AgI nanoparticles/beta-cyclodextrin (beta-CD)/polyacrylonitrile (PAN) composite nanofibers film were prepared via a new route which combined electrospinning technology with the reaction of solid-liquid process. In this article, AgI nanoparticles were successfully prepared in beta-CD/PAN nanofibers which contained different concentration beta-CD by the new route. Firstly, the AgNO3-beta-CD/PAN nanofibers were obtained via electrospinning method, then put the nanofibers into the solution of potassium iodide to prepare AgI-beta-CD/PAN nanofibers. The morphology and structure of the composite nanofibers and nanoparticles have been investigated by scanning electron microscopy (SEM) and transmission electro microscopy (TEM). The existence of the AgI nanoparticles was proved by X-ray photoelectron spectroscopy (XPS) and X-ray diffractometer (XRD) patterns. The results of various characterizations indicated that the sample of AgI-beta-CD (2 wt%)/PAN have the optimum morphology and structure. (C) 2013 Elsevier B.V. All rights reserved.