Inorganic nanoparticles doped with optically active rare-earth ions and coated with organic ligands were synthesized in order to create fluorescent polymethyl methacrylate (PMMA) nanocomposites. Two different aromatic ligands (acetylsalicylic acid, ASA and 2-picolinic acid, PA) were utilized in order to functionalize the surface of Tb 3+ : LaF 3 nanocrystals. The selected aromatic ligand systems were characterized using infrared spectroscopy, thermal analysis, rheological measurements, and optical spectroscopy. Nanoparticles produced in situ with the PMMA contained on average 10 wt% loading of Tb 3+ : LaF 3 at a 6 : 1 La : Tb molar ratio and ∼7 wt% loading of 4 : 1 La : Tb molar ratio for the PA and ASA systems, respectively. Measured diameters ranged from 457±176 nm to 150 ± 105 nm which is indicative that agglomerates formed during the synthesis process. Both nanocomposites exhibited the characteristic Tb 3+ emission peaks upon direct ion excitation (350 nm) and ligand excitation (PA : 265 nm and ASA : 275 nm).