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Nanoconfined impulse synthesis of high-entropy nanocarbides for active and stable electrocatalysis

Nature Synthesis volume 4, pages 1422–1434 (2025)Cite this article

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Abstract

Nanocarbides exhibit interesting mechanical properties and strong oxidation and corrosion resistance. The use of high-entropy effects has enhanced the performance of nanomaterials and enabled new functionalities. Despite the successful development of high-entropy nanoalloys and nanoceramics, controlled synthesis of high-entropy nanocarbides (HENCs) remains challenging due to high growth temperatures, agglomeration of nanoproducts and multi-component immiscibility. Here we achieve synthesis of HENCs containing 5–22 metal elements through a nanoconfined impulse synthetic strategy enabled by Joule heating-induced in situ reactions in carbon nanotube films. These HENCs exhibit multi-element effects and enhanced electrocatalytic activities due to nanoscale size and modification of catalytic sites. In particular, (Pt0.15WTaFe0.15Ni)Cx is highly stable for the hydrogen evolution reaction at 5 A cm−2 and demonstrates low overall-water-splitting cell voltages under industrial conditions. Moreover, (Pt0.5WTaHfCe)Cx shows high mass activities for alcohol oxidation. Density functional theory calculations elucidate the mechanism by which specific sites are modified to achieve optimal adsorption capabilities in HENC catalysts. These results demonstrate the promise of our approach for the synthesis of high performance HENC electrocatalysts.

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Fig. 1: NIS enabled by Joule heating of CNT films.
Fig. 2: Synthesis of HENCs by the NIS method.
Fig. 3: (Pt0.15WTaFe0.15Ni)Cx structural analysis.
Fig. 4: OWS performance of the (Pt0.15WTaFe0.15Ni)Cx/CNT film.
Fig. 5: Alcohol electrooxidation performance of the (Pt0.5WTaHfCe)Cx/CNT film.

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The data supporting this study are available in this Article and its Supplementary Information.

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Acknowledgements

K.L. acknowledges the financial support from Basic Science Center Project of NSFC (grant no. 52388201), National Natural Science Foundation of China (grant no. 52272041) and National Key R&D Program of China (grant no. 2022YFA1203400). J.L. acknowledges the support from the National Key R&D Program of China (grant nos. 2022YFA1203400 and 2021YFA1400100), the National Natural Science Foundation of China (grant no. 12274254), Local Innovative and Research Teams Project of Guangdong Pearl River Talents Program (grant no. 2017BT01N111), Basic Research Project of Shenzhen, China (grant nos. JCYJ20200109142816479, WDZC20200819115243002) and Shenzhen Outstanding Talents Training Fund. Computational resources were supported by High Performance Computing Platform of Nanjing University of Aeronautics and Astronautics. K.Z. acknowledges the financial support from Natural Science Foundation of Shandong, China (grant no. ZR2023MB062). J.C. acknowledges the financial support from Beijing Natural Science Foundation (grant no. QY23095).

Author information

Author notes

  1. These authors contributed equally: Chenyu Li, Zhichao Zhang, Kunlei Zhu, Mingda Liu, Jiayuan Chen.

Authors and Affiliations

  1. State Key Laboratory of New Ceramic Materials, and Key Laboratory of Advanced Materials of Ministry of Education of China, School of Materials Science and Engineering, Tsinghua University, Beijing, People’s Republic of China

    Chenyu Li, Kunlei Zhu, Mingda Liu, Jiayuan Chen, Yonghuang Wu, Jing Guo, Run Shi, Zeqin Xin, Hui Wu & Kai Liu

  2. Shanghai Bright-H Technology Co., Ltd, Shanghai Electric, Shanghai, People’s Republic of China

    Chenyu Li

  3. Shenzhen Geim Graphene Center and Institute of Materials Research, Tsinghua Shenzhen International Graduate School, Tsinghua University, Shenzhen, People’s Republic of China

    Zhichao Zhang & Jia Li

  4. School of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, People’s Republic of China

    Kunlei Zhu

  5. Beijing Key Laboratory for Magneto-Photoelectrical Composite and Interface Science, School of Mathematics and Physics, State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing, People’s Republic of China

    Liang Zhou, Yinghui Sun & Rongming Wang

  6. Institute of Physics, Chinese Academy of Sciences, Beijing, People’s Republic of China

    Qinghua Zhang

  7. Department of Physics, Tsinghua University, Beijing, People’s Republic of China

    Peng Liu & Shoushan Fan

  8. Beijing Electron Microscope Center, School of Materials Science and Engineering, Tsinghua University, Beijing, People’s Republic of China

    Lin Gu

  9. Department of Chemistry, Tsinghua University, Beijing, People’s Republic of China

    Dingsheng Wang & Yadong Li

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  1. Chenyu Li
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Contributions

K.L. and C.L. conceived the project and designed experiments. C.L., M.L., J.C. and Y.W. synthesized the samples. C.L., L.Z., Q.Z., L.G. and R.W. carried out the TEM characterizations. C.L., M.L., J.G., R.S. and Z.X. did other structural characterizations. C.L. performed the electrochemical measurements. J.L. and Z.Z. performed the DFT calculations. C.L., K.Z., K.L., J.L., Z.Z., Y.S. and P.L. analysed the data. K.L., K.Z., J.L., C.L., Z.Z., H.W., D.W., Y.L. and S.F. discussed the working mechanism. C.L., K.Z., K.L., Z.Z. and J.L. wrote and revised the manuscript. All authors discussed the results and contributed to the final version of the manuscript.

Corresponding authors

Correspondence to Jia Li or Kai Liu.

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Nature Synthesis thanks Wei Hsuan Hung, Uk Sim and the other, anonymous, reviewer(s) for their contribution to the peer review of this work. Primary Handling Editor: Alexandra Groves, in collaboration with the Nature Synthesis team.

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Extended data

Extended Data Fig. 1 XAFS spectra of the (Pt0.15WTaFe0.15Ni)Cx/CNT film.

XANES spectra of a, Pt L1-edge, d, W L1-edge, and g, Ta L1-edge. R-space EXAFS spectra of b, Pt L1-edge, e, W L1-edge, and h, Ta L1-edge, where the element ‘M’ represents a metal element (Pt, W, Ta, Fe, or Ni). Wavelet-transform images of c, Pt L1-edge, f, W L1-edge, and i, Ta L1-edge. Pt foil, PtO2, W foil, WO3, Ta foil, and Ta2O5 are used as references. PtO2 data are obtained from ref. 67, Pt-CA-CNT from ref. 68, WC from ref. 69, WO3 from ref. 70, and Ta foil, TaC, and Ta2O5 from ref. 28.

Source data

Extended Data Fig. 2 Electrochemical Performance and DFT Calculations of the (Pt0.15WTaFe0.15Ni)Cx/CNT film.

a, Δη/Δlog|j| ratios of the (Pt0.15WTaFe0.15Ni)Cx/CNT film, (Pt0.15WTa)Cx/CNT film, and (Fe0.15Ni)Cx/CNT film at different current densities. b,c, TOF of different catalysts. When calculating the TOFs, the active sites are Pt and Ta in HER and Ni in OER for (Pt0.15WTaFe0.15Ni)Cx. For (Pt0.15WTa)Cx, Pt and Ta are regarded as active sites in HER, and for (Fe0.15Ni)Cx, Ni is the active site in OER. d, The HER overpotential of (PtWTaFeNi)yCx/CNT films at low current density (100 mA cm−2). e–g, Density of states of the d orbitals for all metal atoms, Pt atom and Ta atom, respectively, in (Pt0.15WTa0.2Fe0.15Ni)Cx (with less Ta), (Pt0.15WTaFe0.15Ni)Cx, and (Pt0.15W0.2TaFe0.15Ni)Cx (with less W). The fermi level (Ef) is denoted by the dashed grey line, while the positions of the d-band centres are shown as dotted lines. h, Volcano plot between the predicted overpotential and the adsorption free energy of H atom (ΔG*H, * denotes the adsorbed state). The red and blue plots represent the averaged activities of each element on the (111) surfaces of (Pt0.15WTaFe0.15Ni)Cx (HM5) and (Pt0.15WTa)Cx (HM3), respectively. The result of Pt(111) is also shown as a dashed line and yellow plot for reference. i, Bader charges of surface Ta sites with different chemical environments. Schematic diagram showing the adjustment of adsorption strength achieved by modulating the d-band occupation of the active site. j, The free energy profiles of the OER at surface Ni sites on (Pt0.15WTaFe0.15Ni)Cx, (Fe0.15Ni)Cx and NiC at 1.23 V vs RHE. The predicted overpotentials are also shown.

Source data

Extended Data Fig. 3 HER stability of the (Pt0.15WTaFe0.15Ni)Cx/CNT film.

a,b, AC-TEM images of the (Pt0.15WTaFe0.15Ni)Cx/CNT film before and after the long-term test, respectively. c, XRD patterns of the (Pt0.15WTaFe0.15Ni)Cx/CNT film before and after the long-term test at 2000 mA cm−2 for ~600 h. d, Comparison of the long-term stability and maximum stable current density of different HER catalysts4,34,35,54,71,72,73,74,75,76,77.

Source data

Supplementary information

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Supplementary Figs. 1–76, Tables 1–17 and Discussion.

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Li, C., Zhang, Z., Zhu, K. et al. Nanoconfined impulse synthesis of high-entropy nanocarbides for active and stable electrocatalysis. Nat. Synth 4, 1422–1434 (2025). https://doi.org/10.1038/s44160-025-00854-z

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