A well-ordered hexagonal structure of the mesopores was produced by previous hydrolysis of tetraethoxysilane with hydrochloric acid and subsequent assembly of cationic surfactant micelles and anionic silicate species at a basic condition. Mesoporous silica nanoparticles (20-50 nm) having a well-ordered hexagonal mesostructure were produced using a mixture of cationic surfactant as a template and nonionic block copolymer as a suppressant of grain growth.

The grain size and regularity of the hexagonal array of mesoporous silica nanoparticles were investigated in a binary surfactant system composed of cetyltrimethylammonium chloride and triblock copolymer EO106PO60EO106. Structural control was achieved by varying the parameters for the prior hydrolysis of silicon alkoxide under an acidic condition and the subsequent assembly of silicates and surfactants under a basic condition. The formation of the mesoscale architectures was based on the balance between the ordered assembly of anionic silicates and the cationic surfactant through electrostatic interaction and the inhibition of grain growth with a nonionic amphiphilic agent through hydrogen bonds.

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The architecture of mesoporous silica was successfully controlled by adjusting the concentrations of a cationic surfactant and ammonia. An excess amount of the surfactant suppressed the grain growth and then induced the formation of small grains with a diameter below 20 nm. Consequently, assembly of the small-sized grains produced a bimodal pore structure consisting of framework mesopores of 2-3 nm and textural mesopores ranging over 10-100 nm.