The effect of the deaeration process on the behavior of acrylonitrile-acrylamide copolymer solutions was demonstrated experimentally in detail. The corresponding mechanical properties and morphology of the resultant precursors were also been examined. It was found that the viscosity of the copolymer solutions at rest increased continuously with the deaeration time prolonged at every fixed temperature stage, but it considerably increased when the deaeration temperature decreased. The changes in the viscosity of the solutions at 808C were less prominent than those of the solutions at 208C in the beginning stage; beyond 60 min, the changes became remarkable. In concentrated copolymer solutions, the dimethyl sulfoxide composition weight percentage decreased with an increase in the deaeration temperature; the increasing temperature reduced the solvent power continuously at a high deaeration temperature, so more solid-elastic gels were formed in the solutions with an increase in time. At the same degree of vacuum, when the temperature varied from 20 to 808C and, in particular, the deaeration temperature was beyond 608C, the products from the copolymer seemed to have slightly narrower molecular weight distributions. With the deaeration temperature increasing, the tensile strength, elongation at break, and bulk density of the resultant precursors increased, but their fineness and coefficient of variation decreased. The morphology of the precursors was more compact and more round beyond 608C than below 608C.