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Amorphous metal–organic frameworks (aMOFs) and phosphate-based glasses are promising materials for developing hybrid luminescent composites. In this work, three amorphous MOFs (Zr/Eu-BTC, Zr/Tb-BTC and Zr/Eu/Tb-BTC) were synthesized and investigated alongside a low-Tg fluorophosphoniobate glass host. Comprehensive structural, thermal, and optical characterizations were performed. Excitation spectra of the co-doped aMOF confirmed an efficient Tb3+-to-Eu3+ energy transfer via a band at 488 nm. However, the most intense excitation occurred at 297 nm (π→π* ligant transition), demonstrating a highly efficient antenna effect that sensitizes both lanthanide ions. By exciting into this ligand band, the emission profiles can be modulated by adjusting the Eu3+/Tb3+ ratio. These amorphous frameworks are currently being investigated for ratiometric thermometry and white-light-emitting applications.
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