Silica nanostructured spheres were obtained by spray drying of silica sol prepared in situ. Their morphologies were significantly affected by the aggregation of the primary particles in the sol. They had the mode of the pore sizes which was about the same order as Laser Particle Size Analyzer (LPA) diameter. Increasing the mixing ratio of the larger particles (20 nm) to smaller ones (7 nm) decreased the Brunauer, Emmett and Teller (BET) specific surface area, as expected. Pore volume decreased with the pore size distribution broadened and the mean pore diameter was not affected by the increase, due to the decrease in aggregation of the primary particles. Either the increase in the drying temperature and use of ethanol as a cosolvent made the agglomerates hollower, the larger of which with thinner shell transformed to doughnut type agglomerates, due to the structural and hydrodynamic instabilities.
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