In situ compatibilization of immiscible blends of PEN and thermotropic LCP was achieved by the ultrasonically-aided extrusion process. Ultrasonically-treated PEN underwent degradation, leading to a decrease of its viscosity. Viscosity of LCP was unaffected by ultrasonic treatment. Because of reduced viscosity ratio of PEN to LCP at high amplitude of ultrasonic treatment, larger LCP domains were observed in molding of the blends. LCP acted as a nucleating agent, promoting higher crystallinity in PEN/LCP blends. Ultrasonically-induced copolymer formation was detected by MALDI-TOF mass spectrometry in the blends. Ultrasonic treatment of 90/10 PEN/LCP blends improved interfacial adhesion in fibers spun at intermediate draw down ratios (DDR), improving their ductility. The lack of improvement in the mechanical properties of fibers spun at high DDR after ultrasonic treatment was attributed to the disturbance of interfacial copolymer by high elongation stresses. (c) 2011 Wiley Periodicals, Inc. J Appl Polym Sci 122: 354-365, 2011