Poly(9,9-dipropargylfluorenylene-biphenylene) was prepared by cross-coupling condensation of 9,9-dipropargylfluorene and 4,4 '-diiodobiphenyl in high yield. The polymer structure was identified by various spectroscopic methods such as IR, (1)H-, (13)C NMR, UV-visible spectroscopies. The acetylenic units in the polymer main chain were found to be thermally crosslinked in the range of 167-278 degrees C. The photoluminescence peak of the polymer is located 396nm which corresponds to a photon energy of 3.13eV.