NMR as a tool to characterize the aggregation structure of silica nanoparticles in a liquid†

Abstract

The NMR-based solvent relaxation technique, a non-invasive tool to characterize the surface of particles, which are dispersed in a liquid, was applied to characterize the nanoparticles’ aggregation structure. The liquid molecules in a dispersion undergo a rapid exchange between the bound states at the interface and highly mobile free states in a bulk liquid. The relaxation time of the liquid molecules bound on the particle surface is shorter than that of the free states liquid. By detecting how much liquid is bound on the particle surface, the wetted specific surface area (SNMR) can be determined. In this study, it was clarified that the water adsorbed at more than a 1.138 layer from the silica surface can be detected by the NMR and the maximum limitation ranged from 2.160 and 3.336 layers. The model aggregates with an artificial solid neck among the particles were mixed with the silica nanoparticle dispersion. Although the determined SNMR was underestimated compared to SBET from gas adsorption, even a low ratio (5 mass%) of the model aggregates in the dispersion can be detected.