Sol-gel processing of spirosilicates

The sol-gel transition of tetra-coordinated spirosilicate via hydrolysis and condensation under acidic and basic conditions is examined to elucidate the effect of catalyst, reaction time and temperature on the properties of obtained gel. The main advantage of this process is the low temperature employed, producing a solid network with a high specific surface area. FTIR spectroscopy and TGA analysis were used to characterize the formation of siloxane bonds (Si–O–Si). It is found that spirosilicate can be hydrolyzed under both acid and base catalyzed conditions. The condensation rate to silicates is shown to be at a minimum in 0.001M HCl, which is the iso-electric point of silica. The prepared xerogel has a low-density and is an amorphous material with a specific surface area of 596 m2/g. Besides the catalyst media, the type of precursor also has a strong influence on the gel formation. An aminospirosilicate, six-membered ring, containing methyl and amino groups as substituents, was chosen for this study. The resulting xerogel is determined by the fact that to obtain the Si–O–Si bonds, a higher concentration of solvent and higher temperature are more favorable, due to the length and branching of alkyl portion.