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In this work, CoFe2O4 nanoparticles have been prepared by co-precipitation technique. The synthesized CoFe2O4 nanoparticles were applied in the preparation of CoFe2O4/Polyacrylonitrile fiber nanocomposites by the electrospinning process. The prepared nanoparticles and nanofibers were characterized using the Scanning Electron Microscopy (SEM) and X-ray diffraction methods. The results manifested that nanofibers of PAN and CoFe2O4 /PAN were successfully prepared with electrospinning method. Grayscale SEM images of nanofibers were analyzed by a new image analysis procedure for determination of fibers diameter, their diameter distribution and the compactness of electrospun nanofibers. It was found that the presence of CoFe2O4 nanoparticles in the PAN solution increases both of the compactness of electrospun nanofibers and their diameter. The prepared CoFe2O4/Polyacrylonitrile fiber nanocomposites have possible applications in fabrication of sensor and magnetic recording media.