This study presents a scalable method for exfoliating inorganic layered compounds, such as MoS₂, BN, transition metal dichalcogenides (TMDs), and transition metal oxides, in aqueous surfactant solutions. The method involves sonication in the presence of a surfactant, which stabilizes the exfoliated nanosheets against re-aggregation. The resulting nanosheets are highly stable, with sizes ranging from tens to hundreds of nanometers, and can be used to form thin films, hybrids, and composites. The method is robust, scalable, and can be performed under ambient conditions. The exfoliated nanosheets exhibit unique properties, such as high surface area and tunable electronic behavior, making them suitable for applications in thermoelectrics, batteries, and supercapacitors. For example, hybrid films of MoS₂ and carbon nanotubes show enhanced electrical conductivity, while MoS₂ films are semiconducting with an optical gap of ~1.6 eV. The method also allows for the production of films with controlled thickness and composition, enabling the creation of materials with tailored properties. The study demonstrates that the exfoliation method is not limited to MoS₂ but can be extended to a wide range of layered compounds, including BN, WS₂, TaSe₂, MoTe₂, MoSe₂, and NbSe₂. These materials can be dispersed in water and used to create films and composites with applications in supercapacitors and other devices. The method is particularly advantageous compared to ion intercalation, as it is faster, more efficient, and less sensitive to environmental conditions. The exfoliated nanosheets are characterized using techniques such as transmission electron microscopy (TEM), Raman spectroscopy, and zeta potential measurements. These analyses confirm the structural integrity and stability of the exfoliated materials. The method also allows for the production of thin films with controlled thickness and composition, enabling the development of materials with enhanced mechanical and electrical properties. Overall, this method provides a versatile and scalable approach for the exfoliation and characterization of inorganic layered compounds, with potential applications in a wide range of technologies, including energy storage, optoelectronics, and materials science.This study presents a scalable method for exfoliating inorganic layered compounds, such as MoS₂, BN, transition metal dichalcogenides (TMDs), and transition metal oxides, in aqueous surfactant solutions. The method involves sonication in the presence of a surfactant, which stabilizes the exfoliated nanosheets against re-aggregation. The resulting nanosheets are highly stable, with sizes ranging from tens to hundreds of nanometers, and can be used to form thin films, hybrids, and composites. The method is robust, scalable, and can be performed under ambient conditions. The exfoliated nanosheets exhibit unique properties, such as high surface area and tunable electronic behavior, making them suitable for applications in thermoelectrics, batteries, and supercapacitors. For example, hybrid films of MoS₂ and carbon nanotubes show enhanced electrical conductivity, while MoS₂ films are semiconducting with an optical gap of ~1.6 eV. The method also allows for the production of films with controlled thickness and composition, enabling the creation of materials with tailored properties. The study demonstrates that the exfoliation method is not limited to MoS₂ but can be extended to a wide range of layered compounds, including BN, WS₂, TaSe₂, MoTe₂, MoSe₂, and NbSe₂. These materials can be dispersed in water and used to create films and composites with applications in supercapacitors and other devices. The method is particularly advantageous compared to ion intercalation, as it is faster, more efficient, and less sensitive to environmental conditions. The exfoliated nanosheets are characterized using techniques such as transmission electron microscopy (TEM), Raman spectroscopy, and zeta potential measurements. These analyses confirm the structural integrity and stability of the exfoliated materials. The method also allows for the production of thin films with controlled thickness and composition, enabling the development of materials with enhanced mechanical and electrical properties. Overall, this method provides a versatile and scalable approach for the exfoliation and characterization of inorganic layered compounds, with potential applications in a wide range of technologies, including energy storage, optoelectronics, and materials science.