Polyamide 66 (PA 66) nanofibers, with the mean diameter of about 140 nm, were prepared by electrospinning. Nano-hybrid shish-kebab (NHSK) structure was achieved in PA 66 nanofibers/isotactic polypropylene (iPP) composites via isothermal solution crystallization. The morphology of such NHSK was observed by scanning electron microscopy (SEM). It was found that PA 66 nanofibers act as "shish", and iPP crystals serve as "kebabs". Furthermore, the concentration of iPP solution remarkably affects the morphology of the NHSK, i.e., the size of iPP crystals becomes much bigger with the increasing iPP solutions' concentration. The reason for this can be explained as that the high concentration of iPP solutions contain more free chains which can participate into the process of crystallization. (C) 2010 Elsevier B.V. All rights reserved.