees C until self-ignition occurred. After combustion, the powder was calcined at 700 degrees C for 2 h. The formation of the spinel phase and the distribution of cations in the tetrahedral and octahedral sites of the crystal structure were investigated by the Rietveld method, using synchrotron X-ray diffraction data and Mossbauer spectroscopy. The material presented a crystallite size of 120 nm and magnetic properties. The resulting stoichiometry after the Rietveld refinement was (Fe-0.989(2) Ni-0.011(2)) [Fe-1.012(2) Ni-0.989(2)] O-4.

Preparation and structural characterization of vulcanized natural rubber nanocomposites containing nickel-zinc ferrite nanopowders

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

Structural and magnetic characterization of MnxZn1-xFe2O4 (x=0.2; 0.35; 0.65; 0.8; 1.0) ferrites obtained by the citrate precursor method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

The effect of preparation method and Sb content on SnO2-CuO sintering

The sintering behavior of SnO2-CuO system has been investigated for two preparation methods and as a function of antimony concentration. A chemical preparation (Pechini's method) resulted in powders with smaller particle sizes than for a conventional oxide mixture. This led to smaller grain sizes in Pechini's method ceramics. The microstructures were heterogeneous in both systems, showing grain coarsening. The densification was aided by liquid phase formation, due to copper, in both systems, but the temperature of maximum shrinkage rate was larger for the Pechini's method ceramic because copper had to diffuse to the grain surface. Independently of the preparation method, antimony did not aid densification, and increasing its concentration led to a higher densification temperature and lower shrinkage rate. (C) 2003 Kluwer Academic Publishers.

A Simple Method Based on ICP-MS for Estimation of Background Levels of Arsenic, Cadmium, Copper, Manganese, Nickel, Lead, and Selenium in Blood of the Brazilian Population

Throughout the world, biomonitoring has become the standard for assessing exposure of individuals to toxic elements as well as for responding to serious environmental public health problems. However, extensive biomonitoring surveys require rapid and simple analytical methods. Thus, a simple and high-throughput method is proposed for the determination of arsenic (As), cadmium (Cd), copper (Cu), manganese (Mn), nickel (Ni), lead (Pb), and selenium (Se) in blood samples by using inductively coupled plasma-mass spectrometry (ICP-MS). Prior to analysis, 200 l of blood samples was mixed with 500 l of 10% v/v tetramethylammonium hydroxide (TMAH) solution, incubated for 10 min, and subsequently diluted to 10 ml with a solution containing 0.05% w/v ethylenediamine tetraacetic acid (EDTA) + 0.005% v/v Triton X-100. After that, samples were directly analyzed by ICP-MS (ELAN DRC II). Rhodium was selected as an internal standard with matrix-matching calibration. Method detection limits were 0.08, 0.04, 0.5, 0.09, 0.12, 0.04, and 0.1 g//L for As, Cd, Cu, Mn, Ni, Pb, and Se, respectively. Validation data are provided based on the analysis of blood samples from the trace elements inter-\comparison program operated by the Institut National de Sante Publique du Quebec, Canada. Additional validation was provided by the analysis of human blood samples by the proposed method and by using electrothermal atomic absorption spectrometry (ETAAS). The method was subsequently applied for the estimation of background metal blood values in the Brazilian population. In general, the mean concentrations of As, Cd, Cu, Mn, Ni, Pb, and Se in blood were 1.1, 0.4, 890, 9.6, 2.1, 65.4, and 89.3 g/L, respectively, and are in agreement with other global populations. Influences of age, gender, smoking habits, alcohol consumption, and geographical variation on the values were also considered. Smoking habits influenced the levels of Cd in blood. The levels of Cu, Mn, and Pb were significantly correlated with gender, whereas Cu and Pb were significantly correlated with age. There were also interesting differences in Mn and Se levels in the population living in the north of Brazil compared to the south.

Sintering of cobalt and strontium doped lanthanum chromite obtained by combustion synthesis

Lanthanum chromite (LaCrO3) is one of the most adequate materials for use as interconnector in solid oxide fuel cell (SOFC) applications, due to its intrinsic properties, namely its good electrical conductivity and resistance to environment conditions in fuel cell operations. Due to difficulties in sintering, additives are usually added to help in the densification process. In this work, the influence of added cobalt and strontium, in the sintering of LaCrO3 obtained by combustion synthesis was studied. The starting materials were respectively nitrates of chromium, lanthanum, cobalt and strontium, and urea was used as fuel. The results show that by increasing the strontium and cobalt concentrations it is possible to reduce the temperature of sintering. Using both additives, the sintering processes took place in lesser times than normally used for this material, as well as greater values of density were attained.

Mechanisms of phase formation along the synthesis of Mn-Zn ferrites by the polymeric precursor method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

A simple method based on ICP-MS for estimation of background levels of arsenic, cadmium, copper, manganese, nickel, lead, and selenium in blood of the Brazillian population

Throughout the world, biomonitoring has become the standard for assessing exposure of individuals to toxic elements as well as for responding to serious environmental public health problems. However, extensive biomonitoring surveys require rapid and simple analytical methods. Thus, a simple and high-throughput method is proposed for the determination of arsenic (As), cadmium (Cd), copper (Cu), manganese (Mn), nickel (Ni), lead (Pb), and selenium (Se) in blood samples by using inductively coupled plasma–mass spectrometry (ICPMS). Prior to analysis, 200 ml of blood samples was mixed with 500 ml of 10% v/v tetramethylammonium hydroxide (TMAH) solution, incubated for 10 min, and subsequently diluted to 10 ml with a solution containing 0.05% w/v ethylenediamine tetraacetic acid (EDTA) + 0.005% v/v Triton X-100. After that, samples were directly analyzed by ICP-MS (ELAN DRC II). Rhodium was selected as an internal standard with matrix-matching calibration. Method detection limits were 0.08, 0.04, 0.5, 0.09, 0.12, 0.04, and 0.1 mg//L for As, Cd, Cu, Mn, Ni, Pb, and Se, respectively. Validation data are provided based on the analysis of blood samples from the trace elements inter-\comparison program operated by the Institut National de Santé Publique du Quebec, Canada. Additional validation was provided by the analysis of human blood samples by the proposed method and by using electrothermal atomic absorption spectrometry (ETAAS). The method was subsequently applied for the estimation of background metal blood values in the Brazilian population. In general, the mean concentrations of As, Cd, Cu, Mn, Ni, Pb, and Se in blood were 1.1, 0.4, 890, 9.6, 2.1, 65.4, and 89.3 mg/L, respectively, and are in agreement with other global populations. Influences of age, gender, smoking habits, alcohol consumption, and geographical variation on the values were also considered. Smoking habits influenced the levels of Cd in blood. The levels of Cu, Mn, and Pb were significantly correlated with gender, whereas Cu and Pb were significantly correlated with age. There were also interesting differences in Mn and Se levels in the population living in the north of Brazil compared to the south.