Transition metal dichalcogenides (TMDs) nanomaterials, especially the mono-or fewlayer ones, have received extensive research interest owing to their suitable band-gap, unique electronic structure, outstanding biocompatibility, excellent stability, and promising catalytic properties. Therefore, the reliable production of these nanomaterials with atomically thin thickness and laterally uniform dimension are essential for their promising applications in transistors, photodetectors, electroluminescent devices, catalysis, energy conversion, environment remediation, biosensing, bioimaging, and so on. Recently, the electrochemical lithium ion-intercalation and exfoliation method has emerged as a mature, efficient and promising strategy for the high-yield production of mono-or few-layer TMDs nanosheets; mono-layer MoS2 (yield of 92%), mono-layer TaS2 (yield of 93%) and bi-layer TiS2 (yield of 93%) with lateral dimensions of around 1 µm. This Protocol describes the details of experimental procedures for the high-yield synthesis of mono-or few-layer TMDs and other inorganic nanosheets such as MoS2, WS2, TiS2, TaS2, ZrS2, graphene, h-BN, NbSe2, WSe2, Sb2Se3, and Bi2Te3 by using the electrochemical lithium ion-intercalation and exfoliation method which involves the electrochemical intercalation of lithium ions into the layered inorganic crystals and a mild sonication. In addition, this method offers some more advantages such as the control over the nature of the crystal polytypes. The whole protocol takes 26-38 h for the successful production of the final ultrathin inorganic nanosheets.