In Situ Probing of the Particle‐Mediated Mechanism of WO₃‐Networked Structures Grown inside Confined Mesoporous Channels

Abstract Nanocasting, using ordered mesoporous silica or carbon as a hard template, has enormous potential for preparing novel mesoporous materials with new structures and compositions. Although a variety of mesoporous materials have been synthesized in recent years, the growth mechanism of nanostructures in a confined space, such as mesoporous channels, is not well understood, which hampers the controlled synthesis and further application of mesoporous materials. Here, the nucleation and growth of WO₃‐networked mesostructures within an ordered mesoporous matrix, using an in situ transmission electron microscopy heating technique and in situ synchrotron small‐angle X‐ray scattering spectroscopy, are probed. It is found that the formation of WO₃ mesostructures involves a particle‐mediated transformation and coalescence mechanism. The liquid‐like particle‐mediated aggregation and mesoscale transformation process can occur in ≈10 nm confined mesoporous channels, which is completely unexpected. The detailed mechanistic study will be of great help for experimental design and to exploit a variety of mesoporous materials for diverse applications, such as catalysis, absorption, separation, energy storage, biomedicine, and nanooptics.