Encapsulation of diclofenac sodium within polymer beads by silica species via vapour-phase synthesis.

The present study concerns the preparation of ternary composites via the in situ encapsulation of solid dispersion of diclofenac sodium within the acrylic polymer beads. The encapsulating species were produced through the hydrolysis and condensation of the silica precursors (tetraethoxysilane or ethyltriethoxysilane) introduced into the solid dispersion. The transformation of precursors occurred in the vapor phase of ammonia. A great advantage of the presented vapor-phase method is preventing the desorption of the highly soluble drug during gelation of silica precursors, which stands in contrast to the conventional sol-gel processes occurring in the solution. The conducted studies, involving the low temperature N2 sorption together with spectroscopic techniques, provide insight into the structural differences of drug loaded particles. They reveal that the formation of silica gel accompanies the conversion of the drug into its amorphous form. Finally, the desorption profiles of diclofenac sodium demonstrate that the deposition of silica gel successfully diminishes the degree of the initial drug desorption while significantly modifying its release rate.

Photodegradation of Stearic Acid Adsorbed on Superhydrophilic TiO2 Surface: In Situ FT-IR and LDI Study.

TiO2 films prepared by template-assisted sol-gel method were characterized by X-ray diffraction spectroscopy, scanning and atomic force electron microscopy, and Fourier transform infrared (FT-IR) spectroscopy. Based on the hexane adsorption-desorption analysis, the films have a surface area of 390-540 m(2)/g with pore size distribution narrowly centered around 10 nm. Optimal component ratio and condition of heat treatment of mesoporous titania films have been found. Photocatalytic activity of the coatings was determined by the destruction of stearic acid layers, monitored using FT-IR spectroscopy and laser desorption-ionization (LDI) mass spectrometry. Under UV illumination, all the used films reach hydrophilicity with water contact angle of 0°. As the result, hydrophobic fat acid molecules undergo self-association and active desorption from the hydrophilic surface during mass-spectrometric experiment.

Insight into the structure of polymer-silica nano-composites prepared by vapor-phase.

Using a new synthesis technique, in which mesoporous Amberlite XAD7HP resin beads swollen with TEOS were exposed to vapors of either (H2O+HCl) or (H2O+NH3), we obtained smooth, porous, mechanically stable silica gel spheres after burning out the sacrificial organic template. Combined N2 sorption, SEM, TEM, (29)Si NMR, and Raman measurements were used to characterize the physical properties and molecular structures of the intermediate and final gels. Our atomically resolved TEM pictures provide the first visual demonstration of the presence of 3 to 6 member siloxane rings predicted by our Raman studies and other indirect methods. It is demonstrated that the physical appearance, morphology and porosity of the acid and base set gels are different from each other and also from those silica gels that were earlier polymerized from TEOS or Na-silicate saturated Amberlite XAD7HP with aqueous NH4OH or HCl solutions in liquid phase. We show that the different physical properties of the vapor-phase set gels are associated with different gelling rates at acidic and basic conditions, which generates molecular differences both in the intermediate and the final products.

Synthesis and characterization of nanostructural polymer-silica composite: positron annihilation lifetime spectroscopy study.

The swelling of poly(TRIM) spherical particles in TEOS is assessed as a potential way for obtaining polymer-silica nanocomposite materials. Silica deposition was achieved by simply stirring of swollen polymer particles in acidic hydrochloric-water solution. This procedure leads to spherical composite particles with dispersed silica gel within the polymer matrix. The resulting material exhibits the same morphology as the initial polymer. Nanocomposite particles are silica rich (about 17 wt.%). Characterization of the nanocomposites was performed using scanning electron microscopy, FT-IR spectroscopy, (29)Si CP MAS NMR spectroscopy and thermogravimetry. Moreover, the use of positron annihilation lifetime spectroscopy PALS to characterize the structural properties of the nanocomposites is presented. This technique gave more realistic pieces of information about the pore structure of the investigated samples in contrast to nitrogen adsorption studies.

Polymer/silica composite of core-shell type by polymer swelling in TEOS.

Monodisperse polymer/silica composite material with a polymer as the core and hydrophilic silica gel as the shell was prepared by a two-stage procedure. In the first stage, the swelling of Amberlite XAD7HP particles in tetraethoxysilane (TEOS) was performed. Subsequently a portion of the XAD7HP particles impregnated with TEOS were transferred to acidic aqueous solution to facilitate a sol-gel process of the silica precursor. This procedure is assessed as a potential route to a composite material with a core-shell morphology. Scanning electron microscopy and (29)Si MAS NMR indicated the formation of silica microfibers on polymer beads. The silica microfibers were anchored in the polymer matrix. In consequence, the silica shell exhibited relatively high mechanical stability. The swelling of the polymer and the formation of the silica phase substantially changed the porosity of the initial polymer material. The final composite surprisingly exhibited very homogeneous porosity. The textural characteristics of the investigated materials were defined by nitrogen adsorption-desorption at 77K.

Porosity evolution of VP-DVB/MCM-41 nanocomposite.

The porous structure of nanostructured vinylpyrrolidone-divinylbenzene (VP-DVB)/MCM-41 composite was characterized using N(2) adsorption at 77K and positronium annihilation lifetime spectroscopy (PALS), atomic force microscopy (AFM) and Raman spectroscopy. Positron annihilation lifetime spectra were measured during outgassing procedure. The voids of differentiated dimensions were detected in the composite material. The number of free volumes and their dimensions depend on the degree of evacuation of volatile components from the samples.