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A new and facile approach has been developed to prepare monodisperse mesoporous silica nanospheres (MMSNs) with controlled particle sizes and pore structures. In our approach, MMSNs were synthesized simply in a sodium acetate solution without adding any other alkali or alcohol additives. MMSNs have a spherical shape and uniform particle sizes, which can be adjusted from 50 to 110nm by increasing the reaction temperature from 40 to 80°C. By performing a subsequent hydrothermal treatment (HT) under basic condition (pH=∼11.5) at 130°C, the mesoporous pore volume and surface area can be enhanced, while keeping the mono-dispersion characteristics and the mesopore size almost unchanged. The pore sizes of MMSNs can be adjusted from 2.8 to 4.0nm under acidic solutions by changing the HT temperature from 100 to 130°C. The formation process of MMSNs has been investigated by …