Silver nanoparticle incorporation into flexible polyamide 12 membranes.

To meet the demands of the market and society, the development of structured polymeric materials for application in the medical field is constantly increasing. Over the last decades, metallic silver nanoparticles have been explored due to their antimicrobial action. Here, we aimed to incorporate metallic silver nanoparticles into polymeric pieces obtained by additive manufacture via a chemical route involving silver nitrate and sodium borohydride. Polyamide 12 membranes were obtained by selective laser sintering, which was followed by washing, pretreatment, and functionalization with the alkoxides tetraethylorthosilicate and 3-aminopropyl tetraethoxysilane. For nanoparticle preparation and incorporation, a chemical route was tested under different conditions. The samples were characterized by techniques, such as X-ray diffraction, ultraviolet-visible spectroscopy, and infrared vibrational spectroscopy. Nanoparticle formation and incorporation into the polyamide 12 membranes were demonstrated by the absorbance band at 420 nm, which indicated that the particles measured between 10 and 50 nm in size; by the X-ray diffraction peaks at 2θ = 38, 44, and 64°, which are typical of crystalline silver; and by vibrational spectroscopy, which evidenced that the nanoparticles interacted with the polyamide 12 nitrogen groups. Polyamide 12 membranes containing metallic silver nanoparticles have promising biomedical applications as antimicrobial wound dressings associated with drug carriers.

Non-hydrolytic Sol-Gel Route: a Powerful Process to Develop UV-Vis-IR Luminescent YVO4 Phosphors.

The spectroscopic properties of lanthanide ions stem from absorption and emission radiation in the solar spectrum range, which promotes numerous applications in areas such as white light emission, bio-imaging, biological markers, and photovoltaic cells, among others. To intensify these properties, several matrixes have been studied, particularly the yttrium vanadate matrix due to its structural, mechanic, and physicochemical properties. The non-hydrolytic sol-gel process is a versatile way to prepare inorganic oxides doped with lanthanide ions. In this work, we describe the synthesis of yttrium vanadate matrixes doped with Eu3+, Er3+, and/or Yb3+ ions (containing 1% lanthanide ions with respect to Y3+ (molar ratio)) by the non-hydrolytic sol-gel, annealed at 800 °C for 4 h, and their characterization by X-ray diffraction and photoluminescence spectroscopy. The X-ray diffraction patterns display the peaks corresponding to the yttrium vanadate tetragonal phase. Laser excitation at 980 nm elicits Er3+ emission bands in the green and red regions and Eu3+ emission at 620 nm. Laser excitation at 322 nm; i.e., the charge transfer band, provides emission in the same regions, as well as infrared emission. This system is a promising candidate for applications in solar cells, optical amplifiers, and biomarkers because it can be excited at different wavelengths. Graphical Abstract Schematic diagram of the energy level of lanthanides and vanadate ions, and energy transfer.

Selective oxidation catalysts obtained by immobilization of iron(III) porphyrins on thiosalicylic acid-modified Mg-Al layered double hydroxides.

Nitrate-intercalated Mg-Al layered double hydroxides (LDHs) were synthesized and exfoliated in formamide. Reaction of the single layer suspension with thiosalicylic acid under different conditions afforded two types of solids: LDHA1, in which the outer surface was modified with the anion thiosalicylate, and LDHA2, which contained the anion thiosalicylate intercalated between the LDH layers. LDHA1 and LDHA2 were used as supports to immobilize neutral (FeP1 and FeP2) and anionic (FeP3) iron(III) porphyrins. For comparison purposes, the iron(III) porphyrins (FePs) were also immobilized on LDH intercalated with nitrate anions obtained by the co-precipitation method. Chemical modification of LDH facilitated immobilization of the FePs through interaction of the functionalizing groups in LDH with the peripheral substituents on the porphyrin ring. The resulting FePx-LDHAy solids were characterized by X-ray diffraction (powder) and UV-Vis and EPR spectroscopies and were investigated as catalysts in the oxidation of cyclooctene and cyclohexane. The immobilized neutral FePs and their homogeneous counterparts gave similar product yields in the oxidation of cyclooctene, suggesting that immobilization of the FePs on the thiosalicylate-modified LDHs only supported the catalyst species without interfering in the catalytic outcome. On the other hand, in the oxidation of cyclohexane, the thiosalicylate anions on the outer surface of LDHA1 or intercalated between the LDHA2 layers influenced the catalytic activity of FePx-LDHAy, leading to different efficiency and selectivity results. FeP1-LDHA2 performed the best (29.6% alcohol yield) due to changes in the polarity of the surface of the support and the presence of FeP1. Interestingly, FeP1 also performed better in solution as compared to the other FePs. Finally, it was possible to recycle FeP1-LDHA2 at least three times.

Synthesis, Characterization, and Environmental Applications of Hybrid Materials Based on Humic Acid Obtained by the Sol-Gel Route.

Humic acids (HAs) are ubiquitous macromolecules in the environment. Due to their high contents of oxygenated functional groups, they can interact with contaminants present in the natural environment and therefore influence the behavior of pollutants. However, a pH of 2 or lower is required to maintain HAs in the solid form. To increase the stability of HAs and their capacity to bind to contaminants, this work proposes the development of new hybrid materials based on alkoxysilanes and HAs for environmental applications such as dye adsorption. Three different materials with new functional groups were prepared by employing the following alkoxysilanes: tetraethyl orthosilicate, (3-aminopropyl)triethoxysilane, and N-[3-(trimethoxylsilyl)propyl]ethylenediamine. The final materials were denoted HWA, HOA, and HTA, respectively, and they were characterized by elemental analysis, diffuse reflectance Fourier-transform infrared spectroscopy (DRIFT), small-angle X-ray scattering (SAXS), scanning electron microscopy (SEM), and N2 gas-volumetric adsorption. The point of zero charge (pzc) and stability of these materials were also determined. Their selectivity was evaluated in adsorption experiments performed with two different charged dyes in aqueous medium, namely anionic rose bengal (RB) and cationic methylene blue (MB). The elemental, DRIFT, SAXS, SEM, and textural analyses confirmed the presence of a combination of the features of HAs and alkoxysilanes. The pzc results showed that the new materials displayed different characteristics and affinities. All the materials were stable in aqueous solution up to pH 10. For MB, the percentage removal values obtained by using HWA, HOA, and HTA were 98, 85, and 67%, respectively. As for RB, the percentage removal values were 19, 18, and 44% for HWA, HOA, and HTA, respectively. These hybrid materials have potential use as adsorbents for the removal of cationic or anionic species and could be viable alternatives to remove various substances present as contaminants in natural environments.

Synthesis and biocompatibility of an experimental glass ionomer cement prepared by a non-hydrolytic sol-gel method.

The aims of this study were to demonstrate the synthesis of an experimental glass ionomer cement (GIC) by the non-hydrolytic sol-gel method and to evaluate its biocompatibility in comparison to a conventional glass ionomer cement (Vidrion R). Four polyethylene tubes containing the tested cements were implanted in the dorsal region of 15 rats, as follows: GI - experimental GIC and GII - conventional GIC. The external tube walls was considered the control group (CG). The rats were sacrificed 7, 21 and 42 days after implant placement for histopathological analysis. A four-point (I-IV) scoring system was used to graduate the inflammatory reaction. Regarding the experimental GIC sintherization, thermogravimetric and x-ray diffraction analysis demonstrated vitreous material formation at 110oC by the sol-gel method. For biocompatibility test, results showed a moderate chronic inflammatory reaction for GI (III), severe for GII (IV) and mild for CG (II) at 7 days. After 21 days, GI presented a mild reaction (II); GII, moderate (III) and CG, mild (II). At 42 days, GI showed a mild/absent inflammatory reaction (II to I), similar to GII (II to I). CG presented absence of chronic inflammatory reaction (I). It was concluded that the experimental GIC presented mild/absent tissue reaction after 42 days, being biocompatible when tested in the connective tissue of rats.

Synthesis and biocompatibility of an experimental glass ionomer cement prepared by a non-hydrolytic sol-gel method

The aims of this study were to demonstrate the synthesis of an experimental glass ionomer cement (GIC) by the non-hydrolytic sol-gel method and to evaluate its biocompatibility in comparison to a conventional glass ionomer cement (Vidrion R). Four polyethylene tubes containing the tested cements were implanted in the dorsal region of 15 rats, as follows: GI - experimental GIC and GII - conventional GIC. The external tube walls was considered the control group (CG). The rats were sacrificed 7, 21 and 42 days after implant placement for histopathological analysis. A four-point (I-IV) scoring system was used to graduate the inflammatory reaction. Regarding the experimental GIC sintherization, thermogravimetric and x-ray diffraction analysis demonstrated vitreous material formation at 110oC by the sol-gel method. For biocompatibility test, results showed a moderate chronic inflammatory reaction for GI (III), severe for GII (IV) and mild for CG (II) at 7 days. After 21 days, GI presented a mild reaction (II); GII, moderate (III) and CG, mild (II). At 42 days, GI showed a mild/absent inflammatory reaction (II to I), similar to GII (II to I). CG presented absence of chronic inflammatory reaction (I). It was concluded that the experimental GIC presented mild/absent tissue reaction after 42 days, being biocompatible when tested in the connective tissue of rats.

O objetivo deste estudo foi demonstrar a sinterização pelo método sol-gel não-hidrolítico de um cimento de ionômero de vidro experimental (CIV) e avaliar sua biocompatibilidade em relação a um cimento de ionômero de vidro convencional (Vidrion R). Quatro tubos de polietileno contendo os cimentos testados foram implantados no dorso de 15 ratos, da seguinte maneira: GI - CIV Experimental e GII - CIV Convencional. A lateral do tubo foi considerada Grupo Controle. Os ratos foram sacrificados em 7, 21 e 42 dias pós-implantação para análise histopatológica. Uma escala de I a IV foi utilizada como sistema de score para graduar a reação inflamatória. Em relação à sinterização do CIV experimental, as análises termogravométrica e por difração de raio-x demonstraram a formação de material vítreo aos 110oC pelo método sol-gel. Para o teste de biocompatibilidade, os resultados mostraram uma reação inflamatória moderada para o GI (III), severa para o GII (IV) e branda para o Grupo Controle (II) aos 7 dias. Após 21 dias, GI apresentou uma reação branda (II); GII, moderada (III) e Grupo Controle, branda (II). Aos 42 dias, GI apresentou uma reação inflamatória branda/ausente (II a I), similar ao GII (II a I). O Grupo Controle demonstrou ausência de reação inflamatória (I). Concluiu-se que o CIV Experimental apresentou reação tecidual branda/ausente após 42 dias, sendo biocompatível quando testado em tecido conjuntivo de ratos.