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Almeida, Pedro L., Sudarshan Kundu, João Paulo Borges, Maria Helena Godinho, and Joao L. Figueirinhas. "Electro-optical light scattering shutter using electrospun cellulose-based nano-and microfibers." Applied Physics Letters 95 (2009): 043501. AbstractWebsite

Electrospun cellulose-based nano and microfibers and a nematic liquid crystal are used to assemble an electro-optical (EO) light-scattering device that shows enhanced characteristics when compared to similar devices. Based on the controlled scattering of light in the composite system, the device can achieve light transmission coefficients tunable from 1% up to around 89%. Simulation of the EO behavior indicates that the roughness of the polymer-liquid crystal interface is crucial for the optical performance of the device.

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.

Baptista, Ana Catarina, Isabel Ferreira, and João Borges. "Cellulose-based bioelectronic devices." In Cellulose - Medical, Pharmaceutical and Electronic Applications, edited by Theo van de Ven and Louis Godbout. InTech, 2013.
Baptista, Ana Catarina, Alexandre Botas, Ana Almeida, Ana Nicolau, Bruno Falcão, Manuel Soares, Joaquim Pratas Leitão, Rodrigo Martins, João Paulo Borges, and Isabel Ferreira. "Down conversion photoluminescence on PVP/Ag-nanoparticles electrospun composite fibers." Optical Materials 39 (2015): 278-281. AbstractWebsite

The influence of Ag nanoparticles (Ag NPs) on the luminescence of electrospun nonwoven mats made of polyvinylpyrrolidone (PVP) has been studied in this work. The PVP fibers incorporating 2.1–4.3 nm size Ag NPs show a significant photoluminescence (PL) band between 580 and 640 nm under 325 nm laser excitation. The down conversion luminescence emission is present even after several hours of laser excitation, which denotes the durability and stability of fibers to consecutive excitations. As so these one-dimensional photonic fibers made using cheap methods is of great importance for organic optoelectronic applications, fluorescent clothing or counterfeiting labels.

Baptista, Ana Catarina, Inês Ropio, Beatriz Romba, Joana Nobre, Célia Henriques, Jorge Carvalho Silva, J. I. Martins, João Paulo Borges, and Isabel Ferreira. "Cellulose-based electrospun fibers functionalized with polypyrrole and polyaniline for fully organic batteries." Journal of Materials Chemistry A 6 (2018): 256-265. AbstractWebsite

A novel cellulose-based bio-battery made of electrospun fibers activated by biological fluids has been developed. This work reports a new concept for a fully organic bio-battery that takes advantage of the high surface to volume ratio achieved by an electrospun matrix composed of sub-micrometric fibers that acts simultaneously as the separator and the support of the electrodes. Polymer composites of polypyrrole (PPy) and polyaniline (PANI) with cellulose acetate (CA) electrospun matrix were produced by in situ chemical oxidation of pyrrole and aniline on the CA fibers. The structure (CA/PPy|CA|CA/PANI) generated a power density of 1.7 mW g−1 in the presence of simulated biological fluids, which is a new and significant contribution to the domain of medical batteries and fully organic devices for biomedical applications.

Baptista, Ana Catarina, Miguel Brito, Ana Marques, and Isabel Ferreira. "Electronic control of drug release from gauze or cellulose acetate fibres for dermal applications." Journal of Materials Chemistry B 9 (2021): 3515-3522. AbstractWebsite

Electronic controlled drug release from fibres was studied using ibuprofen as a model drug, one of the most popular analgesics, to impregnate gauze and cellulose acetate (CA) membranes. Conductivity in the range of 1–10 mS cm−1 was obtained in polypyrrole (Ppy) functionalised gauze and CA fibres, providing voltage-controlled drug release in a system consisting of Ppy/Ibuprofen/Ppy membranes and an Ag electrode. SEM images evidenced the Ppy adhesion to fibres and Micro Raman spectra proved drug incorporation and release. A small wound adhesive built with these membranes retains ibuprofen at 1.5 V and quickly releases it when −0.5 V is applied.

Baptista, Ana Catarina, Isabel Ferreira, and João Paulo Borges. "Cellulose-based composite systems for biomedical applications." In Biomass based Biocomposites, edited by Vijay Kumar Thakur and A. S. Singha, 47-60. U.K.: Smithers Rapra Technology, 2013.
Baptista, Ana Catarina, Paula I. P. Soares, Isabel Ferreira, and João Paulo Borges. "Nanofibers and nanoparticles in biomedical applications." In Bioengineered Nanomaterials, edited by Atul Tiwari and Ashutosh Tiwari. USA: CRC Press (Taylor & Francis Group), 2013.
Baptista, Ana Catarina, Isabel Ferreira, and João Paulo Borges. "Electrospun fibers in composite materials for medical applications." Journal of Composites and Biodegradable Polymers 1 (2013): 56-65. AbstractWebsite

The development of nanoscaled materials has deserved a remarkable interest for biomedical applications. Biological tissues are essentially composite materials with particular mechanical properties that should be carefully considered during the design of innovative biomedical scaffolds. Electrospun membranes are often found in medical applications due to its high specific surface which creates a 3D porous structure that mimics the native extracellular matrix. These electrospun membranes can also be designed to have enhanced mechanical properties, biocompatibility and cellular response making them appealing and inspiring to be used in composites materials.
This paper reviews the new insights in the development of advanced nanostructured composites materials based on electrospun fibers. From tissue engineering to bioelectronics, these composite materials can be found in the most promising research developments for the medical applications.

Borges, João Paulo, João Paulo Canejo, Susete Fernandes, Pedro Brogueira, and Maria Helena Godinho. "Cellulose-Based Liquid Crystalline Composite Systems." In Nanocellulose Polymer Nanocomposites: Fundamentals and Applications, edited by Vijay Kumar Thakur, 215-235. Hoboken, NJ, USA: John Wiley & Sons, Inc., 2014.
Borges, João Paulo, Maria Helena Godinho, Assis Farinha Martins, Ana Catarina Trindade, and Mohamed Naceur Belgacem. "Cellulose-based composite films." Mechanics of composite materials 37 (2001): 257-264. AbstractWebsite

The mechanical and optical properties of cellulose-based composite films are investigated.It is shown that the use of toluene diisocyanate as a coupling agent and Avicel fibers as reinforcing elements give films with the highest mechanical characteristics. Using differential scanning calorimetry, it is also found that the glass transition temperature Tg of all the materials studied is below the room temperature and that the Tg increased with cross-linking and introduction of Avicel.

Borges, João Paulo, Maria Helena Godinho, Mohamed Naceur Belgacem, and Assis Farinha Martins. "New bio-composites based on short fibre reinforced hydroxypropylcellulose films." Composite interfaces 8 (2001): 233-241. AbstractWebsite

The present work deals with the preparation and the characterisation of solid films, having thickness between 15 and 40 μm, prepared with hydroxypropyl cellulose (HPC) and different amounts of commercial cellulose fibres (0; 0.5; 10 and 15% w/w) (system A) and with 1,4-butyl diisocyanate (BDI), as a cross-linking agent (system B). Before the preparation of these films, the surface energy of cellulose fibres, as such and after purification with different solvents, was determined by Inverse Gas Chromatography (IGC), which gave the values of dispersive energy and acid-base properties of their surfaces. The tensile and photo-elastic properties of the solid films obtained were studied. There were no significant changes in Young's modulus between the two systems. However, as expected, the values of the elongation and those of the fracture stress were systematically higher for system B in comparison with system A. The same trend was found for the birefringence, measured at the same elongation values for the films obtained from both systems.

Borges, João Paulo, Maria Helena Godinho, Joao Luis Figueirinhas, MN de Pinho, and Mohamed Naceur Belgacem. "All-cellulosic based composites." In Cellulose Fibers: Bio-and Nano-Polymer Composites, edited by Susheel Kalia, B. S. Kaith and Inderjeet Kaur, 399-421. Springer Berlin Heidelberg, 2011. Abstract

The use of cellulosic fibers as load bearing constituents in composite materials has increased over the last decade due to their relative cheapness compared to conventional materials such as glass and aramid fibers, their ability to recycle, and because they compete well in terms of strength per weight of material. All-cellulosic based composites prepared from cellulose derivatives based matrices and microcrystalline cellulosic fibers made by direct coupling between fibers and matrix present interesting mechanical and gas permeation properties, thus being potential candidates for packaging materials. Both the cellulosic matrix and the reinforcing fibers are biocompatible and widely used in the pharmaceutical industry, which is very important for the envisaged application. In addition to their biocompatibility, cellulosic systems have the ability to form both thermotropic and lyotropic chiral nematic phases, and the composites produced from the latter show improved mechanical properties due to fiber orientation induced by the anisotropic matrix. The preparation and characterization (morphological, topographical, mechanical, gas barrier properties) of all-cellulosic based composites are described in this chapter.

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.

Canejo, João Paulo, João Paulo Borges, Maria Helena Godinho, Pedro Brogueira, Paulo IC Teixeira, and Eugene M. Terentjev. "Helical Twisting of Electrospun Liquid Crystalline Cellulose Micro-and Nanofibers." Advanced Materials 20 (2008): 4821-4825. AbstractWebsite

Helically twisted fibers can be produced by electrospinning liquid-crystalline cellulose solutions. Fiber topographies are studied by atomic force microscopy, scanning electron microscopy (see figure) and polarized optical microscopy. The fibers have a nearly universal pitch-to-diameter ratio and comprise both right- and left-handed helices.

Carrêlo, Henrique, Paula I. P. Soares, João Borges Borges, and Maria Teresa Cidade. "Injectable Composite Systems Based on Microparticles in Hydrogels for Bioactive Cargo Controlled Delivery." Gels 7 (2021): 147. AbstractWebsite

Engineering drug delivery systems (DDS) aim to release bioactive cargo to a specific site within the human body safely and efficiently. Hydrogels have been used as delivery matrices in different studies due to their biocompatibility, biodegradability, and versatility in biomedical purposes. Microparticles have also been used as drug delivery systems for similar reasons. The combination of microparticles and hydrogels in a composite system has been the topic of many research works. These composite systems can be injected in loco as DDS. The hydrogel will serve as a barrier to protect the particles and retard the release of any bioactive cargo within the particles. Additionally, these systems allow different release profiles, where different loads can be released sequentially, thus allowing a synergistic treatment. The reported advantages from several studies of these systems can be of great use in biomedicine for the development of more effective DDS. This review will focus on in situ injectable microparticles in hydrogel composite DDS for biomedical purposes, where a compilation of different studies will be analysed and reported herein.

Castro, Diogo, Pedro Jaeger, Ana Catarina Baptista, and João Pedro Oliveira. "An Overview of High-Entropy Alloys as Biomaterials." Metals 11 (2021): 648. AbstractWebsite

High-entropy alloys (HEAs) have been around since 2004. The breakthroughs in this field led to several potential applications of these alloys as refractory, structural, functional, and biomedical materials. In this work, a short overview on the concept of high-entropy alloys is provided, as well as the theoretical design approach. The special focus of this review concerns one novel class of these alloys: biomedical high-entropy alloys. Here, a literature review on the potential high-entropy alloys for biomedical applications is presented. The characteristics that are required for these alloys to be used in biomedical-oriented applications, namely their mechanical and biocompatibility properties, are discussed and compared to commercially available Ti6Al4V. Different processing routes are also discussed.

Chaparro, Catarina IP, Liliana R. Loureiro, Manuel Almeida Valente, Paula A. Videira, João Paulo Borges, and Paula I. P. Soares. "Synthesis and Characterization of Magnetic Nanoparticles and their internalization on Tumor Cell Lines." 2019 IEEE 6th Portuguese Meeting on Bioengineering (ENBENG) (2019): 1-4. AbstractWebsite

Truncated sialylated O-glycans, such as cell-surface carbohydrate antigen sialyl-Tn (STn) are overexpressed by several cancer types, but not by the respective normal tissues. STn expression is associated with oncogenesis and metastatic ability of cancer cells, with reduced overall survival and lack of response to chemotherapy. Advances in nanomedicine have resulted in rapid development of biocompatible superparamagnetic iron oxide nanoparticles (SPIONs) with considerable potential in cancer treatment. Therefore, in this study SPIONs coated with oleic acid (OA) or dimercaptosuccinic acid (DMSA) were developed and characterized for internalization in two breast cancer cell lines: cell line expressing the STn antigen and the corresponding control. SPIONs with an average diameter of 8 nm showed superparamagnetic behavior and high potential to be used as magnetic hyperthermia agents. OA and DMSA coating provided high stability of SPIONs in physiological conditions while not changing their main properties. NPs internalization studies showed a higher accumulation of DMSA coated NPs in the breast cancer MDA-MB-231 WT cell line. In MDA-MB-231 cell line expressing STn both coated NPs showed a similar accumulation. Therefore, STn antigen can act as a receptor capable of detecting and covalently bind to the molecules present on NPs surface and induce their cellular uptake by endocytosis.

Cidade, Maria Teresa, Diogo J. Ramos, Jenifer Santos, Núria Calero, J. Muñoz, and João Paulo Borges. "Injectable hydrogels based on pluronic/water systems filled with alginate microparticles: Rheological characterization." Publisher Logo Conference Proceedings 1981 (2018): 020091. AbstractWebsite

In this paper the rheological characterization of Pluronic/water systems filled with alginate microparticles is presented. The rheological characterization of the Pluronic/water systems allowed for the choice of the best Pluronic concentration taking into account its applications as injectable hydrogels for tissue repair. The effect on the rheological behavior of the addition of alginate microparticles, to be loaded with the drug, was analyzed and the maximum concentration of microparticles determined.

Cristovão, Ana Filipa, David Sousa, Filipe Silvestre, Inês Ropio, Ana Gaspar, Célia Henriques, Alexandre Velhinho, Ana Catarina Baptista, Miguel Faustino, and Isabel Ferreira. "Customized tracheal design using 3D printing of a polymer hydrogel: influence of UV laser cross-linking on mechanical properties." 3D Printing in Medicine 5 (2019): 12. AbstractWebsite

The use of 3D printing of hydrogels as a cell support in bio-printing of cartilage, organs and tissue has attracted much research interest. For cartilage applications, hydrogels as soft materials must show some degree of rigidity, which can be achieved by photo- or chemical polymerization. In this work, we combined chemical and UV laser polymeric cross-linkage to control the mechanical properties of 3D printed hydrogel blends. Since there are few studies on UV laser cross-linking combined with 3D printing of hydrogels, the work here reported offered many challenges.

Polyethylene glycol diacrylate (PEGDA), sodium alginate (SA) and calcium sulphate (CaSO4) polymer paste containing riboflavin (vitamin B2) and triethanolamine (TEOHA) as a biocompatible photoinitiator was printed in an extrusion 3D plotter using a coupled UV laser. The influence of the laser power on the mechanical properties of the printed samples was then examined in unconfined compression stress-strain tests of 1 × 1 × 1 cm3 sized samples. To evaluate the adhesion of the material between printed layers, compression measurements were performed along the parallel and perpendicular directions to the printing lines.

At a laser density of 70 mW/cm2, Young’s modulus was approximately 6 MPa up to a maximum compression of 20% in the elastic regime for both the parallel and perpendicular measurements. These values were within the range of biological cartilage values. Cytotoxicity tests performed with Vero cells confirmed the cytocompatibility.

We printed a partial tracheal model using optimized printing conditions and proved that the materials and methods developed may be useful for printing of organ models to support surgery or even to produce customized tracheal implants, after further optimization.

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.

Delgado, Beatriz, Henrique Carrêlo, Mónica V. Loureiro, Ana C. Marques, João Borges Borges, and Maria Teresa Cidade. "Injectable hydrogels with two different rates of drug release based on pluronic/water system filled with poly(ε-caprolactone) microcapsules." Journal of Materials Science 56 (2021): 13416-13428. AbstractWebsite

The present paper regards the preparation and characterization of Pluronic F127 + F68/water/poly (ε-caprolactone) microcapsules (MCs) composite systems for tissue repair. The first part of the work relates to the production of poly(ε-caprolactone) (PCL) MCs via water-in-oil-in-water (W/O/W) double emulsion system combined with solvent evaporation method. The study of different process parameters in the final MCs characteristics and their drug release profile is herein reported. Different percentages of PCL, emulsion stabilizer, and volume proportions of the emulsion constituents have been tested, leading to considerable differences in the MCs size distributions. The selected MCs, containing an aqueous solution of methylene blue (MB) as a model drug, were then used to fill a Pluronic F127 + F68/water system leading to the final composite system (5 and 10 wt % MB loaded PCL MCs). The composite systems were characterised in the second part of the work in terms of its rheological behaviour and drug release performance. They were found to gellify at 30 °C, and present an extended drug release to a total of 18 days. The models that best define the release profiles were also studied, with the release of MB occurring mostly by Fick diffusion and polymer chain relaxation. Pluronic F127 + F68/water/poly (ε-caprolactone) MCs composite system is shown to be a promising injectable system, with two different drug release rates, for tissue repair.

Delgado-Lima, Ana, João Paulo Borges, Isabel Ferreira, and Ana Machado. "Fluorescent and conductive cellulose acetate-based membranes with porphyrins." Materials today Communications 11 (2017): 26-37. AbstractWebsite

The unique properties of electrospun nanofibers combined with functional compounds allow the preparation of novelty materials that can be employed in a wide range of applications. Among a vast number of polymers, Cellulose Acetate (CA) it is considered easy to electrospun and it was employed as the polymeric matrix, where free and iridium-porphyrins were incorporated. Two different solvent systems were employed according to the porphyrin used, and the best dispersion level on both the electrospun solution and the membranes, was achieved with the iridium porphyrin. The nanofibers with this porphyrin also exhibited electrical properties, while the fluorescence was quenched by the presence of specific axial ligands.

Echeverria, Coro, Susete N. Fernandes, Maria Helena Godinho, João Borges Borges, and Paula I. P. Soares. "Functional Stimuli-Responsive Gels: Hydrogels and Microgels." Gels 4 (2018): 54. AbstractWebsite

One strategy that has gained much attention in the last decades is the understanding and further mimicking of structures and behaviours found in nature, as inspiration to develop materials with additional functionalities. This review presents recent advances in stimuli-responsive gels with emphasis on functional hydrogels and microgels. The first part of the review highlights the high impact of stimuli-responsive hydrogels in materials science. From macro to micro scale, the review also collects the most recent studies on the preparation of hybrid polymeric microgels composed of a nanoparticle (able to respond to external stimuli), encapsulated or grown into a stimuli-responsive matrix (microgel). This combination gave rise to interesting multi-responsive functional microgels and paved a new path for the preparation of multi-stimuli “smart” systems. Finally, special attention is focused on a new generation of functional stimuli-responsive polymer hydrogels able to self-shape (shape-memory) and/or self-repair. This last functionality could be considered as the closing loop for smart polymeric gels.

Echeverria, Coro, Paula I. P. Soares, Ana Robalo, Laura Pereira, Carlos Novo, Isabel Ferreira, and João Paulo Borges. "One-pot synthesis of dual-stimuli responsive hybrid PNIPAAm-chitosan microgels." Materials & Design 86 (2015): 745-751. AbstractWebsite

The incorporation of magnetic nanoparticles into poly(N-isopropylacrylamide) (PNIPAAm) and chitosan microgels gives rise to hybrid systems that combine the microgels swelling capacity with the interesting features presented in magnetic nanoparticles. The presence of chitosan that act as surfactant for magnetic nanoparticles provides a simplistic approach which allows the encapsulation of magnetic nanoparticles without any previous surface modification. Spherical and highly monodisperse microgels with diameters in the range of 200 to 500 nm were obtained. The encapsulation of magnetic nanoparticles in the polymer matrix was confirmed by high resolution Scanning Electron Microscopy in transmission mode. Volume phase transition of the microgels was accessed by Dynamic Light Scattering measurements. It was observed that the thermosensitivity of the PNIPAM microgels still persists in the hybrid microgels; however, the swelling ability is compromised in the microgels with highest chitosan content. The heating performance of the hybrid magnetic microgels, when submitted to an alternating magnetic field, was also evaluated demonstrating the potential of these systems for hyperthermia treatments.

Faria, Jaime, Bruno Dionísio, Iris Soares, Ana Catarina Baptista, Ana Cláudia Marques, Lídia Gonçalves, Ana Bettencourt, Carlos Baleizão, and Isabel Ferreira. "Cellulose acetate fibres loaded with daptomycin for metal implant coatings." Carbohydrate polymers (2021): 118733. AbstractWebsite

Multifunctional polymeric coatings containing drug delivery vehicles can play a key role in preventing/reducing biofilm formation on implant surfaces. Their requirements are biocompatibility, good adhesion, and controllable drug release. Although cellulose acetate (CA) films and membranes are widely studied for scaffolding, their applications as a protective coating and drug delivery vehicle for metal implants are scarce. The reason is that adhesion to stainless steel (SS) substrates is non-trivial. Grinding SS substrates enhances the adhesion of dip-coated CA films while the adhesion of electrospun CA membranes is improved by an electrosprayed chitosan intermediate layer. PMMA microcapsules containing daptomycin have been successfully incorporated into CA films and fibres. The released drug concentration of 3 x10-3 mg/mL after 120 minutes was confirmed from the peak luminescence intensity under UV radiation of simulated body fluid (SBF) after immersion of the fibres.

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.

Ferreira, Isabel, Ana Catarina Baptista, Joaquim Pratas Leitão, Jorge Soares, Elvira Fortunato, Rodrigo Martins, and João Paulo Borges. "Strongly Photosensitive and Fluorescent F8T2 Electrospun Fibers." Macromol Mater Eng 298 (2013): 174-180. AbstractWebsite

Electrospun fibers of poly[(9,9-dioctylfluorenyl-2,7-diyl)-co-bithiophene] (F8T2) with exceptional electro-optical performance are obtained. The I/T characteristics measured in fibers with 7–15 µm diameter and 1 mm length show a semiconductor behavior; their thermal activation energy is 0.5 eV and the dark conductivity at RT is 5 × 10−9 (Ω cm)−1. Besides exhibiting a photosensitivity of about 60 under white light illumination with a light power intensity of 25 mW · cm−2, the fibers also attain RT photoluminescence in the cyan, yellow, and red wavelength range under ultraviolet, blue, and green light excitation, respectively. Optical microscope images of F8T2 reveal homogeneous electrospun fibers, which are in good agreement with the uniformly radial fluorescence observed.

Ferreira, José Luis, Susana Gomes, Célia Henriques, João Paulo Borges, and Jorge Carvalho Silva. "Electrospinning polycaprolactone dissolved in glacial acetic acid: Fiber production, nonwoven characterization, and In Vitro evaluation." Journal of Applied Polymer Science 131 (2014): 41068. AbstractWebsite

The electrospinning of polycaprolactone (PCL) dissolved in glacial acetic acid and the characterization of the resultant nonwoven fiber mats is reported in this work. For comparison purposes, PCL fiber mats were also obtained by electrospinning the polymer dissolved in chloroform. Given the processing parameters chosen, results show that 14 and 17 wt % PCL solutions are not viscous enough and yield beaded fibers, 20 and 23 wt % solutions give rise to high quality fibers and 26 wt % solutions yield mostly irregular and fused fibers. The nonwoven mats are highly porous, retain the high tensile strain of PCL, and the fibers are semicrystalline. Cells adhere and proliferate equally well on all mats, irrespective of the solvent used in their production. In conclusion, mats obtained by electrospinning PCL dissolved in acetic acid are also a good option to consider when producing scaffolds for tissue engineering. Moreover, acetic acid is miscible with polar solvents, which may allow easier blending of PCL with hydrophilic polymers and therefore achieve the production of electrospun nanofibers with improved properties.

Franco, Patrícia Q., Carlos João, Jorge Carvalho Silva, and João Paulo Borges. "Electrospun hydroxyapatite fibers from a simple sol–gel system." Materials Letters 67 (2012): 233-236. AbstractWebsite

This work reports the production of hydroxyapatite (HA) sub-micron fibers by combining electrospinning and a non-alkoxide sol–gel system, using cheap precursors. Phosphorus pentoxide (P2O5) and calcium nitrate tetrahydrate (Ca(NO3)2.4H2O) were used as precursors of phosphorus and calcium, respectively. The fibers were electrospun from a mixture of the gel formed from the system Ca(NO3)2.4H2O/P2O5 with polymeric solutions of polyvinylpyrrolidone (PVP) in water and ethanol/water mixtures. The fibers were analyzed for their morphology (Scanning Electron Microscopy, SEM), chemical composition (Fourier Transform Infrared Spectroscopy, FTIR) and structure (X-ray diffraction, XRD). The fibers obtained were composed mainly of type B carbonated HA with traces of β-tricalcium phosphate (β-TCP). SEM analysis revealed that increasing the concentration of water in the solvent system, used in the preparation of electrospinning solutions, led to fibers with smaller diameters and narrower diameter distribution.

Gavinho, Sílvia R., Manuel P. Graça, Pedro Prezas, João Borges Borges, Jorge Carvalho Silva, Eduardo Pires, Henrique Armês, and José Coucelo. "Antibacterial bioglass in dental implants: a canine clinical study." European Journal of Public Health 31 (2021): ckab120.006. AbstractWebsite

Peri-implantitis is considered the most challenging biological complication in implantology, as untreated disease can progress and result in implant loss. Therefore, disease prevention is crucial in daily clinical practice. It has been reported that the use of bioactive glass, as an implant coating, can stimulate tissue integration and accelerate tissue regeneration. Besides these properties, it is possible to promote bacterial activity by inserting silver into the bioglass

Bioglass with composition 45S5 was synthesised by the fusion method, replacing the amount of Na2CO3 by AgNO3 (BG 2% wt). The implants were resealed by the CoBlast® technique. Clinical cases with pathology of the mandible/maxilla were selected and implants dimensioned for the canine bone structure were applied.

Three months after implantation, imaging exams, namely CT scans, showed no signs of early rejection by septic or cytotoxic loss. No decrease or loss of peri-implant bone was observed. In all cases the implants remained without signs of instability, and with sufficient support for the application of the exo-prosthesis or dental crown. The results of histological analysis showed no signs of infection or osteolysis. The zone of peri-implant fibrosis was not observable in the samples, showing a good evolution in implant osteointegration.

The results show promising evidences for the use of this biomaterial as a coating, since aseptic rejection, later on, and that related to the shape and biomaterials used in the implant's design, usually begins during the first 3 months.

Gavinho, Sílvia R., Mariana Castro Soares, João Borges Borges, Jorge Carvalho Silva, Isabel Sá Nogueira, and Manuel P. Graça. "Preparation and Characterization of Zinc and Magnesium Doped Bioglasses." Nanoscience and Nanotechnology in Security and Protection against CBRN Threats (2020): 465-475. AbstractWebsite

Peri-implantitis is an infectious disease that affects about one of five patients who receive a dental implant within 5 years after the surgery. To minimize this reaction the development of new biomaterials with antibacterial action is needed that can be used as a coating material in orthodontic implants. In addition, these biomaterials can be doped with several ions, which add specific properties that may act at the cellular level, such as increasing the angiogenesis efficiency. In this work, 45S5 Bioglass® has been used as the base material because it presents higher bioactivity compared to other biomaterials. To add antibacterial function and increase positive effects on bone metabolism, zinc and magnesium ions were introduced in the glass network. The main objective was the synthesis of the 45S5 glass by melt-quenching and study the biological performance as function of the zinc and magnesium concentrations. The structural and biological properties of the prepared samples are discussed.

Gavinho, Sílvia R., Pedro R. Prezas, Diogo J. Ramos, Isabel Sá-Nogueira, João Borges Borges, Carmo M. Lança, Jorge Carvalho Silva, Célia Henriques, Eduardo Pires, Jakka Suresh Kumar, and Manuel P. Graça. "Nontoxic glasses: Preparation, structural, electrical and biological properties." Applied Ceramics Technology 16 (2019): 1885-1894. AbstractWebsite

Bacterial infections affect about 1 in 5 patients who receive a dental implant within 5 years of surgery. To avoid the implant rejection it is necessary for the development of innovative biomaterials, with addition or substitution of the ions, for implant coatings that promote a strong bond with the new host bone and antibacterial action. The objective of this work was to synthesize a bioactive glass with different silver concentrations to evaluate their antibacterial performance. The glasses were synthesized with up to 2% silver content by melt-quenching. Structural, morphological, biological, and electrical properties of all samples were studied. The biological behavior was evaluated through cytotoxicity tests and antibacterial activity. The structural analysis shows that the introduction of silver do not promote significant changes, not altering the advantageous properties of the bioglass of the bioglass. It was verified that the glasses with a silver content from 0.5% to 2%, completely prevented the growth of both Staphylococcus aureus and Escherichia coli while being nontoxic toward mammalian cells. Therefore, these bioglasses are promising materials to be used in the production of dental implants with antimicrobial activity.

Godinho, Maria Helena, João Paulo Canejo, Luis FV Pinto, João Paulo Borges, and Paulo IC Teixeira. "How to mimic the shapes of plant tendrils on the nano and microscale: spirals and helices of electrospun liquid crystalline cellulose derivatives." Soft Matter 5 (2009): 2772-2776. AbstractWebsite

We show that suspended nano and microfibres electrospun from liquid crystalline cellulosic solutions will curl into spirals if they are supported at just one end, or, if they are supported at both ends, will twist into a helix of one handedness over half of its length and of the opposite handedness over the other half, the two halves being connected by a short straight section. This latter phenomenon, known as perversion, is a consequence of the intrinsic curvature of the fibres and of a topological conservation law. Furthermore, agreement between theory and experiment can only be achieved if account is taken of the intrinsic torsion of the fibres. Precisely the same behaviour is known to be exhibited by the tendrils of climbing plants such as Passiflora edulis, albeit on a lengthscale of millimetres, i.e., three to four orders of magnitude larger than in our fibres. This suggests that the same basic, coarse-grained physical model is applicable across a range of lengthscales.

Godinho, Maria Helena, João Paulo Borges, João Carlos Bordado, Maria Teresa Cidade, and Assis Farinha Martins. "Preparation and liquid-crystalline properties of toluene-4-sulphonyl urethane of hydroxypropylcellulose." Liquid Crystals 14 (1993): 653-659. AbstractWebsite

A novel liquid-crystalline polymer, the toluene-4-sulphonyl urethane of hydroxypropylcellulose (TSUHPC), was prepared through chemical modification of hydroxypropylcellulose (HPC) of Mw = 60000 g mol−1. The resulting polymer was characterized by infrared spectroscopy, differential scanning calorimetry (DSC) and polarizing microscopy. It was found that thermotropic liquid crystal phases are formed between about 60°C and 110°C. Concentrated solutions of TSUHPC in acetone and N,N-dimethylacetamide exhibit cholesteric behaviour, at room temperature. When approaching the lyotropic mesophase to solid transition, either by cooling or by solvent evaporation, very interesting arborescent structures of a seemingly fractal nature may be observed, depending on the kinetics of the transition. A banded texture can be observed when the polymer is sheared near the transition to the isotropic phase.

Gomes, Susana, Diana Querido, José Luís Ferreira, João Borges Borges, Célia Henriques, and Jorge Carvalho Silva. "Using water to control electrospun Polycaprolactone fibre morphology for soft tissue engineering." Journal of Polymer Research 26 (2019): 222. AbstractWebsite

Control of the properties of electrospun polycaprolactone can be achieved by adjusting the acetic acid:water ratio used to dissolve and electrospin the polymer. In this work, we studied the effect of using up to 15 wt% water in the solvent mixture. Solution conductivity and viscosity and fibre morphology vary dramatically with water content and solution age. Two days after initial solution preparation, electrospinning yields regular fibres for a water content of 0 wt% and 5 wt%, irregular fibres for a 10 wt% water content and irregular and fused fibres for a 15 wt% water content. Fibres with the highest crystallinity (60%) were obtained from solutions containing 5 wt% water while the highest elastic modulus (8.6 ± 1.4 MPa) and tensile stress (4.3 ± 0.3 MPa) pertain to fibres obtained from solutions containing 10 wt% water. Enzymatic fibre degradation is faster the higher the water content in the precursor solution. Adhesion ratio of human foetal fibroblasts was highest on scaffolds obtained from precursor solutions containing 0 wt% water. Cell population increases for all scaffolds and populations quickly become equivalent, with no statistically significant differences between them. Cells exhibit a more extended morphology on the 5 wt% scaffold and a more compact morphology on the 0 wt% scaffold. In summary, a small water content in the solvent allows a significant control over fibre diameter, scaffold properties and the production of scaffolds that support cell adhesion and proliferation. This strategy can be used in soft tissue engineering to influence cell behaviour and the degradation rate of the scaffolds.

Gonçalves, Adriana, Filipe V. Almeida, João Paulo Borges, and Paula I. P. Soares. "Incorporation of Dual-Stimuli Responsive Microgels in Nanofibrous Membranes for Cancer Treatment by Magnetic Hyperthermia." Gels 7 (2021): 28. AbstractWebsite

The delivery of multiple anti-cancer agents holds great promise for better treatments. The present work focuses on developing multifunctional materials for simultaneous and local combinatory treatment: Chemotherapy and hyperthermia. We first produced hybrid microgels (MG), synthesized by surfactant-free emulsion polymerization, consisting of Poly (N-isopropyl acrylamide) (PNIPAAm), chitosan (40 wt.%), and iron oxide nanoparticles (NPs) (5 wt.%) as the inorganic component. PNIPAAm MGs with a hydrodynamic diameter of about 1 μm (in their swollen state) were successfully synthesized. With the incorporation of chitosan and NPs in PNIPAAm MG, a decrease in MG diameter and swelling capacity was observed, without affecting their thermosensitivity. We then sought to produce biocompatible and mechanically robust membranes containing these dual-responsive MG. To achieve this, MG were incorporated in poly (vinyl pyrrolidone) (PVP) fibers through colloidal electrospinning. The presence of NPs in MG decreases the membrane swelling ratio from 10 to values between 6 and 7, and increases the material stiffness, raising its Young modulus from 20 to 35 MPa. Furthermore, magnetic hyperthermia assay shows that PVP-MG-NP composites perform better than any other formulation, with a temperature variation of about 1 °C. The present work demonstrates the potential of using multifunctional colloidal membranes for magnetic hyperthermia and may in the future be used as an alternative treatment for cancer.

Graça, Manuel P., Silvia Soreto Teixeira, Sílvia R. Gavinho, Manuel Almeida Valente, Cristiana Salgueiro, José Nunes, Paula I. P. Soares, Maria Carmo Lança, Tânia Vieira, Jorge Carvalho Silva, and João Borges Borges. "Nanomaterials for magnetic hyperthermia." European Journal of Public Health 31 (2021): ckab120.066. AbstractWebsite

Cancer remains as one of the major causes of mortality worldwide. Recent advances in nanoparticles based therapy mark a new era on cancer treatment. Many groups have investigated biological/physical effects of nanoparticles on tumour cells and how these vary with physical parameters such as particle size, shape, concentration and distribution. Magnetic hyperthermia (MHT) can be an alternative or an add-value therapy with demonstrated effectiveness. MHT uses magnetic nanoparticles, which can be directly applied to the tumour, where, by applying an external ac magnetic field, will promote a localized temperature increment that can be controlled.

Henriques, Célia, Ricardo Vidinha, David Botequim, João Paulo Borges, and Jorge Carvalho Silva. "A systematic study of solution and processing parameters on nanofiber morphology using a new electrospinning apparatus." Journal of nanoscience and nanotechnology 9 (2009): 3535-3545. AbstractWebsite

We assembled a new electrospinning apparatus and used poly(ethylene oxide) as a model polymer to perform a systematic study on the influence of solution and processing parameters on the morphology of electrospun nanofibers. Solution parameters studied were polymer concentration and molecular mass. The solvent used, 60 wt% water,40 wt% ethanol, was the same throughout the study. Processing parameters analyzed were: solution feed rate, needle tip-collector distance and electrostatic potential difference between the needle and collector. Solution viscosity increased both with polymer concentration and molecular mass. Polymer concentration plays a decisive role on the outcome of the electrospinning process: a low concentration led to the formation of beaded fibers; an intermediate concentration yielded good quality fibers; a high concentration resulted in a bimodal size distribution and at even higher concentration a distributed deposition. Fiber diameter increased with polymer molecular mass and higher molecular masses are associated with a higher frequency of splaying events. Fiber diameter increased linearly with solution feed rate. While an increase in needle-collector distance represents a weaker electric field, a greater distance to be covered by the fibers and a longer flight time, presumably favoring the formation of thinner fibers, as solvent evaporation leads to a local increase of concentration and viscosity, viscoelastic forces opposing stretching caused an increase of fiber diameter with needle-collector distance. A higher voltage applied at the needle is associated with a higher charging of the polymer and a higher electrical current through it ultimately leading to incomplete solvent evaporation and merged fibers being produced. Controlling the charging of the polymer independently of the electric field strength was achieved by applying a voltage to the collector while distance and potential difference were kept constant. The increased electrostatic repulsion associated with an increase of the high voltage applied to the needle led to the disappearance of merged fibers.

João, Carlos, Rute Almeida, Jorge Carvalho Silva, and João Paulo Borges. "A simple sol-gel route to the construction of hydroxyapatite inverted colloidal crystals for bone tissue engineering." Materials Letters 185 (2016): 407-410. AbstractWebsite

Hydroxyapatite (HAp) scaffolds with uniform pore size and interconnected pore network were constructed based on the inverted colloidal crystal (ICC) geometry and a simple sol-gel formulation. Monodisperse polystyrene microspheres were self-assembled and annealed into a hexagonal close packed structure. HAp sol-gel was infiltrated in this template followed by thermal treatment for simultaneous HAp matrix sintering and polymeric colloidal crystal calcination. The resultant ICC scaffolds exhibit an ordered architecture that was able to offer a favorable environment for human osteoblasts adhesion and proliferation, an essential feature for bone ingrowth in tissue engineering applications.