The effect of physical aging of the partially miscible blend of polycarbonate: polystyrene (PC:PS) at temperatures near the glass transition temperature (T g ) of the PS was studied as a function of time. For this purpose, blends of PC and PS with different ratios were elaborated and characterized using SEM, FTIR, DSC, and DMA techniques. The results indicated the presence of weak interaction upon blending with a maximum of interaction for the 50:50 blend. The effect of physical aging on the latter was then investigated via DMA, DSC, and NMR analyses. The DMA results showed that both phases were sensitive to aging. The effect was found to be strongly dependent on both the temperature and time. The aging of PC:PS blend was also found to trap stress during the process which induced an instability in the viscoelastic behavior. The latter was found to be associated with a phase-separation morphology of the blend and influenced by its composition. The NMR analysis also showed a pronounced distortion of the conformation combined with increasing molecular motion. These effects were found to be important for aging below the PS's T g .