Hierarchically porous phenolic resin-based carbons obtained by block copolymer-colloidal silica templating and post-synthesis activation with carbon dioxide and water vapor

A series of hierarchically porous carbons was synthesized by self-assembly of polymeric carbon precursors and block copolymer template in the presence of tetraethyl orthosilicate (TEOS) and colloidal silica under acidic conditions. Resorcinol and formaldehyde were used as carbon precursors, poly(ethylene oxide)–poly(propylene oxide)–poly(ethylene oxide) triblock copolymer was employed as a soft template, and TEOS-generated silica and colloidal silica were used as hard templates. The carbon precursors were polymerized in hydrophilic domains of block copolymer, followed by carbonization and silica dissolution. This resulted in carbons possessing cylindrical (∼12 nm) and spherical (20 or 50 nm) mesopores created by thermal decomposition of the soft template and by the dissolution of colloidal silica, respectively; fine pores were also formed by the dissolution of the TEOS-generated silica (∼2 nm). A further increase in fine porosity was achieved by post-synthesis activation of the carbons with carbon dioxide and/or water vapor, which resulted in hierarchical carbons with a surface area and pore volume approaching 2800 m2/g and 6.0 cm3/g, respectively.

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► Combination of block copolymer and colloidal silica templating (BC-CS-T) is an effective way for the synthesis of phenolic resin-based carbons with multimodal distribution of uniform mesopores.
► Tetraethyl orthosilicate-assisted BC-CS-T synthesis combined with post-synthesis CO2 activation creates micro-mesoporous carbons with hierarchical structures.
► Hierarchically porous carbons with the surface area and pore volume approaching respectively 2800 m2/g and 6 cm3/g are reported.