Ordered Mesoporous Carbon Featuring Single‐Crystal Morphology and Tunable Pore Architectures via EtOH‐Mediated Micelle Assembly

Abstract The precise control of reaction kinetics and the synchronous regulation of the micelle assembly in the soft‐templating method for synthesizing ordered mesoporous carbon presents a significant challenge. In this study, a versatile ethanol‐mediated self‐assembly strategy is introduced to synthesize ordered mesoporous carbons (OMCs) with diverse morphologies and well‐defined mesostructures using liquefied wood (LW). Ethanol functions as both a proton‐trapping agent and a linker between carbon precursors and templates, enabling fine‐tuned regulation of the self‐assembly kinetics while providing additional hydrogen bonding interactions. Furthermore, the micelle structure can be precisely manipulated from cylindrical to spherical through ethanol‐induced selective swelling of hydrophilic blocks, resulting in a reduction in packing parameter ( p) from 1/3 < ( p) < 1/2 to ( p) ≤ 1/3. Notably, the spherical composite micelles self‐assemble into single crystals with highly ordered body‐centered mesostructures. The fabricated ordered mesoporous carbon single crystal (OMCSC) electrochemical sensing polymers exhibit absolute enantiomeric discrimination for L‐ and D‐tryptophan. This EtOH‐mediated self‐assembly approach not only elucidates the role of ethanol in the self‐assembly process but also offers a promising pathway for fabricating versatile OMCs from renewable biomass resources.