Nanoporous silica spherical particles with narrow particle size distributions (standard deviation: 0.03-0.22) were synthesized by the Stöber method combined with supramolecular templating approach using tetraethoxysilane and cetyltrimethylammonium chloride. The reaction was conducted at 276 K to observe particle growth. Particles formed after the reaction for ca. 0.5 h, as shown by the fact that the solution became turbid. After the reaction for 0.5 h, particles with an average particle size of 440 nm in diameter were collected by filtration. The particles grew until the silica source was completely consumed. This took 50 h under the present reaction condition. The average particle size reached to ca. 1.8 mm at this stage. The calcined particles were porous with the surface areas of 380-1060 m 2 g À1 and the pore diameter of 1.6-2.0 nm. Mesoporous silicas prepared by supramolecular templating approach have been investigated as adsorbents, catalysts, and nano-reactors owing to their large surface area, pore size uniformity, and possible surface engineering. 1-4 The morphology of mesoporous silicas is an important issue for their practical applications, 5 so that the syntheses of mesoporous silicas in such morphology as coating films, 6,7 self-standing films, 8-11 monoliths, 12,13 fibers, 14,15 hollow spheres, 15-25 and dense spheres 26-50 have been reported.Mesoporous silica spherical particles with controlled size and size distribution are attractive materials for such uses as optics and chromatography. 50 Accordingly, the preparation of mesoporous silica spherical particles has been reported so far 26-50 utilizing various synthetic approaches including those based on emulsion chemistry 47 and using morphology template. 48 The Stöber method, which was developed for the preparation of silica spherical particles with controlled particle size, 51,52 was also employed to prepare surfactant templated mesoporous silica spherical particles. [26][27][28][29][30][31][32][33][34][35] The preparation of the mesoporous silica particles with the particle size of 60-2300 nm have been reported so far. [26][27][28][29][30][31][32][33][34][35] However, because there are many factors, such as chemical composition and synthetic temperature, which affect the particle sizes, the relationships between the synthetic condition and the particle size are not fully understood. In addition, the particle size of the reported spherical particles 26-35 was ca. 2 nm.So further study on the preparation of nanoporous silica spherical particles with different size and pore geometry is worth investigating. In the present study, we prepared surfactant-silica spherical particles at a low temperature (276 K) in order to follow their growth and to investigate the particle size and nanostructures of the products.
Experimental
Materials.Tetraethoxysilane (abbreviated as TEOS) and cetyltrimethylammonium chloride (abbreviated as CTAC) were obtained from Tokyo Kasei Kogyo Co., Ltd. and were used without further purification. Sodium hydroxide, methanol and 2...