A novel series of poly(aryl ether sulfone ketone)s (PPESKs) containing phthalazinone and biphenyl moieties were prepared by two-step nucleophilic polycondensation reaction. The Mˉw values of these copolymers were between 38,330 and 67,900. The glass transition temperatures (Tg) and 5% decomposition temperatures were ranged in 253-269 8C and 488-500 8C, respectively, The structures of these copolymers were confirmed by FT-IR and 1H NMR. Moreover, all the resultant copolymers were amorphous determined by wide angle X-ray diffraction (WAXD). A novel series of poly (aryl ether sulfone ketone) s (PPESKs) containing phthalazinone and biphenyl moieties were prepared by two-step nucleophilic polycondensation reaction. The Mˉw values ​​of these copolymers were between 38,330 and 67,900. The glass transition temperatures (Tg) and 5% fractionation were ranged in 253-269 8C and 488-500 8C, respectively, The structures of these charts were confirmed by FT-IR and 1H NMR. Moreover, all the resultant ACs were determined by wide angle X-ray diffraction (WAXD).