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Dardouri, Maïssa, João Paulo Borges, and Amel Omrani. "Tailoring the morphology of hydroxyapatite particles using a simple solvothermal route." Ceramics International 43 (2017): 3784-3791. AbstractWebsite

Nanometric and sub-micrometric monodispersed hydroxyapatite (HAp) particles with different morphologies (spheres and rods) were synthesized via a simple solvothermal method using Ca(NO3)2·4H2O and P2O5 as starting materials without any requirement to use organic templates. The growth, evolution and purity of the nanoparticles were investigated by controlling the synthesis conditions, including the alkalinity and the temperature of the solvothermal treatment. The increasing of the alkaline ratio results in a great change of the elaborated particles’ morphology that evolved from anisotropic forms (nanorods, sub-micrometric rod) at pH 9, short rod particles at pH 9.5 to spherical ones at higher pH (pH≥10).
Powder X-Ray diffractometry (XRD), Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR) and Nitrogen adsorption and desorption studies (BET) were used to characterize the structure and composition of the as-prepared samples.
The thermal analysis of the synthesized particles conducted by differential scanning calorimetry (DSC) shows a good stability for all morphologies with a degradation temperature reaching 1300 °C.

Lakhdar, Allagui, João Paulo Borges, Abdesslam Amara, and Amel Omrani. "Template-free synthesis of sub-micrometric cobalt fibers with controlled shape and structure. Characterization and magnetic properties." Journal of Magnetism and Magnetic Materials 425 (2017): 6-11. AbstractWebsite

Sub-micrometric Co fibers were prepared via a modified polyol process at 90 °C under an external magnetic field of about 550 Oe, using ethelyne glycol as solvent and hydrazine as reducing agent. The structure, the size and the morphology of the as-elaborated products were highly controlled through properly monitoring the synthesis parameters (amount of NaOH added, the amount of the reducing agent, precursor’ concentration and precursors mixing protocol). The XRD characterization confirmed the formation of pure cobalt powders with either hexagonal compact (hcp) or face-centered-cubic (fcc) structure depending on the concentration of the metal precursor and sodium hydroxide. The scanning electron microscopy observations of the powders shows sub-micrometric fibers with about 0.4–0.6 µm in diameter and a length that could reach 15 µm. Fibers prepared at high reducing ratio were constituted of flower-like spheres that coalesce in the direction of the applied magnetic field. For their high contact surface, these fibers offer new opportunities for catalysis applications. The hysteresis loop measurements show an enhancement of the Hc of the as-obtained fibers compared to their bulk counterparts and permit to confirm the relationship between the structure and the magnetic properties of the materials.

Borges, João Paulo, Maria Helena Godinho, Assis Farinha Martins, DF Stamatialis, MN de Pinho, and Mohamed Naceur Belgacem. "Tensile properties of cellulose fiber reinforced hydroxypropylcellulose films." Polymer composites 25 (2004): 102-110. AbstractWebsite

The tensile properties of cross-linked and uncross-linked composite films (thickness ∼20–35 μm) prepared from Hydroxypropylcellulose (HPC) with incorporation of microcrystalline cellulose fibers (Avicel) were studied. The concentration of fibers in the composites ranged from 0 to 30 w/w% and cross-linked composites were obtained by the reaction of HPC-Avicel mixtures with 1,4-butyldiisocyanate. It was demonstrated that the inclusion of fibers in a HPC matrix produces composites with enhanced mechanical properties that are improved by cross-linking. Mechanical results seem to indicate that the elastic deformation of the cross-linked composites is predominantly dominated by the fiber content while the cross-linking affects mainly the plastic deformation. Maximum values of the Young's Modulus, yield stress and tensile stress were observed at 10 w/w% for the cross-linked and 20 w/w% for the uncross-linked composites. Furthermore cross-linked films with 10 w/w% of fibers present values of yield stress and tensile stress that are in average 15 to 20% higher than those obtained for uncross-linked composites with 20 w/w% of fibers. Studies in Polarizing Optical Microscopy and Atomic Force Microscopy (AFM) seem to indicate that tensile properties of these composites are correlated to the packing of fibers. For the concentration of the utilized cross-linking agent, and for a fiber content of 10 w/w%, an optimal packing of fibers throughout the matrix has been correlated to the minimal difference between the roughness parameters obtained by AFM analysis of the top and bottom surfaces of the films.

Soares, Paula I. P., Diana Machado, César Laia, Laura Pereira, Joana Coutinho, Isabel Ferreira, Carlos Novo, and João Paulo Borges. "Thermal and magnetic properties of chitosan-iron oxide nanoparticles." Carbohydrate polymers 149 (2016): 382-390. AbstractWebsite

Chitosan is a biopolymer widely used for biomedical applications such as drug delivery systems, wound healing, and tissue engineering. Chitosan can be used as coating for other types of materials such as iron oxide nanoparticles, improving its biocompatibility while extending its range of applications.
In this work iron oxide nanoparticles (Fe3O4 NPs) produced by chemical precipitation and thermal decomposition and coated with chitosan with different molecular weights were studied. Basic characterization on bare and chitosan-Fe3O4 NPs was performed demonstrating that chitosan does not affect the crystallinity, chemical composition, and superparamagnetic properties of the Fe3O4 NPs, and also the incorporation of Fe3O4 NPs into chitosan nanoparticles increases the later hydrodynamic diameter without compromising its physical and chemical properties. The nano-composite was tested for magnetic hyperthermia by applying an alternating current magnetic field to the samples demonstrating that the heating ability of the Fe3O4 NPs was not significantly affected by chitosan.

Soares, Paula I. P., Frederik Lochte, Coro Echeverria, Laura Pereira, Joana Coutinho, Isabel Ferreira, Carlos Novo, and João Paulo Borges. "Thermal and magnetic properties of iron oxide colloids: influence of surfactants." Nanotechnology 26 (2015): 425704. AbstractWebsite

Iron oxide nanoparticles (NPs) have been extensively studied in the last few decades for several biomedical applications such as magnetic resonance imaging, magnetic drug delivery and hyperthermia. Hyperthermia is a technique used for cancer treatment which consists in inducing a temperature of about 41–45 °C in cancerous cells through magnetic NPs and an external magnetic field. Chemical precipitation was used to produce iron oxide NPs 9 nm in size coated with oleic acid and trisodium citrate. The influence of both stabilizers on the heating ability and in vitro cytotoxicity of the produced iron oxide NPs was assessed. Physicochemical characterization of the samples confirmed that the used surfactants do not change the particles' average size and that the presence of the surfactants has a strong effect on both the magnetic properties and the heating ability. The heating ability of Fe3O4 NPs shows a proportional increase with the increase of iron concentration, although when coated with trisodium citrate or oleic acid the heating ability decreases. Cytotoxicity assays demonstrated that both pristine and trisodium citrate Fe3O4 samples do not reduce cell viability. However, oleic acid Fe3O4 strongly reduces cell viability, more drastically in the SaOs-2 cell line. The produced iron oxide NPs are suitable for cancer hyperthermia treatment and the use of a surfactant brings great advantages concerning the dispersion of NPs, also allowing better control of the hyperthermia temperature.

Baptista, Ana Catarina, J. I. Martins, Elvira Fortunato, Rodrigo Martins, João Paulo Borges, and Isabel Ferreira. "Thin and flexible bio-batteries made of electrospun cellulose-based membranes." Biosens Bioelectron 26 (2011): 2742-5. AbstractWebsite

The present work proposes the development of a bio-battery composed by an ultrathin monolithic structure of an electrospun cellulose acetate membrane, over which was deposited metallic thin film electrodes by thermal evaporation on both surfaces. The electrochemical characterization of the bio-batteries was performed under simulated body fluids like sweat and blood plasma [salt solution–0.9% (w/w) NaCl]. Reversible electrochemical reactions were detected through the cellulose acetate structure. Thus, a stable electrochemical behavior was achieved for a bio-battery with silver and aluminum thin films as electrodes. This device exhibits the ability to supply a power density higher than 3 muW cm(-2). Finally, a bio-battery prototype was tested on a sweated skin, demonstrating the potential of applicability of this bio-device as a micropower source.

Soares, Paula I. P., Ana Isabel Sousa, Isabel Ferreira, Carlos Novo, and João Borges Borges. "Towards the development of multifunctional chitosan-based iron oxide nanoparticles: Optimization and modelling of doxorubicin release." Carbohydrate Polymers 153 (2016): 212-221. AbstractWebsite

In the present work composite nanoparticles with a magnetic core and a chitosan-based shell were produced as drug delivery systems for doxorubicin (DOX). The results show that composite nanoparticles with a hydrodynamic diameter within the nanometric range are able to encapsulate more DOX than polymeric nanoparticles alone corresponding also to a higher drug release. Moreover the synthesis method of the iron oxide nanoparticles influences the total amount of DOX released and a high content of iron oxide nanoparticles inhibits DOX release. The modelling of the experimental results revealed a release mechanism dominated by Fickian diffusion.

Faria, Jaime, Coro Echeverria, João Paulo Borges, Maria Helena Godinho, and Paula I. P. Soares. "Towards the development of multifunctional hybrid fibrillary gels: production and optimization by colloidal electrospinning." RSC Advances 7 (2017): 48972-48979. AbstractWebsite

The incorporation of thermosensitive microgels that can act as active sites into polymeric fibers through colloidal electrospinning originates multifunctional, highly porous, and biocompatible membranes suitable for biomedical applications. The use of polyvinylpyrrolidone (PVP), a biocompatible, water-soluble polymer as a fiber template, not only allows the use of a simple set-up to produce composite membranes, but also avoids the use of organic solvents to prepare such systems. Further crosslinking with ultraviolet (UV) radiation avoids membrane dissolution in physiological conditions. Highly porous, UV crosslinked composite membranes with monodisperse mean fiber diameters around 530 nm were successfully produced. These composite membranes showed a Young Modulus of 22 MPa, and an ultimate tensile strength of 3 MPa, accessed in the mechanical tests. Furthermore, the same composite membranes were able to swell about 30 times their weight after 1 hour in aqueous medium. In this work composite multifunctional membranes were designed and extensively studied. PVP, a biocompatible water-soluble polymer, was used as a fiber template to incorporate thermoresponsive poly-(N-isopropylacrylamide) (PNIPAAm)-based microgels into the composite membrane using colloidal electrospinning. The design of multifunctional membranes can be further tailored to several biomedical applications such as temperature-controlled drug delivery systems.

Prezas, Pedro, Bruno Melo, Luís Costa, Manuel Valente, Maria Carmo Lança, José Ventura, Luís Pinto, and Manuel Prezas. "TSDC and impedance spectroscopy measurements on hydroxyapatite, β-tricalcium phosphate and hydroxyapatite/β-tricalcium phosphate biphasic bioceramics." Applied Surface Science 424 (2017): 28-38. AbstractWebsite

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.