By using the interaction between the sulfonated groups and silver ions, nanosilver particles were successfully introduced into S-PEEK nanostructures (nanospheres and nanofibers) by electrospinning. The nanoparticles were characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectra (XPS), UV/vis, etc. The size of the spheres increases with the weight concentration of silver exchanged sulfonated poly(ether ether ketone) (S-PEEK-Ag) increasing. The size of the silver particles can be controlled by adjusting the sulfonated degree (number of sulfonate groups per repeating unit) of sulfonated poly(ether ether ketone) (S-PEEK) and the weight ratio of the S-PEEK solutions. This paper provides a new method for the preparation of nanometal particles into nanostructures. (c) 2006 Elsevier B.V. All rights reserved.