Rapid development in Semiconductor research has brought excitement and challenges. New materials have pushed both academic and industry progress forward at a fast pace. Since the discovery of one-atomic layer of graphene in 2004, tremendous efforts have been devoted to pushing its properties to meet the technology demands, establish metrics and help accomplish milestones. The family of two-dimensional materials continue to expand. Transition metal dichalcogenides (TMDs) help compensate for the zero-bandgap of graphene and greatly increase the opportunities for their applications in electronics, optoelectronics, bioelectronics and medical-related applications. To enable electronic chips with higher density and faster processing/switching speeds and address technology bottlenecks, new correlated or functionalized two-dimensional materials are being positioned under the research spotlight. As one example, 1T phase tantalum disulfide (1T-TaS2) has presented a Mott state at around 180K, at which an abrupt change in its resistivity occurs. This unique property could help achieve two-dimensional Landau switch and realize ultra-low power, collective-state devices. However, large-scale synthesis of single crystalline monolayer of two-dimensional materials is still at its infancy. Fundamental questions as to the structural-property relationships of new materials or heterostructures await to be addressed. This dissertation focuses on the synthesis and characterizations of functional two-dimensional nanomaterials for beyond complementary metal oxide semiconductor industry. This dissertation starts with introducing the state of art of semiconductor industries and the progress of two-dimensional transition metal dichalcogenides (Chapter 1). It then addresses the two-dimensional materials synthesis methods and related characterization techniques (Chapter 2). Precursor selections and precursor-substrate interactions are discussed in Chapter 3. Then two specific nanomaterials are specially addressed in the next three chapters. Chapter 4 includes dissertation research work on synthesizing and characterization of pristine 1T-TaS2 while chapter 5 focus its functionalization and address the potential application and challenges. Chapter 6 is concentrated on 2H-MoS2 and evaluate its potentials in copper diffusion barriers. Chapter 7 provides a summary for all my research work and concludes this dissertation.