Synthesis of volatile Eu(acac)3phen and Tb(acac)3phen complexes by solution technique were reported in this paper. The combination of Eu and Tb complexes, namely TbxEu(1-x)(acac)3phen (x=0.1,0.3,0.5,0.7,0.9) were also synthesized by maintaining stoichiometric ratio. Optical properties of these synthesized complexes were studied using photoluminescence technique. Eu(acac)3phen exhibits red intense emission at 612 nm with a sharp spectral bandwidth 5 nm when excited at a wavelength of 323nm, while Tb(acac)3 phen shows green emission at 547 nm when excited at 347nm. The emission spectra of TbxEu(1-x)(acac)3phen reveals that Tb0.7Eu0.3(acac)3 phen complex exhibits maximum intensity among all the stichiometrically doped complexes. When Tb0.7Eu0.3(acac)3 phen was molecularly doped in poly methyl Metacrylate (PMMA) to check its compatibility in polymers, enhancement in intensity was observed in these blended films, proving that these complexes can be used as emissive materials for fabricating OLEDs and displays by vacuum deposition as well as solution techniques.