In this study, high intensity ultrasound was employed to induce mechano-chemical degradation during melt mixing of polycarbonate (PC) and a series of styrene-acrylonitrile (SAN) copolymers. It was confirmed that generation of macroradicals of constituent polymers can lead to in-situ copolymer formation by their mutual combination, which should be an efficient path to compatibilize immiscible polymer blends and stabilize their phase morphology in the absence of other chemical agents. Based on the effectiveness of the compatibilization by ultrasound assisted mixing process, we investigated the effects of viscosity ratio of PC and SAN and AN content in SAN on the compatibilization of PC/SAN blends. It was found that effectiveness of compatibilization is optimal when the AN content is in the range of favorable interaction with PC and the viscosity of the matrix is higher than that of the dispersed phase. In addition, changes in the interfacial tension between PC and SAN were assessed by examining relaxation spectra which were obtained from measuring rheological properties of ultrasonically treated blends.