Using poly(vinylpyrrolidone) (PVP) as a stabilizing agent graphite nanosheets (GNs) and molybdenum disulfide nanosheets (MNs) were conveniently obtained under ultrasound treatment. The two kinds of obtained nanosheets were detected by transmission electron microscopy (TEM) and atomic force microscopy (AFM) and analyzed by Raman spectroscopy. UV-vis spectrophotometric measurement was performed to test their typical absorption peaks.