Rheological characterization of BaTiO3 sol-gel transition

BaTiO3 gels were prepared by hydrolysis and polycondensation reactions between titanium isopropoxide and barium hydroxide in presence of methoxyethanol, methanol and water. The rheology of the sol-gel transition was studied with a rheometer allowing low amplitude sinusoidal oscillations. Experimental data show a continuous increase in the complex viscosity along with time, showing the progressive character of the transition. The influence of synthesis operating variables was studied. The gelation time, which definition is based on viscoelastic measurements, increases exponentially when the water content is increased, when the dilution due to the methoxyethanol is reduced or when the temperature is lowered. Different growth models were used for the characterization of the particles in the solution. These models suggest that the polymerisation first produces spherical particles (mass fractals) and that these spherical particles then agglomerate to form a linear network

SYNTHESIS OF SIO2-TIO2 XEROGELS BY SOL-GEL PROCESS

A new method to synthesize SiO2-TiO2 gels by sol-gel process has been developed. This technique uses tetraisopropylorthotitanate [Ti(O'Pr)(4)] and tetraethylorthosilicate [TEOS]: they are mixed in the same solvent and then directly hydrolysed. This one-step reaction is possible because of the use of 2-methoxyethanol, a protic polar solvent. This alcohol plays two different specific roles: it acts as a solvent as well as a stabilizer of titanium alkoxide towards the hydrolysis-precipitation reaction. So, by an accurate adjustment of the quantity of methoxyethanol in the mixture, we can control the reactivity of the titanium precursor. Monolithic and transparent xerogels were obtained whatever the composition. Three monolithic SiO2-TiO2 gels containing 20, 50 and 75 mol% of TiO2 were prepared and studied in details. By using the TG-DSC analysis, we can follow the evolution of the loss of water and organic residues. The structural evolution of gels during calcination is characterized by IR spectroscopy and X-Ray diffraction