Two-dimensional nanoscale materials (2D NMs) have exceptional physical characteristics, distinctive structures, and customizable surface chemistry. They consist of infinite transverse dimensions of near-atomic thickness or atoms. They promise advancements in catalysis, renewable energy, and sensing. An extensive summary of the most recent research results on the creation and use of 2D NMs is provided in this work. It is possible to modify the characteristics of these multi-layered materials by means of chemical and physical manipulations. Due to their layer-dependent electrical properties, certain 2D layered inorganic nanomaterials such as MoS2, WS2, and SnS2 have recently been created and used in a variety of applications, including new sensors. In addition, the article delves into the difficulties confronted by sectors reliant on nanotechnology as well as the potential future uses of nanostructures coupled with electrochemical systems. The article begins by outlining the typical “top-down” and “bottom-up” approaches for synthesizing 2D NMs. These approaches include hydrothermal procedures, ion intercalation, mechanical exfoliation, liquid-phase exfoliation assisted by ultrasonic waves, and chemical vapor deposition. 2D NMs are the focus of this work because of their potential applications in gas sensing, photocatalysis, electrocatalysis, photo detection, and electromagnetic wave absorption. In addition, the study predicts patterns of future development and possible issues with 2D NMs based on existing studies. Increased demand for cost-effective, environmentally friendly, and highly connected products is propelling the ongoing research and development of these high-performance materials. This research is significant since it summarizes, in one place, the most recent advances in 2D NM preparation methods and applications.