Highly ordered ethylene bridged periodic mesoporous organosilica (PMO) materials with ultra-largepore sizes up to 14.7 nm were successfully synthesized by using triblock copolymer F127 as a templateand 1,3,5-trimethylbenzene (TMB) as a swelling agent. SAXS and TEM measurements show that PMOproducts have a face-centered cubic (space group of
Fm
m) mesostructure. The influence of reactiontemperature and acidity of the solution on the mesostructure of the PMO products were systematicallystudied. The pore size can be gradually expanded as the temperature decreases, and ordered PMOs canbe obtained at a temperature even down to 5
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C with a relatively low acidity. As compared with mesoporoussilica materials synthesized at identical conditions, our experimental results reveal that differenthydrophobicity between precursors, bis(trimethoxysilyl)ethane and tetraethyl orthosilicate, may influencethe swelling capacity of F127 micelles with TMB as well as the phase behavior of triblock copolymerF127, resulting in the different physicochemical properties of the final products.