Montmorillonite (MMT) effect on the structure of poly(oxyethylene) (PEO)-MMT nanocomposites and silica-PEO-MMT hybrid materials

In this work we report the effects of incorporation of variable amounts (0.5-25%w/w) of montmorillonite in poly(oxyethylene) based materials in order to decrease the polymer crystallinity. Two different classes of materials were studied: silica-poly(oxyethylene)-montmorillonite hybrids prepared by the sol-gel route and poly(oxyethylene)-montmorillonite nanocomposites prepared by mixing the dry clay or the clay aqueous suspension into the melt poly(oxyethylene). The effects of monternorillonite loading on the poly(oxyethylene) crystallization control and on the nanostructural features were investigated by X-ray powder diffraction, small-angle X-ray scattering and differential scanning calorimetry. Experimental results show that free montmorillonite layers coexist with open aggregates and tactoids in the poly(oxyethylene)-montmorillonite nanocomposites, with different features depending on the filler proportion and preparation route. The intercalation of polymer chains in montmorillonite galleries markedly hinders the crystallization of the poly(oxyethylene) matrix. For hybrids materials the silica phase favors the exfoliation of montmorillonite tactoids, so that samples are predominantly constituted by dispersed platelets. (c) 2006 Elsevier B.V. All rights reserved.

Effect of ceria content on the sintering of ZrO2 based ceramics synthesized from a polymeric precursor

Zirconia-ceria powders with ceria concentration varying from 0 to 12 mol% were synthesized using a polymeric precursor route based on the Pechini process. Powder characteristics were evaluated with regard to the crystallite size, BET surface area, phase distribution, nitrogen adsorption/desorption behavior, and agglomeration state. Sintering was studied considering the shrinkage rate, densification, grain size, and phase evolution. It was demonstrated that the synthesis method is effective to prepare nanosized powders of tetragonal zirconia single-phase. Sinterability mainly depended on the agglomeration state of powders and the monoclinic phase content, fully tetragonal zirconia ceramic, with grain size of 2.4 mu m, was obtained after addition of at least 9 mol% ceria and sintering at 1500 degrees C for 4 h. (C) 2000 Elsevier B.V. Ltd. All rights reserved.

Effect of the heat flux direction on electrical properties of SrBi2Nb2O9 thin films crystallized using a microwave oven

Ferroelectric SrBi2Nb2O9 (SBN) thin films were prepared by the polymeric precursors method and deposited by spin coating onto Pt/Ti/SiO2/Si substrate and crystallized using a domestic microwave oven. It was studied the influence of the heat flux direction and the duration of the thermal treatment on the films crystallization. An element with high dielectric loss, a SiC susceptor, was used to absorb the microwave energy and transfers the heat to the film. Influence of the susceptor position to the sample crystallization was verified, the susceptor was, placed or below the substrate or above the film. The SBN perovskite phase was observed after a thermal treatment at 700 degreesC for 10 min when the susceptor was placed below the substrate and for 30 min when the susceptor was placed above the film. Electrical measurements revealed that the film crystallized at 700 degreesC for 10 min, with the susceptor placed below the film, presented dielectric constant, dielectric loss, remanent polarization and coercive field of, 67, 0.011, 4.2 muC/cm(2) and 27.5 kV/cm, respectively. When the films were crystallized at 700 degreesC for 30 min, with the susceptor placed above the film, the dielectric constant was 115 and the dissipation factor was around of 0.033, remanent polarization and coercive field were 10.8 muC/cm(2) and 170 kV/cm, respectively. (C) 2003 Elsevier B.V. All rights reserved.

Effect of the excess of bismuth on the morphology and properties of the BaBi2Ta2O9 ceramics

In this study, the effect of bismuth content on the crystal structure, morphology and electric properties of barium-bismuth-tantalate (BBT) ceramics was explored with the aid of X-ray diffraction (XRD), scanning electron microcopy (SEM), dielectric properties and ferroelectric hysteresis loops. BaBi2Ta2O9 (BBT) ceramics have been successfully prepared by the solid-state reaction. The BBT phase was crystallized at 900 degreesC for 2 h. The excess of bismuth controls the grain size, affecting the density of the material. Measurements of dieletric constant and dieletric losses confirm that the material is a ferroeletric with a Curie temperature around 77 degreesC. The dieletric constant measured at room temperature was 400, with a dielectric loss of 0.03. Both the phase-transition behaviour and ferroelectric properties, such as spontaneous polarization (P-s), showed a dependence on Bi content. (C) 2004 Elsevier B.V. All rights reserved.

The effect of isostructural seeding on the microstructure and piezoelectric properties of PZT ceramics

Pechini's method was used to prepare lead titanate zirconate with Zr/Ti ratio equal to 53/47. X-ray diffraction data revealed the presence of a rhombohedral phase, rich in zirconium, due to difference in carbonate stabilities, in PZT ceramics calcined at 600 degrees C. Infrared spectroscopy presented COO- bonds in the 1400 cm(-1) region, which disappeared after calcining at 700 degrees C. Seeds with rhombohedral (PZT 57/43) or tetragonal structure (PZT 45/55) were added to the precursor. The microstructure was differentially influenced by the nature of seed particles. Rhombohedral nuclei promoted preferential crystallization of lead zirconate. This heterogeneity directly reflected on values of k(p) and d(33). (C) 1999 Elsevier B.V. Limited and Techna S.r.l. All rights reserved.

Effect of commercial mouthwashes on the corrosion resistance of Ti-10Mo experimental alloy

The purpose of this work was to evaluate the effect of three commercial mouthwashes on the corrosion resistance of Ti-10Mo experimental alloy. Experiments were made at 37.0 +/- 0.5 degrees C in a conventional three-compartment double wall glass cell containing commercial mouthwashes. Three mouthwashes with different active ingredients were tested: ( I) 0.05% sodium fluoride + 0.03% triclosan; (II) 0.5 g/l cetylpyridinium chloride + 0.05% sodium fluoride; (III) 0.12% chlorohexidine digluconate. The assessment of the individual effect of active ingredients was studied by using 0.05% sodium fluoride. Commercially pure titanium (CP Ti) was used as control. Microstructures from Ti-10Mo experimental alloy and CP Ti were also evaluated using optical microscopy. Ti-10Mo as-cast alloy shows the typical rapidly cooled dendrites microstructure (beta phase) while CP Ti has exhibited a metastable martensitic microstructure. Electrochemical behavior of dental materials here studied was more affected by mouthwash type than by Ti alloy composition or microstructure. In both alloys passivation phenomenon was observed. This process may be mainly related to Ti oxides or other Ti species present in spontaneously formed film. Small differences in passive current densities values may be connected with changes in film porosity and thickness. Protective characteristics of this passive film are lower in 0.05% sodium fluoride + 0.03% triclosan mouthwash than in the other two mouthwashes tested.

Effect of niobia on the crystal structure and dielectric characteristics of Pb(Zr0.45Ti0.55)O-3 prepared from polymeric precursor

The influence of niobia addition on the phase formation and dielectric properties of Pb(Zr0.45Ti0.55)O-3 powder prepared from polymeric precursor was analyzed. The weight fraction and unit-cell volume of the tetragonal phase decreased, and the mass fraction of the rhombohedral phase increased, with increasing niobia concentration. The rhombohedral unit-cell volume increased up to 5 mol% of added Nb and then decreased. Small amounts of pyrochlore and tetragonal zirconia phases were observed in PZT powder with more than 10 mol% Nb. These results were interpreted as an indication that the Nb ion was substituted for the zirconium ion in the tetragonal phase. For sintered PZT samples at 1100 degrees C, no free-zirconia phase was observed. The dielectric constant increased with the niobia addition up to 5 mol% and decreased for higher concentrations. The Curie temperature decreased with niobia addition up to 10 mol% before the formation of pyrochlore phase. (C) 2000 Elsevier B.V. Ltd. All rights reserved.

Study of Ti-modified columbite route and the effect of lithium doping in 0.9PMN-0.1PT ceramics

The influence of lithium on the structural characteristics of PMN-PT ceramic was studied. The synthesis of PMN-PT powders using this precursor leads to the formation of high amount of perovskite phase. The insertion of Li(+) ions in B-site affects the microstructure because the rise in mass transport changes the mechanical characteristics of sintered ceramic. Higher values of K(m) and T(m) were gotten when lithium is inserted into perovskite phase. Secondary phase was found when lithium content increase beyond 1 mol%, besides the occurrence of transgranular fractures in sintered ceramic. Also, the additive acts increasing the relaxor behavior.

Linear readout of dynamic phase modulation index in an optical voltage sensor using the new J(1) ... J(3) spectral method

The J(1)...J(3) is a recent optical method for linear readout of dynamic phase modulation index in homodyne interferometers. In this work, the J(1)... J(3) method is applied to measure voltage in an optical voltage sensor. Based on the classical J(1)...J(4) method, the J(1)... J(3) technique shows to be more stable to phase drift and simpler for implementation than the original one. The sensor dynamic range is enhanced. The agreement between theoretical and experimental results, based on 1/f noise, is demonstrated.

THE EFFECT OF POSITRONIUM FORMATION IN POSITRON ALKALI-ATOM SCATTERING

We study e+-Na, e+-K, and e+-Rb scattering using the close coupling approach in the static and coupled static expansion schemes. We calculate partial wave elastic scattering phase shifts and total elastic and Ps formation cross sections up to an incident positron energy of 100 eV. The effect of the positronium formation channel on the elastic channel is found to be strong in all cases up to an incident positron energy of 10 eV. We also make an estimate of the total cross section which exhibits a minimum as a function of energy at low energies.

Effect of cytokines on the in vitro fungicidal activity of monocytes from paracoccidioidomycosis patients

Peripheral blood monocytes obtained from paracoccidioidomycosis patients and healthy individuals were preactivated with recombinant gamma interferon (IFN-gamma) in different concentrations (250, 500 and 1000 U/ml) and evaluated for fungicidal activity against Paracoccidiodes brasiliensis strain 18 (Pb 18, high-virulence strain) and strain 265 (Pb 265, low-virulence strain) by plating of cocultures and counting of colony-forming units, after 10 d. Monocytes from healthy individuals failed to present fungicidal activity against P. brasiliensis even after IFN-gamma activation at the three concentrations. However, patient, monocytes activated with IFN-gamma (1 000 U/ml) showed a significant fungicidal activity when compared to that obtained with non-activated or activated cells with other IFN-gamma concentrations (250 and 500 U/ml). Moreover,,patient monocytes presented higher fungicidal activity than the control, even before the activation process. These results may be explained by the activation state of patients' cells as a function of the in vivo contact with the fungus, which was confirmed by their higher capacity to release H2O2 in vitro. Unlike the results obtained with Ph 18, patient and control cells presented a significant fungicidal activity against Pb 265, after priming with IFN-gamma. These results are explained by the higher levels of TNF-alpha in supernatants of cultures challenged with Pb 265. Moreover, higher levels of the cytokine were obtained in patient cell supernatants. Taken together, our results suggest that for effective killing of P. brasiliensis by monocytes, an initial activation signal induced by IFN-gamma is necessary to stimulate the cells to produce TNF-alpha. This cytokine may be involved, through an autocrine pathway, in the final phase activation process. The effectiveness of this process seems to depend on the virulence of the fungal strain and the activation state of the challenged cells. (C) 2003 Editions scientifiques et medicales Elsevier SAS. All fights reserved.

Effect of PbO excess on the formation of lead magnesium niobate perovskite by the columbite method

The effect of lead excess on the pyrochlore-type formation in Pb(Mg1/3Nb2/3)O-3 (PMN) powders has been investigated. The polymeric precursor method was used in the synthesis of the columbite in association to the partial oxalate method to synthesize the PMN powder samples. Structure refinement of the columbite precursor and PMN powders was carried out using the Rietveld method. The quantitative phase analysis showed that the amount of perovskite phase is not affected by PbO excess, but a great excess drives the pyrochlore-type formation so that 3 wt.% of PbO causes the predominance of Mg-containing pyrochlore phase. Using the refined data obtained from the Rietveld refinement, the compositional fluctuation in the perovskite phase was calculated from Nb/Mg ratio values and Pb occupation factor. Mg inclusion occurs concomitant with Ph one into PMN perovskite phase and this effect is directed by PbO excess during powder synthesis. (C) 2003 Elsevier B.V. All rights reserved.

Luminescence effect in amorphous PLT

Amorphous and crystalline powder of PLT phase was synthesized by using the Pechini method. Infrared (FTIR) analysis of the polymeric resin shows intense bands of organic materials from 250 to 1620 cm(-1). X-ray diffraction (XRD) and Raman spectra of calcined powder at different temperatures show amorphous phase at 450 degrees C/3 h, semi-crystalline phase at 550 degrees C/3 h and a crystalline phase at 800 degrees C/3 h. Luminescence effect was observed in amorphous powder calcined from 300 to 350 degrees/3 h with broad absorption peaks in 579 nm at 300 degrees C/3 h and 603 rum at 350 degrees C/3 h, respectively. The photoluminescence effect is attributed to emissions of Ti -> 0 directly from the oxygen 2p orbital (valence band) to the titanate 3d orbital (conduction bands). (c) 2004 Elsevier Ltd. All rights reserved.

Study of the effect of the peptide loading and solvent system in SPPS by HRMAS-NMR

The SPPS methodology has continuously been investigated as a valuable model to monitor the solvation properties of polymeric materials. In this connection, the present work applied HRMAS-NMR spectroscopy to examine the dynamics of an aggregating peptide sequence attached to a resin core with varying peptide loading (up to 80%) and solvent system. Low and high substituted BHAR were used for assembling the VQAAIDYING sequence and some of its minor fragments. The HRMAS-NMR results were in agreement with the swelling of each resin, i.e. there was an improved resolution of resonance peaks in the better solvated conditions. Moreover, the peptide loading and the attached peptide sequence also affected the spectra. Strong peptide chain aggregation was observed mainly in highly peptide loaded resins when solvated in CDCl3. Conversely, due to the better swelling of these highly loaded resins in DMSO, improved NMR spectra were acquired in this polar aprotic solvent, thus enabling the detection of relevant sequence-dependent conformational alterations. The more prominent aggregation was displayed by the VQAAIDYING segment and not by any of its intermediary fragments and these findings were also corroborated by EPR studies of these peptide-resins labelled properly with an amino acid-type spin probe. Copyright (c) 2005 European Peptide Society and John Wiley & Sons, Ltd.

Effect of boron powder purity on superconducting properties of MgB2

The effect of the properties of starting boron powders on the superconducting properties of MgB2 has been studied. The 92% and 96% pure powders produce lower surface reactivity and larger particle size than the 99% boron powder, as can be seen from Brunauer - Emmett - Teller (BET) and scanning electron microscopy (SEM) results, indicating that the low purity powders cannot be used to archive the same superconducting properties as those of samples made from pure 99% boron powder. However, the purity of 92% and 96% boron powders can be improved by using a simple chemical process, leading to enhanced magnetic critical current densities J(c). From x-ray diffraction (XRD) measurement, oxide impurity has been observed, which might be originated from the B2O3 phase in the boron powders. In order to get high performance MgB2, it is obviously important to control the phase composition and microstructure of amorphous boron starting powders and solid reaction conditions.