2,2-Bis [4-((4-fluorophenyl)buta-1,3-diynyl)phenyloxyphenyl] hexafluoropropane and co-polymer of 1,4-bis(4-fluoropheny)buta-1,3-diyne and hexafluorobisphenol-A were prepared for the use as photosensitive multilayered polymeric dielectric insulators. The prepared materials turned out to be stable at high temperatures as well as thermally or photochemically curable. It was found that the mechanical properties of cross-linked products by thermal or photochemical curing of the prepared diacetylenic materials were much more improved in comparison with those of cured poly(triethynylbenzene)(PTEB).