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2024
Tavares, C., T. Vieira, J. C. Silva, J. P. M. R. Borges, and C. M. Lança, "Bioactive Hydroxyapatite Aerogels with Piezoelectric Particles", Biomimetics 2024, Vol. 9, Page 143, vol. 9, no. 3: Multidisciplinary Digital Publishing Institute, pp. 143, feb, 2024. AbstractWebsite

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.

2023
Dias, I. J. G., S. A. Pádua, E. A. Pires, J. P. M. R. Borges, J. C. Silva, and C. M. Lança, "Hydroxyapatite-Barium Titanate Biocoatings Using Room Temperature Coblasting", Crystals 2023, Vol. 13, Page 579, vol. 13, no. 4: Multidisciplinary Digital Publishing Institute, pp. 579, mar, 2023. AbstractWebsite

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.

de Oliveira, I. R., I. dos Santos Gonçalves, K. Wallace dos Santos, M. C. Lança, T. Vieira, J. C. Silva, I. F. Cengiz, R. L. Reis, J. M. Oliveira, and J. P. Miranda Ribeiro Borges, "Biocomposite Macrospheres Based on Strontium-Bioactive Glass for Application as Bone Fillers", ACS Materials Au, vol. 3, no. 6: American Chemical Society, pp. 646–658, 2023. AbstractWebsite

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.

Hammami, I., S. R. Gavinho, A. S. Pádua, M. C. do Lança, J. P. Borges, and J. C. Silva, "Extensive Investigation on the Effect of Niobium Insertion on the Physical and Biological Properties of 45S5 Bioactive Glass for Dental Implant", International Journal of Molecular Sciences, vol. 24, issue 6, pp. 5244-5263, 2023.
Dias, I. J. G. J. G., A. S. S. Pádua, E. Pires, J. P. M. R. Borges, J. C. Silva, and M. C. Lança, "TSDC and surface potential measurements of charged hydroxyapatite/BaTiO 3 biocoatings deposited by CoBlast", ISE19-19th Int Symp on Electrets, 18-22 Sept., Linz, Austria, Johannes Kepler Univ., pp. 77, 2023. Abstract

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2022
Madeira, R. M. D., T. Vieira, J. C. Silva, I. R. Oliveira, J. P. Borges, M. M. R. A. Lima, and C. M. Lança, "Piezoelectric Calcium Modified Barium Titanate for Bone Regeneration", Materials Proceedings 2022, Vol. 8, Page 121, vol. 8, no. 1, Basel Switzerland, Multidisciplinary Digital Publishing Institute, pp. 121, jul, 2022. Abstract

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.

Oliveira, I. R., A. M. Barbosa, K. W. Santos, M. C. Lança, M. M. R. A. Lima, T. Vieira, J. C. Silva, and J. P. Borges, "Properties of strontium-containing BG 58S produced by alkali-mediated sol-gel process", Ceramics International: Elsevier, jan, 2022. AbstractWebsite

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2021
Teixeira, S. S., M. P. F. Graça, J. Lucas, M. A. Valente, P. I. P. Soares, M. C. Lança, T. Vieira, J. C. Silva, J. P. Borges, L. - I. Jinga, G. Socol, C. Mello Salgueiro, J. Nunes, and L. C. Costa, "Nanostructured LiFe5O8 by a Biogenic Method for Applications from Electronics to Medicine", Nanomaterials, vol. 11, no. 1: MDPI AG, pp. 193, jan, 2021. AbstractWebsite

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.

2019
Gavinho, S. R., P. R. Prezas, D. J. Ramos, I. Sá‐Nogueira, J. P. Borges, C. M. Lança, J. C. Silva, C. M. R. Henriques, E. Pires, J. S. Kumar, and M. P. F. Graça, "{Nontoxic glasses: Preparation, structural, electrical and biological properties}", International Journal of Applied Ceramic Technology: John Wiley {&} Sons, Ltd (10.1111), pp. ijac.13243, apr, 2019. AbstractWebsite
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2017
Prezas, P. R., B. M. G. Melo, L. C. Costa, M. A. Valente, M. C. Lança, J. M. G. Ventura, L. F. V. Pinto, and M. P. F. Graça, "TSDC and impedance spectroscopy measurements on hydroxyapatite, β-tricalcium phosphate and hydroxyapatite/β-tricalcium phosphate biphasic bioceramics", Applied Surface Science, vol. 424, issue 1, pp. 28-38, 2017. Abstract

Bone grafting and surgical interventions related with orthopaedic disorders consist in a big business, generating large revenues worldwide every year. There is a need to replace the biomaterials that currently still dominate this market, i.e., autografts and allografts, due to their disadvantages, such as limited availability, need for additional surgeries and diseases transmission possibilities. The most promising replacement materials are biomaterials with bioactive properties, such as the calcium phosphate-based bioceramics group. The bioactivity of these materials, i.e., the rate at which they promote the growth and directly bond with the new host biological bone, can be enhanced through their electrical polarization.In the present work, the electrical polarization features of pure hydroxyapatite (Hap), pure β-tricalcium phosphate (β-TCP) and biphasic hydroxyapatite/β-tricalcium phosphate composites (HTCP) were analyzed by measuring thermally stimulated depolarization currents (TSDC). The samples were thermoelectrically polarized at 500. °C under a DC electric field with a magnitude of 5. kV/cm. The biphasic samples were also polarized under electric fields with different magnitudes: 2, 3, 4 and 5. kV/cm. Additionally, the depolarization processes detected in the TSDC measurements were correlated with dielectric relaxation processes observed in impedance spectroscopy (IS) measurements.The results indicate that the β-TCP crystalline phase has a considerable higher ability to store electrical charge compared with the Hap phase. This indicates that it has a suitable composition and structure for ionic conduction and establishment of a large electric charge density, providing great potential for orthopaedic applications.

2015
Neagu, E. R., M. C. Lanca, C. J. Dias, and J. N. Marat-Mendes, "Space Charge and Dipolar Charge Contribution at Polar Polymers Polarization", Ieee Transactions on Dielectrics and Electrical Insulation, vol. 22, no. 3, pp. 1419-1426, 2015. AbstractWebsite
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2013
AS, P., B. JPMR, N. E, M. - M. JN, and L. MCH, Electrical characterization of biphasic ceramics used in hard tissue replacement, , Coimbra Portugal, pp. 217, 2013. Abstract

Hydroxyapatite [Hap; Ca10(PO4)6(OH)2) and b-tricalcium phosphate [b-TCP; Ca3(PO4)2] are biocompatible calcium phosphates used in skeletal surgery. The natural HAp is one of the main components of bone and, as a synthetic material, has been widely used for bone replacement presenting good bioactivity. Nevertheless synthetic HAp presents a slow in vivo degradation rate which is disadvantageous for bone’s reparative process. b-TCP has also good osteogenic characteristics presenting the ability to form strong bonds with the bone however, its degradation rate is too fast [1]. Therefore, a composite combining these two ceramics is valuable as it exhibits a suitable degradation rate. Because of the piezoelectric properties of bone it is known that electrical polarization of calcium phosphates can enhance the bioactivity and biointegration of implants [2]. Previous studies have already showed that HAp/b-TCP ceramics can be electrically polarized and that electrical polarization enhances osteogenesis in the early stage of the implantation process. However further studies are required to understand, optimize and improve the polarization technique [1]. In this work a commercial biphasic ceramic powders were pressed in a mold at 200 MPa to produce disc shaped samples. Afterwards, the samples were sintered at temperatures from 950ºC to 1150ºC and the influence of the heat treatment in the electrical polarization and subsequent bioactivity was investigated. The samples were polarized under a high DC electric field at relatively lower temperature (200oC) compared to previous studies and the stability of polarization was tested using TSDC (thermally depolarization currents) measurements. It was studied the influence of the water, initially present in the material, in the total charge deposited during polarization, its stability and its relation with heat treatment after pressing. The influence of the addition of b-TCP on sample’s stored charge was also evaluated. Finally bioactivity tests in a simulated body fluid solution were made taking into account the signal of the charge in each surface of the disc samples so that the results could be compared to previous ones.

Lanca, M. C., I. Cunha, J. P. Marques, E. R. Neagu, L. Gil, C. J. Dias, and J. N. Marat-Mendes, "Water Content Control To Improve Space Charge Storage in a Cork Derivative", Advanced Materials Forum Vi, Pts 1 and 2, vol. 730-732, pp. 395-400, 2013. Abstract
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2012
Inês, C., M. J. Paulo, G. Luís, N. E. R., D. C. J., M. - M. J. N., and L. M. C., Water Content Control to Improve Space Charge Storage in a Cork Derivative, , pp. 395-400, Jan, 2012. Abstract
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Inês, C., M. J. Paulo, G. Luís, N. E. R., D. C. J., M. - M. J. N., and L. M. C., "Water Content Control to Improve Space Charge Storage in a Cork Derivative", Materiais2011, 2012. Abstract
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M.C., L., C. I., M. J. Paulo, G. I. L. L., N. E. A. G. U. E.R., D. I. A. S. C.J., and M. - M. J. N., Water Content Control to Improve Space Charge Storage in a Cork Derivative, , vol. 730-732, pp. 395-400, 2012. Abstract
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2011
R., N. E., C. Dias, L. M. Carmo, I. R., I. P., and M. - M. J. N., Discrimination between Space Charge and Dipolar Contributions in Ferroelectric Polymers, , pp. 145-146, Jan, 2011. Abstract
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M.C., L. A. N. Ç. A., N. E. A. G. U. E.R., D. I. A. S. C.J., G. I. L. L., and M. A. R. A. T. - M. E. N. D. E. S. J.N., Electrical properties of cork and derivatives, , vol. 23, pp. 64-70, Jan, 2011. Abstract
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A., P., L. A. N. Ç. A. M.C., B. J.P., N. E. A. G. U. E.R., D. I. A. S. C.J., Marat-Mendes, and J.N., Influence of Polarization on the Bioactivity of Nanopowders of Hydroxyapatite, , pp. 55-56, Jan, 2011. Abstract
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ER, N., D. CJ, L. MC, I. R, I. P, and M. - M. J. N., The use of the final thermally stimulated discharge current technique to study the molecular movements around glass transition, , vol. 354, pp. 385-390, Jan, 2011. Abstract
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R., N. E., C. Dias, L. M. Carmo, I. R., I. P., and M. - M. J. N., "Discrimination between Space Charge and Dipolar Contributions in Ferroelectric Polymers", 14th International Symposium on Electrets, 2011. Abstract

The final thermally stimulated discharge current method allows a better selection of the experimental conditions for sample polarization. By decreasing the ratio between the charging time and the discharging time, the apparent peak is of the same order of magnitude as the genuine peaks and there is only a partial overlap between then. Two peaks have been identified for polyamide 11, one associated with the glass transition around 60 °C and the second associated with the Curie transition around 96 °C.

Neagu, E. R., C. J. Dias, M. C. Lanca, R. Igreja, P. Inacio, J. N. Marat-Mendes, and Ieee, Discrimination between Space Charge and Dipolar Contributions in Ferroelectric Polymers, , pp. 145-146, 2011. AbstractWebsite

The final thermally stimulated discharge current method allows a better selection of the experimental conditions for sample polarization. By decreasing the ratio between the charging time and the discharging time, the apparent peak is of the same order of magnitude as the genuine peaks and there is only a partial overlap between then. Two peaks have been identified for polyamide 11, one associated with the glass transition around 60 degrees C and the second associated with the Curie transition around 96 degrees C.

M.C., L. A. N. Ç. A., N. E. A. G. U. E.R., D. I. A. S. C.J., G. I. L. L., and M. A. R. A. T. - M. E. N. D. E. S. J.N., Electrical properties of cork and derivatives, , vol. 23, issue 3/4, 2011. Abstract
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A., P., L. A. N. Ç. A. M.C., B. J.P., N. E. A. G. U. E.R., D. I. A. S. C.J., Marat-Mendes, and J.N., "Influence of Polarization on the Bioactivity of Nanopowders of Hydroxyapatite", 14th International Symposium on Electrets, 2011. Abstract
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Pedrosa, A., M. C. Lanca, J. P. Borges, E. R. Neagu, C. J. Dias, J. N. Marat-Mendes, and Ieee, "Influence of Polarization on the Bioactivity of Nanopowders of Hydroxyapatite", 2011 14th International Symposium on Electrets (Ise), pp. 55-56, 2011. Abstract
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