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Herein, β-NaGd0.95Eu0.05F4@NaGdF4 core@shell nanoparticles were synthesized by thermal decomposition of lanthanide acetate precursors[2] to investigate the influence of the synthetic method on their structural and luminescence properties. Transmission electron microscopy reveals highly crystalline, spherical nanoparticles, with the average diameter increasing from 13±2 nm to 26±3 nm after shell growth, confirming successful coating. Photoluminescence properties were investigated by excitation and emission spectroscopy. The excitation spectra monitored at 612 nm show characteristic EuIII f-f transitions as well as a GdIII -related band at 271 nm (8S7/2→6IJ), indicating GdIII→EuIII energy transfer. Under 271 nm excitation, the typical EuIII 5D0→7FJ (J = 0–4) emission lines are observed. Notably, the comparable intensity of the 5D0→7F2 and 5D0→7F1 bands suggests EuIII sites with relatively high local symmetry. In addition, a broad emission band centered at 491 nm is attributed to defect-related states in the NaGdF4 lattice.
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