Luminescence nanocomposites based on barium titanate nanoparticles (BaTiO3), polystyrene (PSt), and terbium ion (Tb3+) were synthesized by using a combination of reversible addition fragmentation chain transfer polymerization, Friedel-Crafts alkylation reaction and coordination chemistry. The modification of the surface of BaTiO3 was conducted by an exchange process with S-benzyl S-trimethoxysilylpropyltrithiocarbonate to anchor macro-initiators for the polymerization of styrene. Subsequently, PSt grafted barium titanate was functionalized by the substitution reaction between 4-(chloromethyl) benzoic acid and PSt to produce hybrids, BaTiO3-g-PSt -COOH. The coordination of the hybrids with Tb3+ ions in the presence of 1,10-phenanthroline (Phen) afforded fluorescent Tb3+ tagged carboxylic acid functionalized polystyrene/barium titanate (BaTiO3-g-PSt-Tb3+-Phen). FT-IR, XRD, TGA, and SEM analyses revealed the formation of BaTiO3-g-PSt-Tb3+-Phen hybrids. The optical properties of BaTiO-3-g-PSt-Tb3+-Phen were investigated by using fluorescence spectroscopy. © 2015 Taylor & Francis Group, LLC.