The effect of coagulation bath condition on the structure and property of the nascent fibers and polyacrylonitrile fibers during wet-spinning is studied. The best coagulation condition to produce polyacrylonitrile fibers has been found by examination of EA, XRD, SEM, and so on. The results indicated that when the coagulation bath was DMSO/H 2 O system, the temperature was 608C, the concentration was 65%, the minus stretch ratio was À10%, fine crystallites and high degree of crystallization in the nascent fibers and polyacrylonitrile fibers could be achieved, and less solvents remained in the nascent fibers with circular cross section morphology.