Analysis of the Al-PANI interfaces by complex impedance spectroscopy

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Dielectric spectroscopy and thermally stimulated discharge current in PEEK film

A permissividade complexa de filmes de poli(eter-eter-cetona) (PEEK) foram investigados num grande intervalo de frequência. Não foram observados picos de relaxação no intervalo de frequência de 1,0 Hz a 10(5) Hz, mas no intervalo de baixa frequência (10-4 Hz) há uma evidência de pico, o qual também pode ser observado com medidas de corrente de despolarização termo-estimulada (TSDC). Este pico está relacionado com a transição vítrea do polímero. A energia de ativação relacionada a esta relaxação dipolar foi obtida e ovalor é Ea = 0,44 eV, que é similar à energia de ativação de muitos polímeros sintéticos. As cargas espaciais se mostraram importantes no mecanismo de condução como evidenciado nas medidas da corrente de despolarização.

Corrosion of the component phases presents in high copper dental amalgams. Application of electrochemical impedance spectroscopy and electrochemical noise analysis

The corrosion resistance of three of the constituent phases in high copper dental amalgams has been investigated by electrochemical methods in 0.9% NaCl solution. Polarization curves show corrosion potentials most positive for gamma(1)-Ag2Hg3, followed by Ag-Cu, and gamma-Ag3Sn in agreement with the order of corrosion resistance deduced from the corrosion currents. Complex plane impedance plots at the open circuit potential showed distorted semicircles with diffusional components at low frequency for Ag-Hg and Ag-Cu, while for gamma-Ag3Sn a layer of corrosion products is formed, partially or completely covering the surface of the electrode. Impedance and noise spectra have been compared in the frequency domain, and show good agreement. (C) 2004 Elsevier Ltd. All rights reserved.

Structural study of thin films prepared from tungstate glass matrix by Raman and X-ray absorption spectroscopy

Thin films were prepared using glass precursors obtained in the ternary system NaPO(3)-BaF(2)-WO(3) and the binary system NaPO(3)-WO(3) with high concentrations of WO(3) (above 40% molar). Vitreous samples have been used as a target to prepare thin films. Such films were deposited using the electron beam evaporation method onto soda-lime glass substrates. Several structural characterizations were performed by Raman spectroscopy and X-ray Absorption Near Edge Spectroscopy (XANES) at the tungsten L(I) and L(III) absorption edges. XANES investigations showed that tungsten atoms are only sixfold coordinated (octahedral WO(6)) and that these films are free of tungstate tetrahedral units (WO(4)). In addition, Raman spectroscopy allowed identifying a break in the linear phosphate chains as the amount of WO(3) increases and the formation of P-O-W bonds in the films network indicating the intermediary behavior of WO(6) octahedra in the film network. Based on XANES data, we suggested a new attribution of several Raman absorption bands which allowed identifying the presence of W-O and W=O terminal bonds and a progressive apparition of W-O-W bridging bonds for the most WO(3) concentrated samples (above 40% molar) attributed to the formation of WO(6) clusters. (C) 2008 Elsevier B.V. All rights reserved.

Absence of relaxor-like ferroelectric phase transition in (Pb,Sr)TiO3 thin films

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.

Dielectric loss and phase transition of sodium potassium niobate ceramic investigated by impedance spectroscopy

The dielectric permittivity of Na0.80K0.20NbO3 ceramic was investigated by impedance spectroscopy. The dielectric characterization was performed from room temperature to 800 degreesC, in the frequency range 5 Hz-13 MHz. The bulk permittivity was derived by the variation of the imaginary part of the impedance as a function of reciprocal angular frequency. The permittivity values as a function of temperature showed two maxima. The first maximum is very similar at 200degreesC and the second one positioned at around 400degreesC, which was associated to Curie's temperature. The evolution of the complex permittivity as a function of frequency and temperature was investigated. At low frequency dispersion was investigated in terms of dielectric loss. The Na0.80K0.20NbO3 showed a dissipation factor between 5 and 40 over a frequency range from 1 to 10(2) kHz. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Admittance and dielectric spectroscopy of polycrystalline semiconductors

This text discusses about advantageous, powerful and limitations of admittance and dielectric spectroscopy in the characterization of polycrystalline semiconductors. In the context of polycrystalline semiconductors or dielectric materials, the admittance or dielectric frequency response analyses are shown to be sometimes more useful than impedance spectra analysis, mainly because information on the capacitances or deep trap states are possible to be monitored from admittance or dielectric spectra as a function of dopant concentration or annealing effects. The majority of examples of the application of admittance or dielectric analysis approach were here based on SnO2- and ZnO-based polycrystalline semiconductors devices presenting nonohmic properties. Examples of how to perform the characterization of Schottky barrier in such devices are clearly depicted. The approach is based on findings of the true Mott-Schottky pattern of the barrier by extracting the grain boundary capacitance value from complex capacitance diagram analysis. The equivalent circuit of such kind of devices is mainly consistent with the existence of three parallel elements: the high-frequency limit related to grain boundary capacitances, the complex incremental capacitance at intermediate frequency related to the deep trap relaxation and finally at low frequency region the manifestation of the conductance term representing the dc conductance of the multi-junction device. (c) 2007 Elsevier Ltd. All rights reserved.

Structural study of tungstate fluorophosphate glasses by Raman and X-ray absorption spectroscopy

Transparent glasses were synthesized in the NaPO3-BaF2 WO3 tertiary system and several structural characterizations were performed by X-ray absorption spectroscopy (XANES) at the tungsten L-I and L-III absorption edges and by Raman spectroscopy. Special attention was paid to the coordination state of tungsten atoms in the vitreous network.XANES investigations showed that tungsten atoms are only six-fold coordinated (octahedra WO6) and that these glasses are free of tungstate tetrahedra (WO4).In addition, Raman spectroscopy allowed to identify a break in the linear phosphate chains as the amount of WO3 increases and the formation of P-O-W bonds in the vitreous network indicating the modifier behavior of WO6 octahedra in the glass network. Based on XANES data, we suggested a new attribution of several Raman absorption bands which allowed to identify the presence of W-O- and W=O terminal bonds and a progressive apparition of W-O-W bridging bonds for the most WO3 concentrated samples (≥ 30% molar) due to the formation of WO6 clusters. © 2004 Elsevier B.V. All rights reserved.

Reflux synthesis and hydrothermal processing of ZrO2 nanopowders at low temperature

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Using the electrochemical impedance spectroscopy to characterize carbon steel in biodiesel medium

Electrochemical impedance spectroscopy measurements using two carbon steel electrodes in soybean biodiesel medium, produced by methylic route, were performed in an electrochemical cell that allows positioning the two electrodes face-to-face. To retain the biodiesel between the electrodes and prevent its leakage a porous membrane soaked in biodiesel was used. The amplitude of the AC potential and the area of the electrodes were varied. The linearity between disturbance and response signals was observed for tests when the amplitude of the AC potential was lower than 1500 mV (rms). The electrical resistance of biodiesel dominates the global response and carbon steel presents low corrosion, which is observed only at low frequency, and was confirmed by chemical tests performed in the membrane. In conclusion the electrical resistance of biodiesel can be estimated using electrochemical impedance spectroscopy with two electrodes set up. ©The Electrochemical Society.

Low-temperature synthesis of nanosized bismuth ferrite by the soft chemical method

This paper describes research on a simple low-temperature synthesis route to prepare bismuth ferrite nanopowders by the polymeric precursor method using bismuth and iron nitrates. BiFeO 3 (BFO) nanopowders were characterized by means of X-ray diffraction analyses, (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy (Raman), thermogravimnetric analyses (TG-DTA), ultra-violet/vis (UV/Vis) and field emission scanning electron microscopy (FE-SEM). XRD patterns confirmed that a pure perovskite BiFeO 3 structure with a rhombohedral distorted perovskite structure was obtained by heating at 850 °C for 4 hours. Typical FT-IR spectra for BFO powders revealed the formation of a perovskite structure at high temperatures due to a metal-oxygen bond while Raman modes indicated oxygen octahedral tilts induced by structural distortion. A homogeneous size distribution of BFO powders obtained at 850 °C for 4 hours was verified by FE-SEM analyses. © 2012 Elsevier Ltd and Techna Group S.r.l.

Pitahaya aging diagnostic by impedance/capacitance spectroscopy

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

Raman and XRD study on brookite-anatase coexistence in cathodic electrosynthesized titania

Among the many methods developed for the synthesis of titanium dioxide, cathodic electrosynthesis has not received much attention because the resulting amorphous oxy-hydroxide matrix demands a further thermal annealing step to be transformed into crystalline titania. However, the possibility of filling deep recessed templates by the control of the solidliquid interface makes it a potentially suitable technique for the fabrication of porous scaffolds for photovoltaics and photocatalysis. Furthermore, a careful control of the crystallization process enables the growth of larger grains with lower density of grain boundaries, which act as electron traps that slow down electronic transport and promote charge recombination. In this report, well crystallized titania deposits were obtained by thermal annealing of amorphous deposits fabricated by cathodically assisted electrosynthesis on indium-tin oxide (ITO)substrates. The combined use of Raman spectroscopy and X-ray diffraction showed that the crystallization process is more intricate than previously assumed. It is shown that the amorphous matrix evolves into a rutile-free mixture of brookite and anatase at temperatures as low as 200 degrees C that persists up to 800 degrees C, when pure anatase dominates. The amount of brookite in the brookiteanatase mixture reaches a maximum at 400 degrees C. This very simple method for obtaining a brookiteanatase mixture and the ability to tune their proportions by thermal annealing is a promising alternative whose potential for solar cells and photocatalysis deserves a careful evaluation. Copyright (C) 2011 John Wiley & Sons, Ltd.

USE OF THE LINEAR LIGHT SENSOR ILX554 IN OPTICAL SPECTROSCOPY

USE OF THE LINEAR LIGHT SENSOR ILX554 IN OPTICAL SPECTROSCOPY. This technical note describes the construction of a low-cost optical detector. This device is composed by a high-sensitive linear light sensor (model ILX554) and a microcontroller. The performance or the detector was demonstrated by the detection of emission and Raman spectra of the several atomic systems and the results reproduce those found in the literature.

Trasmission and Reflection (ATR)Far-Infrared Spectroscopy Applied in the Analysis of Cultural Heritage Materials

FIR spectroscopy is an alternative way of collecting spectra of many inorganic pigments and corrosion products found on art objects, which is not normally observed in the MIR region. Most FIR spectra are traditionally collected in transmission mode but as a real novelty it is now also possible to record FIR spectra in ATR (Attenuated Total Reflectance) mode. In FIR transmission we employ polyethylene (PE) for preparation of pellets by embedding the sample in PE. Unfortunately, the preparation requires heating of the PE in order to produces at transparent pellet. This will affect compounds with low melting points, especially those with structurally incorporated water. Another option in FIR transmission is the use of thin films. We test the use of polyethylene thin film (PETF), both commercial and laboratory-made PETF. ATR collection of samples is possible in both the MIR and FIR region on solid, powdery or liquid samples. Changing from the MIR to the FIR region is easy as it simply requires the change of detector and beamsplitter (which can be performed within a few minutes). No preparation of the sample is necessary, which is a huge advantage over the PE transmission method. The most obvious difference, when comparing transmission with ATR, is the distortion of band shape (which appears asymmetrical in the lower wavenumber region) and intensity differences. However, the biggest difference can be the shift of strong absorbing bands moving to lower wavenumbers in ATR mode. The sometimes huge band shift necessitates the collection of standard library spectra in both FIR transmission and ATR modes, provided these two methods of collecting are to be employed for analyses of unknown samples. Standard samples of 150 pigment and corrosion compounds are thus collected in both FIR transmission and ATR mode in order to build up a digital library of spectra for comparison with unknown samples. XRD, XRF and Raman spectroscopy assists us in confirming the purity or impurity of our standard samples. 24 didactic test tables, with known pigment and binder painted on the surface of a limestone tablet, are used for testing the established library and different ways of collecting in ATR and transmission mode. In ATR, micro samples are scratched from the surface and examined in both the MIR and FIR region. Additionally, direct surface contact of the didactic tablets with the ATR crystal are tested together with water enhanced surface contact. In FIR transmission we compare the powder from our test tablet on the laboratory PETF and embedded in PE. We also compare the PE pellets collected using a 4x beam condenser, focusing the IR beam area from 8 mm to 2 mm. A few samples collected from a mural painting in a Nepalese temple, corrosion products collected from archaeological Chinese bronze objects and samples from a mural paintings in an Italian abbey, are examined by ATR or transmission spectroscopy.