903 resultados para Electrochemical impedance spectroscopy measurements


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The authors investigated the influence of defects on the piezoelectric and dielectric properties of Bi4Ti3O12 (BIT), SrBi4Ti4O15 (SBTi) and CaBi4Ti4O15 (CBTi144) thin films by x-ray photoemission spectroscopy measurements. In the SBTi film, Sr which is a nonpolarizable ion restricting the movement of Ti4+ ions and thus leads to a low piezoresponse. Meanwhile, the oxygen environment is quite different in the BIT and CBTi144 films exhibiting excellent piezoelectric properties. The piezoelectric coefficient and the dielectric behavior were larger for a-b axis oriented than for c axis-oriented films due to the defects created during the films crystallization. (c) 2007 American Institute of Physics.

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Two series of lead zirconate titanate (PZT) ceramics with composition Zr/Ti approximate to 53/47 have been prepared by the organic solution route. The effects on the electrical properties of calcination temperature in one series and of sintering time period in the other were examined. Dielectric constant, electrical conductivity and impedance spectroscopy results differed from one series to the other, probably due to differences in structure of the precursor powders, as seen by X-ray diffraction. Tetragonal and rhombohedral phases predominate in the powders used, respectively, in the calcined and sintered series. Physical and electrical behavior of ceramics prepared from predominantly rhombohedral powder suggests the evaporation of PbO. The presence of two semi-circles in impedance plots leads to the association of the low frequency semi-circle to the presence of PbO, which, apparently, was not eliminated from ceramics prepared from predominantly tetragonal powder. (C) 2001 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

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Siloxane-polypropyleneoxide (PPO) hybrids doped with sodium perchlorate (NaClO4) obtained by the sol-gel process were prepared with two PPO molecular weights (2000 and 4000 g/mol) and two sodium concentrations such as [O]/[Na] = 4 and 15 (O being the ether-type oxygen of PPO chains). The structure of these hybrids was investigated by Na-23 nuclear magnetic resonance (NMR) and X-ray absorption spectroscopy at the sodium K-edge (1071.8 eV) whereas complex impedance spectroscopy was used to determine their ionic conductivity. Three sodium sites were determined by NMR. The conjunction of NMR and X-ray absorption results allows us to identify one site in which Na is in a NaCl structure, a second one in which Na is in contact with perchlorate anions. The third site is attributed to mobile sodium species in interaction with the polymeric chain. The relative proportion of the different sites in the materials determines the ionic conductivity of the materials at room temperature: the largest ionic conductivity is 8.9 x 10(-6) Omega(-1) cm(-1) and is observed on the material with the larger amount (at least 85%) of sites in which sodium interacts with the polymer. (C) 2002 Elsevier B.V. B.V. All rights reserved.

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The electrical properties of the grain boundary region of electroceramic sensor temperature based on inverse spinel Zn7Sb2O12 were investigated at high temperature. The zinc antimoniate was synthesized by a chemical route based on the modified Pechini method. The electric properties of Zn7Sb2O12 were investigated by impedance spectroscopy in the frequency range from 5 Hz to 13 MHz and from 250 up to 600 degreesC. The grain boundary conductivity follows the Arrhenius law, with two linear branches of different slopes. These branches exhibit activation energies with very similar values; the low-temperature (less than or equal to350 degreesC) and high-temperature (greater than or equal to400 degreesC) regions are equal to 1.15 and 1.16 eV, respectively. Dissimilar behavior is observed on the relaxation time (tau) curve as a function of temperature, where a single slope is identified. The negative temperature coefficient parameters and nature of the polarization phenomenon of the grain boundary are discussed. (C) 2003 American Institute of Physics.

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Langmuir-Blodgett (LB) films from a ruthenium complex, mer-[RuCl3(dppb)(py)] (dppb = PPh2(CH2)(4)PPh2; py = pyridine) (Rupy), and from mixtures with varied amounts of polyaniline (PANi) were fabricated. Molecular-level interactions between the two components are investigated by surface potential, dc conductivity and Raman spectroscopy measurements, particularly for the mixed film with 10% of Rupy. For the latter, the better miscibility led to an interaction with Rupy inducing a decrease in the conducting state of PANi, as observed in the Raman spectra and conductivity measurement. The interaction causes the final film properties to depend on the concentration of Rupy, and this was exploited to produce a sensor array made up of sensing units consisting of 11-layer LB films from pure PANi, pure Rupy and mixtures with 10 and 30% of Rupy. It is shown that the combination of only four non-specific sensing units allows one to distinguish the basic tastes detected by biological systems, viz. saltiness, sweetness, sourness and bitterness, at the muM level. (C) 2003 Elsevier B.V. Ltd. All rights reserved.

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We have carried out dielectric and Raman spectroscopy studies at the 298-623 K temperature range in polycrystalline Pb0.70Sr0.30TiO3 thin films grown by a soft chemical method. The diffuse phase-transition behavior of the thin films was observed by means of the dielectric constant versus temperature curves, which show a broad peak. Such behavior was confirmed later by Raman spectroscopy measurements up to 823 K, indicating that a diffuselike phase transition takes place at around 548-573 K. The damping factor of the E(1TO) soft mode was calculated using the damped simple harmonic oscillator model. on the other hand, Raman modes persist above the tetragonal to cubic phase transition temperature although all optical modes should be Raman inactive. The origin of these modes was interpreted in terms of a breakdown of the microscopic local cubic symmetry by chemical disorder. The lack of a well-defined transition temperature and the presence of broad bands at some temperature interval above the ferroelectric-paraelectric phase-transition temperature suggested a diffuse nature of the phase transition. This result corroborates the dielectric constant versus temperature data, which showed a broad ferroelectric phase transition in this thin film. (C) 2004 American Institute of Physics.

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We have performed dielectric and micro-Raman spectroscopy measurements in the 298 - 673 K temperature range in polycrystalline Pb0.50Sr0.50TiO3 thin films prepared by a soft chemical method. The phase transition have been investigated by dielectric measurements at various frequencies during the heating cycle. It was found that the temperature corresponding to the peak value of the dielectric constant is frequency-independent, indicating a non-relaxor ferroelectric behavior. However, the dielectric constant versus temperature curves associated with the ferroelectric to paraelectric phase transition showed a broad maximum peak at around 433 K. The observed behavior is explained in terms of a diffuse phase transition. The obtained Raman spectra indicate the presence of a local symmetry disorder, due to a higher strontium concentration in the host lattice. The monitoring of some modes, conducted in the Pb0.50Sr0.50TiO3 thin films, showed that the ferroelectric tetragonal phase undergoes a transition to the paraelectric cubic phase at around 423 K. However, the Raman activity did not disappear, as would be expected from a transition to the cubic paraelectric phase. The strong Raman spectrum observed for this cubic phase is indicative that a diffuse-type phase transition is taking place. This behavior is attributed to distortions of the perovskite structure, allowing the persistence of low-symmetry phase features in cubic phase high above the transition temperature. This result is in contrast to the forbidden first-order Raman spectrum, which would be expected from a cubic paraelectric phase, such as the one observed at high temperature in pure PbTiO3 perovskite.

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The electrical and microstructural properties of SnO2-based varistors with the addition of 0.025 and 0.050 mol% of Fe2O3 have been characterised. Electric field (E) versus current density (J) curves showed that the effect of Fe2O3 addition is to increase both the non-linear coefficient and the breakdown voltage. Variations in the potential barrier height were inferred from impedance spectroscopy (IS) analysis. Through transmission electron microscopy (TEM), the presence of precipitates of secondary phases was confirmed. Samples with precipitates displayed poor electrical properties. (c) 2004 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

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This paper reports on the exposure of superhydrophobic polytetrafluoroethylene ( PTFE) coatings to common aqueous solutions which are used in biology, biotechnology and chemical sensor applications. Advancing contact angles as high as 173 degrees for aqueous solutions were measured on the PTFE surface. Water drop sliding angles at 2 degrees show a very low contact angle hysteresis. X-ray photoelectron spectroscopy measurements confirm that aqueous solutions can move or stay on the superhydrophobic surface without contamination. Owing to the chemical inertness of the polymer, these results indicate that superhydrophobic PTFE can be used in lab-on-a-chip and multi-sensor devices as well as in biological cultures, where aqueous solutions meet solid surfaces, without contaminating the interface.

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Intense and broad visible photoluminescent (PL) band in structurally disordered SrWO4 compounds was observed at room temperature. The polycrystalline scheelite strontium tungstate (SrWO4) samples prepared by the polymeric precursor method at different temperatures of annealing were structurally characterized by x-ray diffraction and Fourier transform Raman spectroscopy measurements. Quantum-mechanical calculations showed that the local disorder in the cluster of the network modifiers Sr has a very important role in the charge transfer. The experimental and theoretical results are in good agreement, indicating that the generation of the intense visible PL band can be related to short-range order-disorder degree in the scheelite structure. (c) 2006 American Institute of Physics.

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Since high-temperature superconductors were discovered, several studies have been made on their physical properties, attempting to associate them to the origin of superconductivity. Obviously, the oxygen atoms interstitially dissolved in the matrix have an important role in superconductivity, since they move easily in the lattice. In addition, they contribute to hole creation in the CuO2 planes. Anelastic spectroscopy ( internal friction) measurements are sensitive tools for the study of defects in solids, in particular for oxygen mobility. In this paper, Bi2Sr2CaCu2O8+y samples with several different amounts of interstitial oxygen were analysed by means of anelastic spectroscopy measurements. The measurements were performed by using a torsion pendulum operating at a frequency of about 40 Hz. Complex relaxation structures were observed and attributed to the shift of the oxygen interstitial atoms in BiO chains.

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Transparent, flexible, and luminescent EU3+-doped siloxane-poly(ethylene glycol) (PEG) nanocomposites have been obtained by the sol-gel process. The inorganic (siloxane) and organic PEG phases are usually linked by weak bonds (hydrogen bonds or van der Waals forces), and small-angle X-ray scattering (SAXS) measurements suggest that the structure of these materials consists of fractal siloxane aggregates embedded in the PEG matrix. For low Eu3+ contents, n = 300 and n = 80, the aggregates are small and isolated and their fractal dimensions are 2.1 and 1.7, respectively. These values are close to those expected for gelation mechanisms consisting of reaction-limited cluster-cluster aggregation (RLCCA) and diffusion-limited cluster-cluster aggregation (DLCCA). For high Eu3+ content, SAYS results are consistent with a two-level structure: a primary level of siloxane aggregates and a second level, much larger, formed by the coalescence of the primary ones. The observed increase in the glass transition temperature for increasing Eu3+ content is consistent with the structural model derived from SAXS measurements. Extended X-ray absorption fine structure (EXAFS) and luminescence spectroscopy measurements indicate that under the experimental conditions utilized here Eu3+ ions do not strongly interact with the polymeric phase.

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The laser Welding process was introduced into dentistry by the end of the 1980s, resulting on a great impulse to that area with the development of cheaper and smaller equipment, using simpler technique. This allowed greater use of that process on the confection of prostheses compared to the brazing process since the heat source for that process is a concentrated light beam of high power, which minimizes distortion problems on the prosthetic pieces. Ag-Pd-Au-Cu alloy used on the confection of dental implant prostheses was observed before and after subjection to the laser welding process. The microstructure was analyzed with the. use of optic microscopy and the corrosion resistance was studied by the traditional electrochemical techniques and by electrochemical impedance, under environmental conditions simulating the aggressiveness found in the mouth cavity. A structural change was detected on the weld area, which presented a refined microstructure deriving from the high-speed cooling. The base metal out of the weld area presented a fusion coarse microstructure. The electrochemical essays showed differences on the potentiodynamic polarization behavior in both weld and metal base areas, indicating superior corrosion resistance in the weld area. The impedance spectra were characterized by capacitive distorted components, presenting linear impedance in the low frequencies area. (C) 2002 Elsevier B.V. B.V. All rights reserved.

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Ultra-fine powders of Na1-xLixNbO3 (x=0; 0.06; 0.09; 0.12) were synthesized by the Polymeric Precursors Method. Such powders had their orthorhombic structures determined by X-ray diffraction and their surface area determined by BET isotherms (less than 10 m(2) g(-1)). Densification was followed by dilatometric study. The powders, calcined at 700 degrees C for 5 h, were sintered at 1290 degrees C during 2 h under ambient atmosphere with no application of extra pressure. The samples with relative densities higher than 95% were analyzed by impedance spectroscopy at room temperature, under a signal amplitude of 1 V-rms. Dielectric constants of about 180 and dielectric loss factor of about 0.03 were measured showing small dependence with frequency. The electrical properties were similar to those obtained for samples sintered by hot pressing. (C) 1999 Elsevier B.V. Limited and Techna S.r.l. All rights reserved.

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We report the preparation and characterization of yttria-stabilized zirconia/nickel oxide composites (YSZ/NiO). This composite is the precursor material of the cermet YSZ/Ni, which is used as solid oxide fuel cell anode material. The performance of the anode is strongly dependent on the microstructural properties of the cermet. Therefore, the control of the microstructure of the YSZ/NiO composite is a key step for the fabrication of high-performance anodes. In this study, the composites were prepared by a modified liquid mixture technique. Scanning electron microscopy analysis evidenced the good dispersion of the phases and that NiO nanoparticles are spread over the YSZ surface. Sintered pellets were studied by X-ray diffraction and impedance spectroscopy. The main results show that the composite is comprised of a well-dispersed mixture of the two phases. The electrical conductivity data show that there is a strong dependence of the transport mechanism on the relative composition of phases. (c) 2005 Elsevier Ltd. All rights reserved.