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Fundamentals of MXene synthesis

Nature Synthesis volume 1, pages 601–614 (2022)Cite this article

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Abstract

Since the first report on Ti3C2Tx in 2011, the family of two-dimensional transition metal carbides, nitrides, and carbonitrides (MXenes) has increased substantially to include single and multi-element MXenes, with many more yet to be synthesized but predicted to possess attractive properties. To synthesize these elusive MXenes as well as to improve and scale up the manufacturing of known MXenes, a deeper mechanistic understanding of their synthesis processes is necessary, from the precursors to the etching–exfoliation and final intercalation–delamination steps. Here we examine computational modelling and in situ and ex situ characterization data to rationalize the reactivity and selectivity of MXenes towards various common etching and delamination methods. We discuss the effects of MAX phases, the predominant precursor, and other non-MAX layered materials on MXene synthesis and their resultant properties. Finally, we summarize the parameters behind successful (and unsuccessful) etching and delamination protocols. By highlighting the factors behind each step, we hope to guide the future development of MXenes with improved quality, yield and tunable properties.

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Fig. 1: Synthesis of MXenes.
Fig. 2: Relating the chemistry of mono-transition metal MXene precursor phases to their exfoliation energy.
Fig. 3: Effect of the MAX synthesis method on the mono-transition metal MXene produced.
Fig. 4: Top–down etching routes for MXene synthesis.
Fig. 5: Mechanism of HF-based etching and exfoliation.
Fig. 6: Intercalation–delamination mechanisms.

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Acknowledgements

K.R.G.L. acknowledges financial support from the Agency for Science, Technology and Research (A*STAR) Singapore National Science Scholarship (PhD). B.C.W. acknowledges financial support from the National Defense Engineering & Science Graduate Fellowship Program. M.S. acknowledges financial support from Murata Manufacturing, Japan. B.A. acknowledges funding from the US National Science Foundation (grant no. CMMI-2134607). Y.G. acknowledges funding from the US National Science Foundation (grant no. DMR-2041050). Z.W.S. acknowledges the support of the Singapore National Research Foundation (NRF-NRFF2017-04) and Agency for Science, Technology and Research (Central Research Fund Award).

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  1. These authors contributed equally: Kang Rui Garrick Lim, Mikhail Shekhirev, Brian C. Wyatt.

Authors and Affiliations

  1. Department of Chemistry and Chemical Biology, Harvard University, Cambridge, MA, USA

    Kang Rui Garrick Lim

  2. Institute of Materials Research and Engineering, Agency for Science, Technology and Research (A*STAR), Innovis, Singapore, Singapore

    Kang Rui Garrick Lim & Zhi Wei Seh

  3. A. J. Drexel Nanomaterials Institute, and Department of Materials Science and Engineering, Drexel University, Philadelphia, PA, USA

    Mikhail Shekhirev & Yury Gogotsi

  4. Department of Mechanical and Energy Engineering and Integrated Nanosystems Development Institute, Purdue School of Engineering and Technology, Indiana University–Purdue University Indianapolis, Indianapolis, IN, USA

    Brian C. Wyatt & Babak Anasori

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  4. Babak Anasori
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  5. Yury Gogotsi
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Contributions

K.R.G.L., M.S. and B.C.W. conducted the literature review and wrote the manuscript under the supervision of B.A., Y.G. and Z.W.S. All authors have given approval to the final version of the manuscript.

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Correspondence to Babak Anasori, Yury Gogotsi or Zhi Wei Seh.

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Nature Synthesis thanks Qing Huang and the other, anonymous, reviewer(s) for their contribution to the peer review of this work. Primary Handling Editor: Alison Stoddart, in collaboration with the Nature Synthesis team.

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Lim, K.R.G., Shekhirev, M., Wyatt, B.C. et al. Fundamentals of MXene synthesis. Nat. Synth 1, 601–614 (2022). https://doi.org/10.1038/s44160-022-00104-6

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