In the presence of a high TMOS concentration, mono-dispersed mesoporous pure silica spheres with different pore sizes were successfully synthesized using C16TMACl, C14TMACl, and C12TMACl as templates in a methanol–water system, whereas they could not be obtained using C10TMACl. The standard deviation of the particle size prepared with high TMOS concentrations was approximately 10%. Mono-dispersed mesoporous Al-containing spheres could also be synthesized using NaAlO2 as an aluminum source from starting synthesis mixtures with a TMOS/Al ratio of more than 10, but not with a TMOS/Al ratio of less than 8. It was found that the particle size and standard deviation of mono-dispersed mesoporous aluminum-containing spheres depended on the TMOS/Al ratio.
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