In recent years, two-dimensional (2D) atomically thin crystals ranging from insulator to superconductor such as graphene, hexagonal boron nitride (h-BN), transition metal dichalcogenides (TMDs), etc. have attracted extensive attention due to their exceptional properties and many potential applications in various areas. In this chapter we focus on the experimental characterization of 2D materials and their heterostructures andcover brief introduction and detailed structural, optical, and chemical characterizations of some important 2D materials. © 2020 Elsevier Inc.