Infrared and thermogravimetric study of high pressure consolidation in alkoxide silica gel powders

TLDR: In this paper, high density, transparent, crack-free and hard compacts of silica gel were produced by compaction under nearly hydrostatic environment at 4.5 GPa, at room temperature.

Abstract: High density, transparent, crack-free and hard compacts of silica gel were produced by compaction under nearly hydrostatic environment at 4.5 GPa, at room temperature. The starting material was used three days after synthesis by hydrolysis of alkoxides without additional treatment. Fourier transform infrared spectroscopy (FTIR), using the KBr technique and a high vacuum cell at temperatures up to 450°C, and thermogravimetric analysis (TGA) up to 900°C was conducted. A reduction up to 60% in the adsorbed water content of the compacted silica gel was observed. Changes in the 3000 to 3800 cm−1 region indicate that the surface silanol groups became bridged, which promotes condensation reactions of dehydroxylation. Those results suggest that the mechanism for consolidation under high-pressure, is ‘cold sintering’ process, where silanol groups at the surface of the nanoparticles condense to form siloxane bonds between the particles and water, resulting in a stiff body with closed nanopores containing trapped water.