Abstract The synthesis and characterization of organic–inorganic mesoporous luminescent hybrid materials were presented. The hybrid materials were obtained by linking the binary and ternary Tb 3+ complexes to the functionalized ordered mesoporous SBA-15 with modified acetylacetone (ACAC-Si), and the synthesis was achieved via co-condensation of tetraethoxysilane (TEOS) in the presence of Pluronic P123 surfactant as a template. The precursor for the preparation of mesoporous materials was synthesized by grafting acetylacetone (ACAC) to the coupling agent 3-(triethoxysilyl)-propyl isocyanate (TEPIC). The mesoporous material covalently bonded Tb 3+ complex (denoted as Tb(ACAC-SBA-15) 3phen) exhibits the stronger characteristic emission of Tb 3+ due to the triplet state energy of organic ligand ACAC-Si matches with the emissive energy level of Tb 3+ very well. This material was obtained by introducing Tb(NO 3) 3 and 1,10-phenanthroline (phen) complex into the hybrid material via a ligand exchange reaction. The luminescence properties of the resulting material (denoted as Tb (ACAC-SBA-15) 3phen) were characterized in detail, and the results reveal that luminescent mesoporous materials have high surface area, uniformity in the mesopore structure and good crystallinity.