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A simple and effective approach to prepare conductive polystyrene/carbon nanofiber (PS/CNF) nanocomposite films via a solution dispersion method is presented. Inexpensive CNF, which has a structure similar to multi-walled carbon nanotubes, is chosen as a nanofiller in this experiment to achieve conductivity in PS films. A good dispersion is achieved in the PS matrix with ultrasonication. The experiment to prepare PS/CNF system is suitable as a laboratory experiment for college chemistry or material science course. The experiment provides students with a hands-on laboratory experience in nanotechnology and its related fundamental concept.