Characterizing Dispersion and Fragmentation of Fractal, Pyrogenic Silica Nanoagglomerates by Small-Angle X-ray Scattering

Typical characterization of nanoparticle dispersion and compounding processes by dynamic light scattering (DLS) and TEM lack quantitative information on fractal structure, aggregation number, and specific surface area. In this work a synchrotron ultra-small-angle X-ray scattering (USAXS) investigation on diffusion flame and ‘Aerosil' silica powders, as well as on their desagglomeration by high-pressure liquid dispersion (200−1400 bar) is presented. Primary particle size, polydispersity, and specific surface area are measured for powders, stirred-in dispersions, and after high-pressure processing with identical results, showing the in-situ applicability of USAXS. These parameters, as well as the hard aggregate mass fractal dimension, with typically D_f = 2.15 representing reaction-limited cluster aggregation, are determined by synthesis process conditions. They are unchanged even at the highest hydrodynamic stresses; thus, neither comminution nor agglomerate restructuring nor re-agglomeration occurs. Fragmentation reflects in decreasing radii of gyration, which are compared to mobility equivalent radii from DLS in agreement with theory.