In order to give students a better understanding of two-dimensional materials, a comprehensiveexperiment on the preparation and optical characterization of two-dimensional materials was designed.Severatypical two-dimensional materials were selected as the research objects in the experiment.Two-dimensionasamples were prepared by mechanical exfoliation method, and their basic lamellar morphology and stabilitywere explored by optical microscopy. The layer-dependent Raman optical properties of two-dimensional materials were studied by Raman spectroscopy. The integration of academie frontier and experimental teachinginereases the exploratory and innovative nature of experiments, which is conducive to improve studentsinnovative spirit and comprehensive practical ability.