L. Téllez

FT-IR Study of the Hydrolysis and Polymerization of Tetraethyl Orthosilicate and Polydimethyl Siloxane in the Presence of Tetrabutyl Orthotitanate

Abstract In this work, we have used FT‐IR spectroscopy to study the hydrolysis and polymerization reactions of tetraethyl orthosilicate (TEOS) and polydimethyl‐siloxane (PDMS) in the presence of tetrabutyl orthotitanate (TBOT). These reactions are used for obtaining SiO2–PDMS–TiO2 organically modified silicates (Ormosils). In order to obtain semi‐quantitative information about such reactions, a deconvolution procedure of the FT‐IR spectra has been done by use of a computer program. Hydrolysis reactions have been characterized by Me–O–C (Me = Si, Ti) bonds, and polymerization reactions by Me–O–Me bonds. Instantaneous hydrolysis of TEOS has been observed, together with condensation reactions between Si–OH groups, which give crosslinked and linear Si–O–Si structures. The TBOT is also hydrolyzed, but the high acid concentration inhibits condensation reactions between Ti–OH groups. The PDMS also condenses mainly with Si–OH groups and probably with Ti–OH, finally forming Me–O–PDMS bonds. The formation of Si–O–Si crosslinked structures and also Me–O–PDMS structures continues until the end of reaction. The gelling time is dependent on TBOT concentration in the reaction medium and, therefore, polycondensation reactions are dependent on TBOT concentration.

Solvent effect on the sol-gel synthesis of lithium aluminate

Abstract Lithium aluminate was prepared from different alcohols as solvents. Aluminum sec-butoxide was dissolved with ethyl, isopropyl or n -butyl alcohol and hydrolyzed simultaneously with LiOH. The resulting solids were characterized by XRD, DTA, TGA and SEM. Lithium aluminates were also prepared by fusion and peroxide methods as comparison in thermal behavior. It was found that the precursors are semi-cristalline Al-Li mixed carbonates if ethyl or isopropyl alcohol was used, whereas a highly cristalline Al–Li hydroxyl was obtained with the n -butyl alcohol. In the ethyl and isopropyl calcined preparations (800°C), the carbonates were partially eliminated, while the highest yield of γ-LiAlO 2 phase was obtained in the n -butyl sample.

Surface properties of bioactive TEOS–PDMS–TiO2–CaO ormosils

Tetraethyl orthosilicate (TEOS)–polydimethyl siloxane (PDMS) ormosils with different amounts of Ti and Ca were prepared and characterized. Several surface properties such as specific surface area, porosity, fractality, dispersive and polar surface energies were determined and related with their in-vitro bioactivity. It has been found a dependence of the surface fractal dimension with the concentration of Ca2+ ions that induce the appearance of rough surfaces. The dispersive surface energy, γSd, increased with the incorporation of Ti or Ca and the presence of micropores, but Ca(NO3)2 precipitates in the surface coming from non-incorporated Ca lead to a decrease of the surface energy values. In relation with the polar surface energy, it has been observed that all ormosil materials presented amphoteric character with a larger presence of base surface sites than acid ones. The basicity of the surface increased with the concentration of Ti and Ca, while the acidity decreased. The in-vitro bioactivity of the surface was estimated by soaking samples in simulated body fluid (SBF) and afterwards characterized by means of X-ray diffraction (TF-XRD) and field emission scanning electron microscopy (FE-SEM). It has been observed that in vitro bioactivity is related with the polar surface characteristics of these materials, being necessary for the bioactivity, the presence of a highly polar surface with intermediate base/acid ratio and specific roughness.