In this study we found that complicated mesostructures featuring bimodal mesopore distributions could be fabricated through simple evaporation-induced self-assembly when employing lab-made poly(ethylene-b-ethylene oxide-b-ε-caprolactone) (PE-PEO-PCL) triblock copolymers as single templates without any other additives. Using this approach, we produced two kinds of ultra-complicated hierarchical mesoporous silica samples as a result of the unusual composition of the ABC-type triblock copolymer: hydrophobic segments at the termini and a hydrophilic segment in the middle. Notably, by adjusting the amount of tetraethyl orthosilicate (TEOS) in the reaction medium, we obtained a series of silica samples with well-defined morphologies and two types of well-ordered hierarchical mesostructures, namely “alternate body-centered cubic” and “tetragonal cylinder alternated with face-centered cubic.” Using small-angle X-ray spectroscopy, transmission electron microscopy, and isothermal N2 adsorption–desorption experiments, we studied the phase behavior of the mesoporous silica samples templated by a series of PE-PEO-PCL triblock copolymers at various TEOS-to-PE-PEO-PCL-to-HCl weight ratios. Notably, we report the first example of the fabrication and characterization of the special “alternate body-centered cubic” mesostructure (E1T40).
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