Complexes Eu2L3L' and Tb2L3L' (L = 0-phthalate, L' = 2,2'-dipyridyl) have been synthesized. Mixed the both complexes as different molar ratio, mechanically ground them, then obtained a series mixed solid complexes of europium and terbium. Their fluoresence and infrared spectra were investigated. The results showed that there were obviously change for their fluorescence intensities and peak positions as compared with Eu2L3L' or Tb2L3L'. The fluorescence intensities of europium ions were sensitized by terbium ions and those of terbium ions were quenched by europium ions. FTIR spectra indicated that there were a combined force between the two complexes in the mixed solid complexes.