The synthesis of hierarchical or nanosized metal‐organic framework (MOF) superstructures is highly desirable. However, the development of synthetic methods for designed MOF structures via mechanochemical reaction remains extremely limited. We discovered the eco‐friendly and fast strategy that mechanochemical reaction of FeCl3·6H2O and sodium fumarate resulted in Fe‐MIL‐88A MOF hierarchical superstructures. The resulting MOFs possesses a higher surface area than conventional MIL‐88A. The key finding is that the types of the medium during mechanochemical reaction influence on the morphology of MIL‐88A MOFs, generating 3D superstructure and 1D nanorod. We believe that the synthetic strategy adopted opens the door for the modulation of MOF morphologies under mechanochemical condition.

Ag/AgCl nanoparticles embedded in defective porous titanium dioxide (Ag/AgCl-pTiO2) have been successfully prepared via the solvent-free sol-gel process, and their role as visible-light-responsive photocatalysts was investigated. The crystal phase, morphology,...