Carmo Lança

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.

Traditional bioactive glass powders are typically composed of irregular particles that can be packed into dense configurations presenting low interconnectivity, which can limit bone ingrowth. The use of novel biocomposite sphere formulations comprising bioactive factors as bone fillers are most advantageous, as it simultaneously allows for packing the particles in a 3-dimensional manner to achieve an adequate interconnected porosity, enhanced biological performance, and ultimately a superior new bone formation. In this work, we develop and characterize novel biocomposite macrospheres of Sr-bioactive glass using sodium alginate, polylactic acid (PLA), and chitosan (CH) as encapsulating materials for finding applications as bone fillers. The biocomposite macrospheres that were obtained using PLA have a larger size distribution and higher porosity and an interconnectivity of 99.7%. Loose apatite particles were observed on the surface of macrospheres prepared with alginate and CH by means of soaking into a simulated body fluid (SBF) for 7 days. A dense apatite layer was formed on the biocomposite macrospheres' surface produced with PLA, which served to protect PLA from degradation. In vitro investigations demonstrated that biocomposite macrospheres had minimal cytotoxic effects on a human osteosarcoma cell line (SaOS-2 cells). However, the accelerated degradation of PLA due to the degradation of bioactive glass may account for the observed decrease in SaOS-2 cells viability. Among the biocomposite macrospheres, those composed of PLA exhibited the most promising characteristics for their potential use as fillers in bone tissue repair applications.

Opposite results concerning the sign of the parasitic charge accumulated at the metal dielectric contact in RF microelectromechanical systems (MEMS) capacitive switches are found in the literature. The mechanism concerning charge injection/extraction at the metal-dielectric contact and its influence on the pull-in voltage needs to be further clarified. A model-switch, for which only one dimension is in the microns range, is used to study the behaviour of a capacitive RF MEMS switch. The aim is to analyze how the electric charge is injected/extracted into or from the dielectric material under the applied field and to obtain realistic data to understand how this parasitic charge influences the pull-in voltage V-pi and the pull-off voltage V-po. A triangle voltage is employed to measure V-pi and V-po by measuring the isothermal charging/discharging currents. Our results demonstrate that V-pi is strongly dependent on the injected/extracted charge on the free surface of the dielectric. The charge injected/extracted at the bottom side of the dielectric has no influence on the actuation voltage. The charge injected/extracted on the free surface of the dielectric determines an increase of the modulus of V-pi and, eventually, the switch can fail to actuate. An estimation of the charge stored into the material was obtained (i) by measuring the charging current and the discharging current and (ii) from the value of the V-pi. The parasitic charge necessary to keep the bridge stick to the insulator is 5.3 x 10(-4) cm(-2) for our experimental conditions. The modification of the V-pi determined by the stored charge in the dielectric is analyzed. An increase of the relative dielectric permittivity by a factor of 2 produces a decrease of the actuation voltage of 10%. A variation of 30% in the elastic constant determines a variation of about 20% in the V-pi. A voltage threshold for charge injection/extraction was not observed.

A new experimental procedure combining usual isothermal DC charging and discharging with non-isothermal current measurements has been recently proposed. It is mainly suitable for very high insulating polymers and it was successfully applied to the study of space charge trapping and transport in low-density polyethylene. The analysis of the isothermal currents revealed the presence of different traps whose characteristic (de)trapping times can be deduced. The isothermal procedures allowed the selective charging of the sample. By choosing the charging field and the ratio of charge/discharge times, non-isothermal analysis permitted the differentiation of three or four peaks (at approximate to50degreesC, approximate to65degreesC, approximate to70degreesC and approximate to85degreesC) associated with charge detrapping from surface or near-surface (<20 mum) traps. These traps have activation energies between 0.21 and 1.54 eV. The mobility at 30degreesC is around 5 x 10(-16) m(2) V-1 s(-1). Samples had to be conditioned before each experiment in order to obtain reproducible results.

A new experimental procedure combining usual isothermal DC charging and discharging with non-isothermal current measurements has been recently proposed. It is mainly suitable for very high insulating polymers and it was successfully applied to the study of space charge trapping and transport in low-density polyethylene. The analysis of the isothermal currents revealed the presence of different traps whose characteristic (de)trapping times can be deduced. The isothermal procedures allowed the selective charging of the sample. By choosing the charging field and the ratio of charge/discharge times, non-isothermal analysis permitted the differentiation of three or four peaks (at approximate to50degreesC, approximate to65degreesC, approximate to70degreesC and approximate to85degreesC) associated with charge detrapping from surface or near-surface (<20 mum) traps. These traps have activation energies between 0.21 and 1.54 eV. The mobility at 30degreesC is around 5 x 10(-16) m(2) V-1 s(-1). Samples had to be conditioned before each experiment in order to obtain reproducible results.

Low-density polyethylene (LDPE) films were thermally aged in a sodium chloride aqueous solution at constant temperature (thermal aging). Some of the samples were simultaneously immersed in solution and subjected to an electric AC field (electrical aging). The dielectric relaxation spectra at 30 degreesC in the range of 10(-5) Hz to 10(5) Hz were obtained for unaged and aged samples. For the low frequency (LF) region (10(-5) Hz to 10(-1) Hz) the time domain technique was used. A lock-in amplifier was used for the 10(-1) Hz to 10(1) Hz medium frequency (MF) region. While for the high frequency (HF), 10(-1) Hz to 10(5) Hz, RLC bridge measurements were performed. The main differences can be seen between electrically, thermally aged and unaged LDPE in the HF and LF regions. The LF peak is a broad peak related to localized space charge injection driven by the electric field. For electrically aged samples this peak increases in an earlier stage of electrical aging, decreasing afterwards. While in thermally aged samples the peak amplitude always increases with aging time. Finally the HF shows the beginning of a peak due to the gamma and beta transitions. This peak decreases with aging disappearing for the most aged samples.

Low-density polyethylene (LDPE) films were thermally aged in a sodium chloride aqueous solution at constant temperature (thermal aging). Some of the samples were simultaneously immersed in solution and subjected to an electric AC field (electrical aging). The dielectric relaxation spectra at 30 degreesC in the range of 10(-5) Hz to 10(5) Hz were obtained for unaged and aged samples. For the low frequency (LF) region (10(-5) Hz to 10(-1) Hz) the time domain technique was used. A lock-in amplifier was used for the 10(-1) Hz to 10(1) Hz medium frequency (MF) region. While for the high frequency (HF), 10(-1) Hz to 10(5) Hz, RLC bridge measurements were performed. The main differences can be seen between electrically, thermally aged and unaged LDPE in the HF and LF regions. The LF peak is a broad peak related to localized space charge injection driven by the electric field. For electrically aged samples this peak increases in an earlier stage of electrical aging, decreasing afterwards. While in thermally aged samples the peak amplitude always increases with aging time. Finally the HF shows the beginning of a peak due to the gamma and beta transitions. This peak decreases with aging disappearing for the most aged samples.

Polyethylene is one of the most widely used polymeric insulators in medium and high voltage power cables. However the importance of space charge distribution and its influence on the electrical aging in this polymer is not fully understood. The very good insulating properties of the material implying very long relaxation times (few days and even longer are usual) and low currents (few pA or below) make individual measurements of isothermal charge/discharge currents and thermostimulated currents difficult to analyze and reproduce. A single type of measurements does not take into account the space charge that remains trapped for long times. A combined procedure of isothermal and non-isothermal current measurements developed for high insulating polymers was used for low density polyethylene (LDPE) and crosslinked polyethylene (XLPE) films electrically aged. The press-molded LDPE and XLPE films were electrically aged under similar conditions using an AC electric field while immersed in a sodium chloride aqueous solution at constant temperature (electro-thermal aging). The use of the combined procedure for current measurement allowed obtaining information about space charge traps, activation energies and relaxation times for both LDPE and XLPE. This data was used to compare electrical aging under similar conditions for the two types of polyethylene.

Polyethylene is one of the most widely used polymeric insulators in medium and high voltage power cables. However the importance of space charge distribution and its influence on the electrical aging in this polymer is not fully understood. The very good insulating properties of the material implying very long relaxation times (few days and even longer are usual) and low currents (few pA or below) make individual measurements of isothermal charge/discharge currents and thermostimulated currents difficult to analyze and reproduce. A single type of measurements does not take into account the space charge that remains trapped for long times. A combined procedure of isothermal and non-isothermal current measurements developed for high insulating polymers was used for low density polyethylene (LDPE) and crosslinked polyethylene (XLPE) films electrically aged. The press-molded LDPE and XLPE films were electrically aged under similar conditions using an AC electric field while immersed in a sodium chloride aqueous solution at constant temperature (electro-thermal aging). The use of the combined procedure for current measurement allowed obtaining information about space charge traps, activation energies and relaxation times for both LDPE and XLPE. This data was used to compare electrical aging under similar conditions for the two types of polyethylene.

An understanding of space charge build-up in the polymeric insulation of power cables is important in determining how aging occurs and progresses and, also in predicting cable lifetime. In this investigation electric-field induced space charge in peelings from XLPE (cross-linked polyethylene) cables was measured using two different methods: the pulsed electro-acoustic technique (PEA) and the combined procedure of isothermal and non-isothermal charging/discharging currents (FTSDC). These two methods allow the study of space charge in highly insulating materials. Also, since electric fields of different orders of magnitude are applied to the sample in the two methods, it is possible to analyze different characteristics of the space charge traps. Prior to the measurements the samples were subjected to conditioning to remove volatiles. Cable peelings from various brands aged under different conditions (including field aged and thermally aged samples) were studied as received from the manufacturers. Some of the samples have undergone further ageing in AC electric field (50Hz) for 1000h to see the influence of further ageing on space charge build-up. The results for the different types of samples are compared in an attempt to correlate different ageing parameters.

There is a sustained interest both from theoretical and from practical points of view to understand the isothermal charging and the isothermal discharging currents in dielectrics. The measured 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. As long as we do not know the nature of the origin of the current, it is not clear what information we can get by analyzing the experimental data. 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 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. An analytical expression for the current is proposed. By fitting the experimental data to this analytical equation, 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 of the potential barrier W-0 at the metal-dielectric interface at the initial time when the step voltage is applied. The value obtained for Al-polyethylene terephthalate interface is (0.43 +/- 0.02) eV. For a charging voltage of 220 V there are 6x10(14) trapped electrons/m(2). (c) 2008 American Institute of Physics.

The dielectric breakdown of thin films of low-density polyethylene (LDPE) electrically aged in an aqueous solution of NaCl under an AC electric field was investigated. A two-parameter Weibull function was used for the dielectric breakdown time to failure. The probability of failure for a sample was obtained by the White method for progressively censored data. Samples aged at different temperatures were compared. The results show that initially the samples aged at lower temperature (approximate to25degreesC) are more prone to fail, while those aged at higher temperature (50degreesC) fail at longer times. This was attributed to a competition between oxidation and diffusion.