Carmo Lança

The isothermal charging current and the isothermal discharging current in low mobility materials are analyzed either in terms of polarization mechanisms or in terms of charge injection/extraction at the metal-dielectric interface and the conduction current through the dielectric material. We propose to measure the open-circuit isothermal charging and discharging currents just to overpass the difficulties related to the analysis of the conduction mechanisms in dielectric materials. We demonstrate that besides a polarization current there is a current related to charge injection or extraction at the metal-dielectric interface and a reverse current related to the charge trapped into the shallow superficial or near superficial states of the dielectric and which can move at the interface in the opposite way that occurring during injection. Two important parameters can be determined (i) the highest value of the relaxation time for the polarization mechanisms which are involved into the transient current and (ii) the height of the potential barrier W-0 at the metal-dielectric interface. The experimental data demonstrate that there is no threshold field for electron injection/extraction at a metal-dielectric interface.

The thermally stimulated discharge current (TSDC.) method is a very sensitive and a very selective technique to analyze dipole disorientation and the movement of de-trapped space charge (SC). We have proposed a variant of the TSDC method, namely the final thermally stimulated discharge current (FTSDC) technique. flee experimental conditions can be selected so that the FTSDC is mainly determined by the SC de-trapping. The temperatures of the maximum intensity of the fractional polarization peaks obtained at low temperature, in the range of the local (secondary) relaxation, are in general about 10 to 20 K above the poling temperature. Measurements of the FTSDC in a wide temperature range demonstrate the existence of an apparent peak at a temperature T-ma shifted with about 10 to 30 K above the charging temperature T-c. The shift of T-ma with respect to T-c depends on the experimental conditions. The peak width at the half maximum intensity decreases as T-c increases and the thermal apparent activation energy increases. The variations are not monotonous revealing the temperature range where the molecular motion is stronger and consequently the charge trapping and de-trapping processes are affected. Our results demonstrate that there is a strong similarity between the elementary peaks obtained by the two methods, and the current is mainly determined by SC de-trapping. Even the best elementary peaks are not fitted very well by the analytical equation, indicating that the hypothesis behind this equation have to be reconsidered.

The thermally stimulated discharge current (TSDC.) method is a very sensitive and a very selective technique to analyze dipole disorientation and the movement of de-trapped space charge (SC). We have proposed a variant of the TSDC method, namely the final thermally stimulated discharge current (FTSDC) technique. flee experimental conditions can be selected so that the FTSDC is mainly determined by the SC de-trapping. The temperatures of the maximum intensity of the fractional polarization peaks obtained at low temperature, in the range of the local (secondary) relaxation, are in general about 10 to 20 K above the poling temperature. Measurements of the FTSDC in a wide temperature range demonstrate the existence of an apparent peak at a temperature T-ma shifted with about 10 to 30 K above the charging temperature T-c. The shift of T-ma with respect to T-c depends on the experimental conditions. The peak width at the half maximum intensity decreases as T-c increases and the thermal apparent activation energy increases. The variations are not monotonous revealing the temperature range where the molecular motion is stronger and consequently the charge trapping and de-trapping processes are affected. Our results demonstrate that there is a strong similarity between the elementary peaks obtained by the two methods, and the current is mainly determined by SC de-trapping. Even the best elementary peaks are not fitted very well by the analytical equation, indicating that the hypothesis behind this equation have to be reconsidered.

The Thermally Stimulated Discharge Current (TSDC) method is a very sensitive technique to analyze the movement of dipoles and of space charge (SC). To increase the selectivity of the method we have proposed a variant of the TSDC method, namely the final thermally stimulated discharge current (FTSDC) technique. The experimental conditions can be selected so that the FTSDC is mainly determined by SC de-trapping. The aim of this paper is to analyze if the elementary peaks obtained by using the two methods can be assumed as elementary Debye peaks and to determine the best experimental conditions to obtain a narrow experimental peak which means to increase the selectivity of the method.

Cross-linked polyethylene (XLPE) peelings from aged power cables from three different sources were studied using a combined procedure of isothermal and thermo-stimulated current measurements. Different parameters, such as electric field, temperature, charging/discharging times, can be selected in order to make an analysis of the space charge characteristics (such as, relaxation times and activation energies). Three different cables peelings were analyzed: A - electrically aged in the laboratory at high temperature, B - service aged for 18 years and C - thermally aged in the laboratory at high temperature. The results were compared for the different types of samples and also with previous results on laboratory aged and produced films of low-density polyethylene (LDPE) and XLPE.

Space charge in electrically aged cross-linked polyethylene (XLPE) was studied using a procedure combining isothermal and non-isothermal measurements of charge and discharge currents. Aging is carried out using an AC field while immersing the disk-shaped samples in an ionic aqueous solution at constant temperature. After aging the samples were isothermally DC charged and discharged. Next a non-isothermal experiment with constant heating rate was performed (FTSDC). Finally the sample was kept at the highest temperature in order to completely discharge the polymer. The space charge introduced in the XLPE during aging can be analyzed from the study of the FTSDC spectra. The thermogram (FTSDC) shows a very broad peak. The peak is attributed to trapped space charge in traps with long relaxation times. It is possible to decompose it into three or four individual peaks and obtain the corresponding activation energies. The results were compared with previous ones obtained for LDPE (low density polyethylene) aged under similar conditions.

Electrical properties of natural cork, commercial cork agglomerates (for floor and wall coverings) and a recently developed composite of cork/TetraPak (R) were studied. Measurements of isothermal charge and discharge currents were made for natural cork samples in different directions (axial, radial and tangential cuts). The isothermal current characteristics and the samples conductivity were investigated under different conditions (electric field, temperature and environmental conditions: in air at ambient relative humidity (RH), dry air and vacuum), also the samples could be or not conditioned (dried in vacuum or in a P2O5 atmosphere at room temperature). From these results the influence of water on the electrical properties of natural cork could be seen. In order to compare the three different cork materials a preliminary study was made. Isothermal charge and discharge currents and conductivity after 1h charging were measured and compared for different electric fields and temperature in air at ambient RH.

The electrical methods used to study the molecular movements are based on the movement of the dipoles under DC or AC electric field. We have proposed recently a combined measuring protocol to analyze charge injection/extraction, transport, trapping and de-trapping in polar or non-polar dielectric materials. The method is used here to analyze the molecular movements in polyimide in the temperature range from 293 to 572 K. A strong relaxation was observed around 402 K and a very weak relaxation around 345 K. This is the beta relaxation which is quite complex. As concern the behavior at high temperatures, above the beta relaxation, a high peak was observed that shifts continuously to higher temperatures as the charging temperature and/or the charging field increase. The maximum current of the peak increases and the temperature corresponding to the maximum current increases as the charging temperature and/or the charging field increase, given a direct observation of the so called cross-over effect related to current decay for sample charged at high fields and/or high temperatures.

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Solid state reaction was used to produced barium titanate modified with calcium (BCT) showing the presence of the piezoelectric tetragonal phase after sintering at 1350 °C. Bioglass 45S5 (BG) was synthetized by sol-gel route. From these two materials and commercial hydroxyapatite (HAp) were obtained composites. The BG produced showed some cytotoxic character that was weakened by passivation. All other materials were non-cytotoxic. Contact polarization at constant temperature was chosen composites polarization. Electric/dielectric properties were evaluated by thermally stimulated depolarization currents (TSDC). The material showed bioactivity with the composite with BCT/BG/HAp 90/5/5 (wt%) showing increased bioactivity. In vitro test showed high proliferation rates for the composites.

The measured isothermal charging and discharging currents are analyzed either in terms of polarization mechanisms or in terms of charge injection/extraction at the metal-dielectric interface and the conduction current through the dielectric material. We propose to measure the open-circuit isothermal charging and discharging currents just to overpass the difficulties related to the analysis of the conduction mechanisms through the dielectric materials. Besides a polarization current, there is a current related with charge injection or extraction at the metal-dielectric contact and a reverse current related to the charge trapped into the superficial trap states of the dielectric and that can jump at the interface in a reverse way. By fitting the experimental data, two important parameters can be determined (i) the highest value of the relaxation time for the polarization mechanisms still involved into the transient current and (ii) the height W-0 of the potential barrier at the metal-dielectric interface immediately after the step voltage is applied. Only the initial part of the measured isothermal charging or discharging current can be used to obtain information about the polarization processes. By transforming the time-domain data into the frequency domain, a maximum for the imaginary part of the dielectric permittivity is obtained, in good agreement with the data obtained from AC dielectric measurements and the finally thermally stimulated discharge current measurements. (C) 2009 Elsevier B.V. All rights reserved.

Open-cell foams based on hydroxyapatite (HAp) can mimic the extracellular matrix (ECM) to better replace damaged hard tissues and assist in their regeneration processes. Aerogels of HAp nanowires (NW) with barium titanate (BT) particles were produced and characterized regarding their physical and chemical properties, bioactivity, and in vitro cytotoxicity. Considering the role of piezoelectricity (mainly due to collagen) and surface charges in bone remodeling, all BT particles, of size 280 nm and 2 and 3 µm, contained BaTiO3 in their piezoelectric tetragonal phase. The synthesized nanowires were verified to be AB-type carbonated hydroxyapatite. The aerogels showed high porosity and relatively homogeneous distribution of the BT particles. Barium titanate proved to be non-cytotoxic while all the aerogels produced were cytotoxic for an extract concentration of 1 mg/mL but became non-cytotoxic at concentrations of 0.5 mg/mL and below. It is possible that these results were affected by the higher surface area and quicker dissolution rate of the aerogels. In the bioactivity assays, SEM/EDS, it was not easy to differentiate between the apatite deposition and the surface of the HAp wires. However, a quantitative EDS analysis shows a possible CaP deposition/dissolution cycle taking place.