Highly ordered mesoporous carbons and silicas with ultralarge accessible pores have beensuccessfully synthesized by using laboratory-made poly(ethylene oxide)-
b-polystyrene (PEO-
b-PS) diblockcopolymers as templates via the evaporation-induced self-assembly (EISA) approach. Resols and tetraethylorthosilicate (TEOS) serve as carbon and silica precursors, respectively. Small-angle X-ray scattering (SAXS)and transmission electron microscopy (TEM) measurements show that the mesoporous carbons (denotedas C-FDU-18) possess face centered cubic closed-packing (
fcc) mesostructure (
Fmm) with large-domainordering. N
2 sorption isotherms reveal a large mesopore at the mean value of 22.6 nm with a narrowpore-size distribution. Mesoporous silicas (Si-FDU-18) also display a highly ordered
fcc closed-packingmesostructure with an ultralarge unit cell (
a = 54.6 nm). A hydrothermal recrystallization was introducedfor the first time to produce micropores in thick silica walls (~7.7 nm) and thus to generate ultralargeaccessible mesopores (30.8 nm). Notably, the amphiphilic diblock copolymer with high molecular weight(PEO
125-PS
230, 29700 g mol
-1) in this report was prepared via a simple method of atom transfer radicalpolymerization (ATRP). It can be easily available for chemists even without any experience in polymersynthesis.