Versatile Synthesis of Mesoporous Nanomaterials via Monomicelle‐Directed Assembly

Mesoporous nanomaterials have attracted significant attention due to their diverse compositions and multileveled architectures. The soft-templating strategy serves as a foundational methodology for synthesizing mesoporous materials, achieving structural modulation via manipulation of thermodynamic and kinetic pathways during the self-assembly. In particular, recent breakthroughs in monomicelle-directed assembly have enabled the precise engineering of the morphologies, nanostructures, and porous architectures. This approach relies on the formation of composite monomicelles composed of block copolymers/surfactants and precursor species, which act as structure-directed units. The assembly of composites monomicelles through a well-defined and controlled stacking process resulted in mesoporous nanomaterials. Crucially, the size, composition, and geometry of monomicelles can be readily tailored by optimizing the synthetic conditions, which enables precise control over the architectures inaccessible by conventional approaches. Here, we review the historical development and design principles of monomicelles, along with the synthetic chemistry involved in the assembly of monomicelles with precursors. Subsequently, monomicelle assembly via aggregate and interfacial assembly is highlighted to achieve the controllable synthesis of mesoporous nanomaterials for applications in catalysis (e.g., thermal, electro-, photo-catalysis) and energy storage (e.g., batteries and supercapacitors). Finally, current challenges and future opportunities are discussed to enhance the design of mesoporous materials for future applications.