Carmo Lança

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.

The use of orthopaedic and dental implants is expanding as a consequence of an ageing population and also due to illness or trauma in younger age groups. The implant must be biocompatible, bioactive and interact favourably with the recipient's bone, as rapid osseointegration is key to success. In this work, Ti-6Al-4V plates were coated using the CoBlastTM technique, with hydroxyapatite (HAp) and HAp/BaTiO3 (barium titanate, BT) non-piezoelectric cubic nanopowders (HAp/cBT) and piezoelectric tetragonal micropowders (HAp/tBT). The addition of BT, a piezoelectric ceramic, is a strategy to accelerate osseointegration by using surface electric charges as cues for cells. For comparison with commercial coatings, plates were coated with HAp using the plasma spray technique. Using XRD and FTIR, both plasma spray and CoBlastTM coatings showed crystalline HAp and no presence of by-products. However, the XRD of the plasma-sprayed coatings revealed the presence of amorphous HAp. The average surface roughness was close to the coatings' thickness (≈5 $μ$m for CoBlastTM and ≈13 $μ$m for plasma spray). Cytotoxicity assays proved that the coatings are biocompatible. Therefore, it can be concluded that for HAp-based coatings, CoBlastTM is a viable alternative to plasma spray, with the advantage of facilitating room temperature addition of other ceramics, like piezoelectric BaTiO3.

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.

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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.

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The physical properties of the cubic and ferrimagnetic spinel ferrite LiFe5O8 has made it an attractive material for electronic and medical applications. In this work, LiFe5O8 nanosized crystallites were synthesized by a novel and eco-friendly sol-gel process, by using powder coconut water as a mediated reaction medium. The dried powders were heat-treated (HT) at temperatures between 400 and 1000 °C, and their structure, morphology, electrical and magnetic characteristics, cytotoxicity, and magnetic hyperthermia assays were performed. The heat treatment of the LiFe5O8 powder tunes the crystallite sizes between 50 nm and 200 nm. When increasing the temperature of the HT, secondary phases start to form. The dielectric analysis revealed, at 300 K and 10 kHz, an increase of $ε$′ (≈10 up to ≈14) with a tan$δ$ almost constant (≈0.3) with the increase of the HT temperature. The cytotoxicity results reveal, for concentrations below 2.5 mg/mL, that all samples have a non-cytotoxicity property. The sample heat-treated at 1000 °C, which revealed hysteresis and magnetic saturation of 73 emu g−1 at 300 K, showed a heating profile adequate for magnetic hyperthermia applications, showing the potential for biomedical applications.

Lately the electrical and dielectric properties of cork and some cork-based materials (commercial and non-commercial) have been studied in order to understand their ability to store electrical charge. The main problem found so far is related to the water content in cork, only of a few % weight. but large enough to influence greatly the conductivity of cork and, consequently, the charge storage capability. To overcome this problem cork has been combined with hydrophobic materials. In this work a commercial wax (paraffin wax) was used to produce a cork/paraffin composite by hot pressing. After milled and mixed natural cork. TetraPak (R) containers waste and paraffin were pressed to make plaques of a new composite. Different concentrations of cork. TetraPak (R) and paraffin, different granules sire, different temperature and pressure were used to produce the samples. The electrical properties of the new composite were measured by the isothermal charging and discharging current method and the results compared to previously ones obtained for natural cork and other derivative products. The new composite has shown to have lower conductivity than the commercial agglomerate. which makes it a better material for charge storage.

Lately the electrical and dielectric properties of cork and some cork-based materials (commercial and non-commercial) have been studied in order to understand their ability to store electrical charge. The main problem found so far is related to the water content in cork, only of a few % weight. but large enough to influence greatly the conductivity of cork and, consequently, the charge storage capability. To overcome this problem cork has been combined with hydrophobic materials. In this work a commercial wax (paraffin wax) was used to produce a cork/paraffin composite by hot pressing. After milled and mixed natural cork. TetraPak (R) containers waste and paraffin were pressed to make plaques of a new composite. Different concentrations of cork. TetraPak (R) and paraffin, different granules sire, different temperature and pressure were used to produce the samples. The electrical properties of the new composite were measured by the isothermal charging and discharging current method and the results compared to previously ones obtained for natural cork and other derivative products. The new composite has shown to have lower conductivity than the commercial agglomerate. which makes it a better material for charge storage.

Lately the electrical and dielectric properties of cork and some cork-based materials (commercial and non-commercial) have been studied in order to understand their ability to store electrical charge. The main problem found so far is related to the water content in cork, only of a few % weight. but large enough to influence greatly the conductivity of cork and, consequently, the charge storage capability. To overcome this problem cork has been combined with hydrophobic materials. In this work a commercial wax (paraffin wax) was used to produce a cork/paraffin composite by hot pressing. After milled and mixed natural cork. TetraPak (R) containers waste and paraffin were pressed to make plaques of a new composite. Different concentrations of cork. TetraPak (R) and paraffin, different granules sire, different temperature and pressure were used to produce the samples. The electrical properties of the new composite were measured by the isothermal charging and discharging current method and the results compared to previously ones obtained for natural cork and other derivative products. The new composite has shown to have lower conductivity than the commercial agglomerate. which makes it a better material for charge storage.

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.

Cross-linked polyethylene (XLPE) is currently widely used as an insulating material for power cables due to its good physical properties, however when in use it undergoes an electrical ageing process. Its ability to trap electric charge can give rise to space charge accumulation in the bulk of the polymer and produce localised electric stresses that can lead to cable failure, since the electric field will be increased above the design stress in some regions favouring the initiation of degradation there. In this work the PEA (pulsed electro-acoustic) method was used to compare the charge dynamics in three samples (XLPE cable peelings) aged in different ways (electrothermally in the laboratory, field aged in service and thermally aged in the laboratory). Very different transient behavior was found depending upon the ageing history. This is related to differences in the migration of chemical species in the insulation layer, which are known to act as charge traps. All materials showed heterocharge peaks when the space charge reached stability, the magnitude of which seems to be related to the severity of the ageing.

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.