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1.
Materials (Basel) ; 13(22)2020 Nov 13.
Artículo en Inglés | MEDLINE | ID: mdl-33202741

RESUMEN

There is an increasing clinical need to develop novel biomaterials that combine regenerative and biocidal properties. In this work, we present the preparation of silver/silica-based glassy bioactive (ABG) compositions via a facile, fast (20 h), and low temperature (80 °C) approach and their characterization. The fabrication process included the synthesis of the bioactive glass (BG) particles followed by the surface modification of the bioactive glass with silver nanoparticles. The microstructural features of ABG samples before and after exposure to simulated body fluid (SBF), as well as their ion release behavior during SBF test were evaluated using infrared spectrometry (FTIR), ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), electron microscopies (TEM and SEM) and optical emission spectroscopy (OES). The antibacterial properties of the experimental compositions were tested against Escherichia coli (E. coli). The results indicated that the prepared ABG materials possess antibacterial activity against E. coli, which is directly correlated with the glass surface modification.

2.
Materials (Basel) ; 12(23)2019 Nov 22.
Artículo en Inglés | MEDLINE | ID: mdl-31766736

RESUMEN

In the present work, Ca-containing silicon oxycarbides (SiCaOC) with varying Ca content have been synthesized via sol-gel processing and thermal treatment in inert gas atmosphere (pyrolysis). It has been shown that the as-prepared SiCaOC materials with low Ca loadings (Ca/Si molar ratios = 0.05 or 0.12) were X-ray amorphous; their glassy network contains Q3 sites, indicating the presence of Ca2+ at non-bridging-oxygen sites. SiCaOC with high Ca content (i.e., Ca/Si molar ratio = 0.50) exhibits the presence of crystalline calcium silicate (mainly pseudowollastonite). Furthermore, it has been shown that the incorporation of Ca into the SiOC glassy network has a significant effect on its porosity and specific surface area. Thus, the as-prepared Ca-free SiOC material is shown to be non-porous and having a specific surface area (SSA) of 22.5 m2/g; whereas SiCaOC with Ca/Si molar ratio of 0.05 exhibits mesoporosity and a SSA value of 123.4 m2/g. The further increase of Ca content leads to a decrease of the SSA and the generation of macroporosity in SiCaOC; thus, SiCaOC with Ca/Si molar ratio of 0.12 is macroporous and exhibits a SSA value of 39.5 m2/g. Bioactivity assessment in simulated body fluid (SBF) confirms the hydroxyapatite formation on all SiCaOC samples after seven days soaking, unlike the relatively inert ternary silicon oxycarbide reference. In particular, SiCaOC with a Ca/Si molar ratio of 0.05 shows an increased apatite forming ability compared to that of SiCaOC with Ca/Si molar ratio of 0.12; this difference is considered to be a direct consequence of the significantly higher SSA of the sample with the Ca/Si ratio of 0.05. The present work indicates two effects of Ca incorporation into the silicon oxycarbide glassy network on its bioactivity: Firstly, Ca2+ is shown to contribute to the slight depolymerization of the network, which clearly triggers the hydroxyapatite formation (compare the bioactive behavior of SiOC to that of SiCaOC with Ca/Si molar ratio 0.12 upon SBF exposure); secondly, the Ca2+ incorporation seems to strongly affect the porosity and SSA in the prepared SiCaOC materials. There is an optimum of Ca loading into the silicon oxycarbide glassy network (at a Ca/Si molar ration of 0.05), which provides mesoporosity and reaches maximum SSA, both highly beneficial for the bioactive behavior of the materials. An increase of the Ca loading leads, in addition to the crystallization of calcium silicates, to a coarsening of the pores (i.e., macroporosity) and a significant decrease of the SSA, both negatively affecting the bioactivity.

3.
ACS Biomater Sci Eng ; 5(10): 5337-5347, 2019 Oct 14.
Artículo en Inglés | MEDLINE | ID: mdl-33464075

RESUMEN

The bioactivity of Ca and/or B modified silicon oxycarbides has been assessed in vitro upon immersion in SBF (simulated body fluid). In the context of the present work, bioactivity refers to the likeliness of hydroxyapatite crystallization (biomineralization) on the surface of a material when in contact with physiological fluids. The incorporation of Ca and B into the silicon oxycarbide glass network is found to increase its bioactivity, which seems to scale with the content of Ca; thus, SiOC glass with a relatively large Ca/Si molar ratio (i.e., 0.12) is shown to exhibit bioactive characteristics similar to those of the benchmark silicate bioactive glass of 45S5 composition. The release kinetics of the SiOC glasses modified with Ca and/or B during the SBF test was studied by inductively coupled plasma-optical emission spectroscopy. It has been observed that the Si release kinetics can be correlated with the Ca content in the SiOC glasses: SiOC based glasses modified with Ca exhibited low Si release activation energies (i.e., 0.07 eV), being comparable to that of 45S5 bioactive glass (i.e., 0.04 eV); whereas silicon oxycarbides without Ca modification showed higher activation energies for Si release (i.e., 0.27 eV).

4.
ACS Appl Mater Interfaces ; 10(12): 10173-10184, 2018 Mar 28.
Artículo en Inglés | MEDLINE | ID: mdl-29504743

RESUMEN

Tin dioxide (SnO2) nanoparticles were straightforwardly synthesized using an easily scaled-up liquid route that involves the hydrothermal treatment, either under acidic or basic conditions, of a commercial tin dioxide particle suspension including potassium counterions. After further thermal post-treatment, the nanomaterials have been thoroughly characterized by Fourier transform infrared and Raman spectroscopy, powder X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and nitrogen sorption porosimetry. Varying pH conditions and temperature of the thermal treatment provided cassiterite SnO2 nanoparticles with crystallite sizes ranging from 7.3 to 9.7 nm and Brunauer-Emmett-Teller surface areas ranging from 61 to 106 m2·g-1, acidic conditions favoring potassium cation removal. Upon exposure to a reducing gas (H2, CO, and volatile organic compounds such as ethanol and acetone) or oxidizing gas (NO2), layers of these SnO2 nanoparticles led to highly sensitive, reversible, and reproducible responses. The sensing results were discussed in regard to the crystallite size, specific area, valence band energy, Debye length, and chemical composition. Results highlight the impact of the counterion residuals, which affect the gas-sensing performance to an extent much higher than that of size and surface area effects. Tin dioxide nanoparticles prepared under acidic conditions and calcined in air showed the best sensing performances because of lower amount of potassium cations and higher crystallinity, despite the lower surface area.

5.
Materials (Basel) ; 9(12)2016 Nov 24.
Artículo en Inglés | MEDLINE | ID: mdl-28774079

RESUMEN

Novel bioactive glasses based on a Ca- and Mg-modified silicon oxycarbide (SiCaMgOC) were prepared from a polymeric single-source precursor, and their in vitro activity towards hydroxyapatite mineralization was investigated upon incubating the samples in simulated body fluid (SBF) at 37 °C. The as-prepared materials exhibit an outstanding resistance against devitrification processes and maintain their amorphous nature even after exposure to 1300 °C. The X-ray diffraction (XRD) analysis of the SiCaMgOC samples after the SBF test showed characteristic reflections of apatite after only three days, indicating a promising bioactivity. The release kinetics of the Ca2+ and Mg2+ and the adsorption of H⁺ after immersion of SiCaMgOC in simulated body fluid for different soaking times were analyzed via optical emission spectroscopy. The results show that the mechanism of formation of apatite on the surface of the SiCaMgOC powders is similar to that observed for standard (silicate) bioactive glasses. A preliminary cytotoxicity investigation of the SiOC-based bioactive glasses was performed in the presence of mouse embryonic fibroblasts (MEF) as well as human embryonic kidney cells (HEK-293). Due to their excellent high-temperature crystallization resistance in addition to bioactivity, the Ca- and Mg-modified SiOC glasses presented here might have high potential in applications related to bone repair and regeneration.

6.
J Phys Chem B ; 117(6): 1664-9, 2013 Feb 14.
Artículo en Inglés | MEDLINE | ID: mdl-22908936

RESUMEN

Monolayers of iron oxide nanoparticles of two different sizes, 9.6 nm and 16.5 nm, were fabricated through electrophoretic deposition. The arrangements of nanoparticles within the films were analyzed using the technique of Voronoi tessellations. These analyses indicated that the films possessed equivalent degrees of ordering, and that the films were uniform over centimeter length scales. Precise measurements of the interparticle spacing were obtained, and the magnitudes of magnetic dipole interactions were calculated. The dipole-dipole interaction among the larger nanoparticles was 14 times larger than that of the smaller nanoparticles, indicating that magnetic coupling interactions could not have been the lone source of ordering in the system.

7.
Nanoscale ; 3(9): 3799-804, 2011 Sep 01.
Artículo en Inglés | MEDLINE | ID: mdl-21845260

RESUMEN

A versatile synthetic method, based on a solvothermal synthesis technique, has been developed for the fabrication of TiO(2) nanocrystals with different shapes, such as nanowires, nanorods and nanospheres. The central characteristic of our approach is the production of a coordination complex at an intermediate stage of the reaction that possesses appropriate symmetry using two distinct ligands, oleic acid and oleylamine. Those ligands have different binding strengths, which specifically dictate the shape of both the coordination complex and the resulting TiO(2) nanostructures. Additionally, this approach yields, for the first time, monodisperse, 4 nm anatase TiO(2) nanocrystals by controlling the symmetry of the intermediate and solvothermal conditions.


Asunto(s)
Ligandos , Nanopartículas del Metal/química , Nanotubos/química , Nanocables/química , Titanio/química , Aminas/química , Nanopartículas del Metal/ultraestructura , Nanotubos/ultraestructura , Nanocables/ultraestructura , Ácido Oléico/química , Solventes/química , Espectroscopía Infrarroja por Transformada de Fourier
8.
ACS Appl Mater Interfaces ; 3(9): 3611-5, 2011 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-21846090

RESUMEN

Iron-oxide nanoparticle monolayers and multilayers were assembled using dc electrophoretic deposition. The rate of deposition and the total particle deposition were controlled by varying the concentration of nanoparticles and the deposition time, respectively. Using scanning electron microscopy, we performed a time-resolved study that demonstrated the growth of the monolayer from a single isolated nanoparticle to a nearly complete layer. We observed tight, hexagonal packing of the nanoparticles indicating strong particle-particle interaction. Multilayer growth was assessed using scanning electron microscopy and atomic force microscopy, revealing a monolayer-by-monolayer growth process.


Asunto(s)
Compuestos Férricos/química , Nanopartículas del Metal/química , Electrodos , Galvanoplastia , Microscopía de Fuerza Atómica
9.
ACS Nano ; 4(12): 7367-72, 2010 Dec 28.
Artículo en Inglés | MEDLINE | ID: mdl-21114272

RESUMEN

This report describes methods to produce large-area films of graphene oxide from aqueous suspensions using electrophoretic deposition. By selecting the appropriate suspension pH and deposition voltage, films of the negatively charged graphene oxide sheets can be produced with either a smooth "rug" microstructure on the anode or a porous "brick" microstructure on the cathode. Cathodic deposition occurs in the low pH suspension with the application of a relatively high voltage, which facilitates a gradual change in the colloids' charge from negative to positive as they adsorb protons released by the electrolysis of water. The shift in the colloids' charge also gives rise to the brick microstructure, as the concurrent decrease in electrostatic repulsion between graphene oxide sheets results in the formation of multilayered aggregates (the "bricks"). Measurements of water contact angle revealed the brick films (79°) to be more hydrophobic than the rug films (41°), a difference we attribute primarily to the distinct microstructures. Finally, we describe a sacrificial layer technique to make these graphene oxide films free-standing, which would enable them to be placed on arbitrary substrates.


Asunto(s)
Grafito/química , Microtecnología/métodos , Óxidos/química , Electroforesis , Suspensiones
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