Transition metal dichalcogenide (TMD) nanomaterials, especially the mono- or few-layer ones, have received extensive research interest owing to their versatile properties, ranging from true metals (e.g., NbS2 and VSe2) and semimetals (e.g., WTe2 and TiSe2) to semiconductors (e.g., MoS2 and We2) and insulators (e.g., HfS2). Therefore, the reliable production of these nanomaterials with atomically thin thickness and laterally uniform dimension is 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-based exfoliation method has emerged as a mature, efficient and promising strategy for the high-yield production of mono- or few-layer TMD nanosheets; monolayer MoS2 (yield of 92%), monolayer TaS2 (yield of 93%) and bilayer TiS2 (yield of 93%) with lateral dimensions of ~1 µm (refs. 1,2,3). 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-based exfoliation method, which involves the electrochemical intercalation of lithium ions into layered inorganic crystals and a mild sonication process. The whole protocol takes 26–38 h for the successful production of ultrathin inorganic nanosheets.
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Z.Z. thanks the Start-Up Grant from CityU (CityU9610435) and ECS scheme (CityU9048163) from RGC in Hong Kong, and the Basic Research Project from Shenzhen Science and Technology Innovation Committee in Shenzhen, China (JCYJ20210324134012034). H.S.S. acknowledges support by research funds (2020M3D1A1110548 and 2019M1A2A2065616) through NRF, Republic of Korea.
The authors declare no competing interests.
Peer review information Nature Protocols thanks the anonymous reviewers for their contribution to the peer review of this work.
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Key references using this protocol
Huang, X. et al. Nat. Commun. 4, 1444 (2013): https://www.nature.com/articles/ncomms2472#citeas
Zhu, C. et al. J. Am. Chem. Soc. 135, 5998–6001 (2013): https://pubs.acs.org/doi/10.1021/ja4019572
Mei, L. et al. Chem. Commun. 57, 2879 (2021): https://doi.org/10.1039/D0CC08091H
Key data used in this protocol
Zeng, Z. et al. Angew. Chem. Int. Ed. 50, 11093–11097 (2011): https://onlinelibrary.wiley.com/doi/10.1002/anie.201106004
Zeng, Z. et al. Angew. Chem. Int. Ed. 51, 9052–9056 (2012): https://onlinelibrary.wiley.com/doi/full/10.1002/anie.201204208
Zeng, Z. et al. Energy Environ. Sci. 7, 797–803 (2014): https://doi.org/10.1039/C3EE42620C
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Yang, R., Mei, L., Zhang, Q. et al. High-yield production of mono- or few-layer transition metal dichalcogenide nanosheets by an electrochemical lithium ion intercalation-based exfoliation method. Nat Protoc 17, 358–377 (2022). https://doi.org/10.1038/s41596-021-00643-w
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