The production of polymer nanocomposites from solution consists of the mixing of the polymer and nanoparticle in solution and subsequent evaporation of the solvent. We examine the formation of polyacrylonitrile and C-60 fullerene nanocomposites, with a focus on monitoring these two steps. The results of this study indicate that the nanoparticles are individually dispersed with the polymer chains in solution prior to deposition and in the final film. As the solution becomes more concentrated, the nanoparticles are sequestered to the outer edges of the polymer crystals, altering the detected crystal structure. The self-assembled structure of the crystalline polymer is directed by the addition of C-60 and manifests itself as a peak in small-angle X-ray scattering on a length scale of similar to 150 angstrom. The results suggest that the non-covalent molecular interactions between C-60 and polyacrylonitrile matrix are sufficiently strong to alter the self-assembled morphology of the polymer and the meso-and nanoscale structures in the nanocomposite. (C) 2015 Elsevier Ltd. All rights reserved.