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Contribution to the Determination of Kinetic Parameters of the Sol-Gel Transformation by Rheological Measurements.

The system tetraethoxysilane(TEOS)-water-ethanol has been studied by rheological measurements. Different molar ratios of TEOS : water (1 : 4, 1 : 10, and 1 : 20) are studied at different temperatures (30, 40, and 50 degrees C). The dynamic viscosity (rotating mode) at a constant shear rate (100 s(-1)) and the elastic and viscous moduli (oscillating mode) at a constant frequency (1 Hz) are determined. The viscosity-time curves are evaluated by application of a nucleation and particle growth model. Good agreement between experiments and theory is observed. The model allows the determination of the complex rate constant of silica precipitation. The temperature-dependent measurements gave the possibility to determine the apparent energy of activation by common methods. The results are in agreement with data from the literature. The gel time defined as intersection point of elastic and plastic moduli and its dependence on temperature are evaluated by the Smoluchowski model. The energy of activation for the coagulation was determined and found to be in the correct order of magnitude. Copyright 2000 Academic Press.