Two strongly fluorescent terbium-pyrazolone complexes, Dimethyldioctadecylammonium bis(1,6-bis(4-(1-phenyl-3-methyl-5-pyrazolone)hexanedionato)terbium(III)(Me2N(C18H37)(2) . Tb(BPMPHD)(2)) and tris(1-phenyl-3-methyl-4-hexadecanoyl-5-pyrazolone)terbium(III) ethanate Tb(PMHP)(3)(EtOH), were synthesized and characterized by Fourier transform infrared and UV-vis spectra, differential thermal analysis and thermogravimetric analysis, and X-ray diffraction. Both of them could form stable Langmuir films at the air/water interface, which are readily transferred onto hydrophilic substrates to build up good quality Langmuir-Blodgett (LB) films. Their LB films have good layered structure as confirmed by their low-angle X-ray diffractions. The fluorescence spectra and fluorescence lifetimes of the LB films are quite different compared with their corresponding solid powders and solutions.