Template-in-template assembly nanostructured microspheres for high performance chromatography

Abstract Concurrent precision architecture of morphology and nanostructure in mesoporous microspheres is pivotal for high performance separations. Herein, we develop a template-in-template assembly nanostructuring (TiTAN) strategy to precisely synthesize monodisperse microspheres with ordered mesoporous nanostructure. Microfluidic droplet templating ensures uniform particle morphology (CV = 3%), while structure-directing agents within droplets enable tailored pore configurations, including 2D hexagonal, body-centered cubic, face-centered cubic, and cubic double gyroidal mesostructures. Through regulating hydrothermal conditions, structural parameters can be fined-tuned with 2 Å spatial resolution. By extending this manufacturing capability to a variety of material chemistries, chromatographic materials can now be de novo architectured with rationales, with the performance demonstrated by the solution of a classical separation challenge: resolving critical pairs (whose selectivity, α, infinitely approaching to 1), and with the shortest possible time. Beyond separation medium, the TiTAN strategy also suggests a route towards general synthesis of porous material with precision macroscopic morphology and microscopic nanostructure.