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A series of different molecular weight amphiphilic diblock copolymer poly(ethylene glycol)-block-poly(ε-caprolactone) (PEO-b-PCL) were prepared as soft templates for synthesis of mesoporous silica through evaporation induced self-assembly (EISA) approach.The different feed ratios by changing the length ratio of the two blocks in those block copolymers were characterized by gel permeation chromatography (GPC) and nuclear magnetic resonance spectroscopy (NMR) measurements.The mesoporous silica with different large pores ca.15~25 nm was obtained through transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS) analyses and the self-assembly of mesophases was transformed from lamellae of pure diblock copolymer to hexagonal packed cylinder with the increase of HCl or TEOS contents.