Synthesis of microporous silica spheres

R. Vacassy, R. J. Flatt, H. Hofmann, K. S. Choi, R. K. Singh

Research output: Contribution to journalArticlepeer-review

101 Scopus citations


Spherical microporous silica powders with a narrow size distribution have been prepared by a precipitation technique involving the hydrolysis reaction of a silicon alkoxide in ethanol. The formation of the important microporosity has been investigated following two templating methods: the co- hydrolysis and condensation of two alkoxides, one of which presents porogen function, and the adsorption of an organic compound (glycerol) as the porogen. In both processes, the organic porogen is removed by a simple calcination. In the first method, the addition of more than 20 mol% of the porogen alkoxide, necessary for generating enough microporosity, disturbs completely the condensation process resulting in microporous, nonuniform silica particles of large size distribution. The best result has been obtained with the glycerol method where submicrometersized silica spheres with a very narrow size distribution and about 40 vol% porosity have been synthesized. The presence of glycerol during the synthesis considerably affects the precipitation mechanism, resulting in a larger mean particle size. The use of an aggregative growth model has successfully been employed to explain the effect of the porogen during panicle formation. The precipitation mechanism of silica involves the aggregation between particles of similar size until a critical size is reached, resulting in a uniform particle size distribution. In the presence of glycerol, it has been shown that a second aggregative growth between still-nucleating primary particles and large particles occurred with increasing reaction time. This second aggregative growth appears at an intermediate stage of the precipitation process and is due to both the precipitation of smaller primary particles and the destabilization of the colloidal stability of the system. This explains why the final particle size reached in this system is larger compared to silica particles synthesized without glycerol and shows how glycerol is incorporated in the silica particles. The synthesis of silica microporous spheres of narrow size distribution, by varying particle size and porosity, should yield a wide range of aqueous silica slurries for particular chemical mechanical polishing applications. (C) 2000 Academic Press.

Original languageEnglish
Pages (from-to)302-315
Number of pages14
JournalJournal of Colloid and Interface Science
Issue number2
StatePublished - 15 Jul 2000
Externally publishedYes


  • Aggregative growth
  • Colloidal stability
  • Microporosity
  • Particles
  • Precipitation
  • Silica


Dive into the research topics of 'Synthesis of microporous silica spheres'. Together they form a unique fingerprint.

Cite this