Meso‐tetra (carbonyl phenyl) porphyrin palladium (denoted as Pd‐TCPP), a typical organometallic compound, was used as phosphor and entrapped in micelle‐hybridized supramolecular hydrogels. As a novel matrix material of phosphors, the hybrid system was comprised of two ordered structures: a supramolecular 3D network structure formed by the self‐assembly of the gelator and the micelles formed from a Gemini surfactant. The dual‐ordered structure of the system was verified by SEM, TEM and fluorescent optical microscopy. By contrast with corresponding mono‐ordered structure, the room temperature phosphorescence (RTP) of Pd‐TCPP was greatly enhanced by the dual‐ordered structure of the system. The enhancement mechanism of RTP was studied by hydrophobicity of the system, RTP quenching and disassembly of supramolecular aggregates. Enhanced RTP could be attributed to the efficient inhibition of the non‐radiative transition of Pd‐TCPP by dual‐ordered structures. Significantly, the RTP intensity of Pd‐TCPP can be adjusted by changing the concentration of Gemini surfactants. Furthermore, deoxygenation was not required in this hybrid system in comparison with corresponding mono‐component systems.
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