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Ligand-assisted interfacial monomicelle assembly to incorporate intermetallic nanoparticles into mesoporous carbon nanostructures

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Abstract

Intermetallic nanoparticles (iNPs) exhibit ordered superlattice structures characterized by unique properties, for example, long-range ordering, robust metallic bonding and site-isolation effects. Multicomponent (>2) iNPs are particularly interesting for the development of advanced metallic catalysts for electrochemical applications. Integration of iNPs within mesoporous carbon nanostructures enhances mass and electron transfer during electrolysis and provides a protective mesoporous confinement that prevents iNP sintering and loss during operation. Here we describe a generalized two-step strategy to integrate iNPs with up to eight metal components into mesoporous carbon nanostructures that allows control over the ordering degree, phases and morphology. Ligand-assisted interfacial assembly of monomicelles on diverse metal substrates (using a laboratory-made amphiphilic copolymer as a structure-directing agent, with dopamine acting as both carbon precursor and metal-coordinating ligand) results in mesostructured metal–organic superstructures. All of the examples described have at least one noble metal (Pt or Pd) combined with transition metal elements (for example, Fe, Co, among others). Thermal processing of these metal–organic superstructures in an ammonia (NH3) atmosphere induces the formation of chemically ordered iNPs while simultaneously creating the mesoporous structure. The Protocol also includes procedures for two example electrochemical applications: the oxygen reduction reaction and nitrate reduction reaction for NH3 production. The entire synthetic procedure takes ~5 d, while physical characterization via electron microscopy, X-ray diffraction and nitrogen sorption isotherms require ~2 d. Investigating the catalytic mechanisms, utilizing in situ Fourier-transform infrared spectroscopy and online differential electrochemical mass analysis typically take 4–6 h for electrocatalytic reactions.

Key points

  • Multisite catalysts are important in driving complex electrochemical processes. This Protocol describes a general approach to incorporate intermetallic nanoparticles into mesoporous carbon nanostructures with different ordering degree, crystalline phases and morphology.

  • The approach starts with the preparation of mesostructured metal–organic superstructures via a ligand-assisted interfacial monomicelle assembly process. Then, annealing metal–organic superstructures in NH3 facilitates the formation of a mesoporous structure and the crystallization of metals into intermetallic nanoparticles.

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Fig. 1: Schematic illustrations of conventional synthetic approaches for construction of ordered intermetallic NPs.
Fig. 2: Schematic illustrations of synthetic approaches for construction of iNPs onto or within the carbon supports.
Fig. 3: Schematic illustrations showing the synthesis of iNPs-mC with corresponding photographs, using the PMMA-b-PEO copolymer as an example template.
Fig. 4: Schematic illustrations for the synthesis of M–DA@PMMA-b-PEO composite monomicelles.
Fig. 5: Schematic illustrations and characterizations of the MOSs, taking GO as the hydrophilic support for an example.
Fig. 6: Schemes, SEM and TEM characterization of PdFe iNPs-mC supported on various substrate supports.
Fig. 7: Characterization of PtFeCoNiCu iNPs-mC-GO annealed at different T.
Fig. 8: Characterization of binary to octonary Pt-based iNPs-mC-GO.
Fig. 9: Optical photos showing how to make high-quality electrode film.
Fig. 10: Characterization of PdFe iNPs-mC-CF.
Fig. 11: ORR study of the three represented catalysts.
Fig. 12: NO3−RR study of the three represented catalysts.

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All data generated or analyzed during this study are included in this published article. Source data are provided with this paper.

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Acknowledgements

This work was supported by the National Natural Science Foundation of China (grant nos. 52225204, W2511047, and 52572067), the Natural Science Foundation of Shanghai (grant no. 23ZR1479200), the Shanghai Scientific and Technological Innovation Project (grant no. 24520712800), Fundamental and Interdisciplinary Disciplines Breakthrough Plan of the Ministry of Education of China (grant no. JYB2025XDXM402), the Innovation Program of Shanghai Municipal Education Commission (grant no. 2021-01-07-00-03-E00109), and AI-Enhanced Research Program of Shanghai Municipal Education Commission (grant no. AMEC-AI-DHUZ-04).

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Authors and Affiliations

  1. State Key Laboratory of Advanced Fiber Materials, College of Materials Science and Engineering, Donghua University, Shanghai, China

    Pengpeng Qiu, Guihua Zhu, Minghao Li, Lianjun Wang, Wan Jiang & Wei Luo

  2. State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Shanghai, China

    Weichao Bao

  3. School of Materials Science and Engineering, Zhejiang University, Hangzhou, China

    Ying Jiang

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  1. Pengpeng Qiu
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Contributions

P.Q. and W.L. developed the Protocol and guided the project. G.Z. and M.L. performed the experiments. W.B. and Y.J. analyzed the morphology. W.B. and W. L. contributed to the discussion and manuscript modification. All authors contributed to the manuscript.

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Correspondence to Wei Luo.

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Key references

Zhu, G. et al. Adv. Mater. 37, 2413560 (2025): https://doi.org/10.1002/adma.202413560

Xie, M. et al. Adv. Energy Mater. 14, 2401717 (2024): https://doi.org/10.1002/aenm.202401717

Qiu, P. et al. NPG Asia Mater. 15, 35 (2023): https://doi.org/10.1038/s41427-023-00482-z

Zhu, G. et al. Adv. Mater. 34, 2110128 (2022): https://doi.org/10.1002/adma.202110128

Extended data

Extended Data Fig. 1 Characterization of the various binary iNPs-mC.

(a) XRD patterns, (b) Dark field STEM image of PdMn iNPs-mC-CF and corresponding EDS maps, and (c) Dark field STEM image of PdZn iNPs-mC-CF and corresponding EDS maps. Panels b and c adapted from ref. 49; Wiley.

Source data

Extended Data Fig. 2 Atomic structure characterizations of binary PtFe iNPs-mC-GO and octonary PtPdFeCoNiCuMn iNPs-mC-GO.

(a1) Atomic HAADF-STEM image of PtFe iNPs-mC-GO and (a2) Enlarged HAADF-STEM image in white frame observed in figure a1; (a3) the corresponding FFT patterns; (a4) the simulative FFT pattern projected along the [101] direction and (a5) the simulative axial rotation atomic structure scheme. (b1) Atomic HAADF-STEM image of PtPdFeCoNiCuMn iNPs-mC-GO and (b2) Enlarged HAADF-STEM image in white frame observed in figure b1; (b3) the corresponding FFT patterns; (b4) the simulative FFT pattern projected along the [100] direction and (b5) the simulative axial rotation atomic structure scheme. Panels a and b reproduced from ref. 51; Wiley.

Extended Data Fig. 3 Atomic structure characterization of PdFeCoNiCu iNPs-mC-GO.

(a,b) Atom-scale HAADF-STEM image and corresponding FFT pattern acquired along the [100] zone axis, (c,d) Atom-scale HAADF-STEM image and corresponding FFT pattern acquired along [110] zone axis, (e) Atom-resolved HAADF-STEM image and corresponding EDS maps, (f) Schematic illustration of the elemental distribution across lattice sites, superposed on the HAADF image along the [100] zone axis, (g) Column intensities along the line in (e,h) Atomic fraction for each element. Reproduced from ref. 50; Wiley.

Extended Data Fig. 4 Characterization of the recycled PdFeCoNiCu iNPs-mC-GO catalyst after NO3−RR test.

(a) Dark field STEM image with corresponding EDS elemental mapping, (b) HAADF-STTEM image with its associated FFT pattern (c). Reproduced from ref. 50; Wiley.

Supplementary information

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Qiu, P., Zhu, G., Li, M. et al. Ligand-assisted interfacial monomicelle assembly to incorporate intermetallic nanoparticles into mesoporous carbon nanostructures. Nat Protoc (2026). https://doi.org/10.1038/s41596-025-01326-6

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