Poly (9,9-dialkylfluorene-2.7-diyl)s were synthesized by nickel (0) mediated polymerization. This polymerilntion yielilt tl high molecular weight and thermally stable polymers. To study the structure-property relationship of excimer formation in the polymer films. absorption and fluorescence spectra were measured before and after,annealing at elevated temperature. The annealed films showed 3 longer wavelength emission band corresponding to excimer formation in the homopolymers.