Aqueous Sol−Gel Process in the Silica−Metasilicate System. A Microrheological Study

Abstract

The electrochemical quartz crystal microbalance (EQCM) was used to investigate the sol-gel process from an aqueous sodium metasilicate solution at 25°C and pH 3. From the EQCM data it was possible to obtain information on the changing rheological properties of the system during the whole process. Besides sensing changes in the rheological properties, the EQCM detected film formation on the sensor surface. This additional information was used to estimate, using a model for film formation kinetics, the sol particle size (the model prediction was confirmed by light scattering measurements). The particle size estimation was of importance in the analysis of the sol viscosity behavior during the earlier stages of the particle aggregation process. The analysis, based on a classical model for the viscosity of a dispersion of charged particles in an electrolyte, provided some insight into the initial aggregation phenomena and microgel formation. Determination of the gelling point was made by examining the evolution of the shear storage modulus of the system. The gelation point was identified as being the time at which the storage modulus rose abruptly from zero. The rheological behavior of the system beyond the gelation point was analyzed in terms of the loss tangent, which value decreased noticeably before becoming constant. The observed decrease in the loss tangent, as a measure of the increasing importance of the elastic energy storage relative to the energy dissipation in the gel, was evidence that Si-O-Si bond formation continued to take place for some time after the sol-gel transition.

Physical Properties of Water Near a Gold Surface: A Nanorheological Analysis

“…Case (c): If the solutes cause only thin rigid film formation on the electrode contacting the semi-infinite medium, the resonant frequency will change according to Equation (2) without resistance changes [Eqs. (19) and (20)]: [18] D DR ð Þ ¼ 0 ð19Þ…”

Electrochemical and Spectroscopic Characterization of Surface Sol−Gel Processes

“…Dunn et al introduced alternating current impedance spectroscopy for studies of the evolution of the sol−gel process and gel aging. In addition, Tenan et al applied an electrochemical quartz crystal microbalance to the study of silica gelation from an aqueous silica sol prepared by the hydrolysis of the metasilicate ion . Our study concentrates on characterization of the MTS sol−gel process on platinum substrates by use of gold nanoparticles as markers.…”

Detecting sol–gel transition using light transmission

“…Anglaret et al determined gelation by visually inspecting solution flow properties in a tilted container [7]. Tenan et al used an electrochemical quartz crystal microbalance (EQCM) to monitor the oscillation of a quartz crystal submerged in solution as the solution gels [8]. They showed that EQCM could effectively measure rheological properties using only small-scale perturbations.…”