Two-dimensional (2-D) materials are the significantly preferred candidates for developing new optoelectronic and electronic devices due to their superlative properties and active sites which promote 2-D materials in various applications such as sensing, photodetectors, batteries, supercapacitors, thermoelectric, photocatalysis etc. 2-D materials include transition metal oxides (TMOs), transition metal dichalcogenides (TMDCs), 2-D graphene, black phosphorus, carbide, nitride-based 2-D materials. The exceptional properties of 2-D materials such as their tunable atomic thickness, larger surface-to-volume ratio, excellent electron mobility, high light absorption capacity, and their tunable bandgap in the photonic range from UV (∼390 nm) to visible light (∼480 nm) which is an extremely critical requirement in the current energy crisis scenario. The controllable synthesis of high-quality 2-D materials is the first critical step for their efficient application as their structure morphology, chemistry, thickness, surface area, and creation of defects directly controls their overall properties. This chapter summarizes two feasible approaches along with their advantages and disadvantages for the synthesis of 2-D materials, namely, the top-down strategy and bottom-up strategies. It also summarizes the specific characterization techniques to study, and understand the structural, morphological, chemical, and physical properties of the synthesized 2-D materials.