The activation of inert C–H bonds under mild conditions with high selectivity remains a central challenge in catalysis. Metal–organic frameworks (MOFs) and polyoxometalate-based MOFs (POMOFs) offer atomically precise, tunable structures that integrate light absorption, charge separation, and catalytic sites. This review systematically summarizes recent progress in the development of MOFs/POMOFs for light-mediated C–H bond activation over the past decade. We discuss design strategies for active sites, including metal nodes, functionalized ligands, guest encapsulation, defect engineering, and single-site regulation. The synergistic role of POMs as electron sponges in promoting charge separation and modulating reactive oxygen species (·O₂⁻, ¹O₂, and ·OH) pathways is discussed. Structure–activity relationships governing the activation of aromatic, benzylic, allylic, and aliphatic C–H bonds are discussed. Finally, perspectives on operando characterization, precision synthesis, green manufacturing, and AI-assisted design are provided to guide the development of next-generation photocatalysts.

Gadolinium gallium garnet (GGG) polycrystalline powders doped with Nd,Yb were prepared by coprecipitation method. The structure, phase and properties of powders were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDS) and fluorescence spectroscopy. XRD analysis indicated that the crystallization of Nd,Yb:GGG powders occur at 900 ℃. SEM analysis showed that the morphology of the powders was irregular and the average radius is 68.74 nm. FTIR analysis manifested that pure Nd,Yb:GGG powders were formed at 900 ℃. The fluorescence spectrum revealed that the most strong emission of Nd,Yb:GGG powders was 1030 nm, which was attributed to ²F_5/2→²F_7/2 of Yb³⁺. The possible formation mechanism of Nd,Yb:GGG powders were preliminarily discussed.