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Versatile synthesis of uniform mesoporous superparticles from stable monomicelle units

Nature Protocols volume 20, pages 1310–1351 (2025)Cite this article

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Abstract

Superstructures with architectural complexity and unique functionalities are promising for a variety of practical applications in many fields, including mechanics, sensing, photonics, catalysis, drug delivery and energy storage/conversion. In the past five years, a number of attempts have been made to build superparticles based on amphiphilic polymeric micelle units, but most have failed owing to their inherent poor stability. Determining how to stabilize micelles and control their superassembly is critical to obtaining the desired mesoporous superparticles. Here we provide a detailed procedure for the preparation of ultrastable polymeric monomicelle building units, the creation of a library of ultrasmall organic–inorganic nanohybrids, the modular superassembly of monomicelles into hierarchical superstructures and creation of novel multilevel mesoporous superstructures. The protocol enables precise control of the number of monomicelle units and the derived mesopores for superparticles. We show that ultrafine nanohybrids display enhanced mechanical antipressure performance compared with pristine polymeric micelles, and describe the functional characterization of mesoporous superstructures that exhibit excellent oxygen reduction reactivity. Except for the time (4.5 d) needed for the preparation of the triblock polystyrene-block-poly(4-vinylpyridine)-block-poly(ethylene oxide) PS-PVP-PEO or the polystyrene-block-poly(acrylic acid)-block-poly(ethylene oxide) (PS-PAA-PEO) copolymer, the synthesis of the ultrastable monomicelle, ultrafine organic–inorganic nanohybrids, hierarchical superstructures and mesoporous superparticles require ~6, 30, 8 and 24 h, respectively. The time needed for all characterizations and applications are 18 and 10 h, respectively.

Key points

  • This protocol describes the preparation of ultrastable polymeric monomicelle building units, the construction of a library of ultrasmall organic–inorganic nanohybrids, the superassembly of monomicelles into hierarchical superstructures and the generation of multilevel mesoporous superstructures.

  • Compared with pristine polymeric micelles, ultrafine nanohybrids exhibit enhanced mechanical antipressure performance and the mesoporous superstructures exhibit excellent oxygen reduction reactivity.

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Fig. 1: Schematic representation of the versatile fabrication process of superstructures based on ultrastable monomicelle superassembly.
Fig. 2: Photographs and corresponding models during the synthesis of ultrastable monomicelles and ultrafine nanohybrids.
Fig. 3: Photographs and corresponding models during the synthesis of the hierarchical superstructures and mesoporous superparticles.
Fig. 4: Detailed schematic illustrations of the entire fabrication process from ultrastable monomicelle formation to ultrafine organic/inorganic nanohybrid formation.
Fig. 5: Characterization of monomicelles and derived ultrafine micelles/SiO2 nanohybrids.
Fig. 6: Dependences of particle sizes and SiO2 shell thickness for the micelle/SiO2 nanohybrids on the molecular weights of the PS-PVP-PEO copolymers.
Fig. 7: Characterization of ultrafine micelles/ZnO nanohybrids.
Fig. 8: The characterization of a library of ultrafine nanohybrids templated by PS-PVP-PEO or PS-PAA-PEO ultrastable monomicelles.
Fig. 9: Dependence of monomicelle size for ‘core–satellites’ SiO2@monomicelles superstructures on molecular weights of the PS-PVP-PEO copolymers.
Fig. 10: Variability of the monomicelle superassembly approach for ‘core–satellites’ and ‘core–satellites–satellites’ superstructures.
Fig. 11: Dependence of mesopore number for the mesoporous carbon superparticles on the added amount of ammonia.
Fig. 12: Physicochemical characterizations of the mesoporous carbon superparticles.
Fig. 13: The mechanical antipressure performance of polymeric PS-PVP-PEO monomicelles and the ultrasmall organic–inorganic micelles/SiO2 nanohybrids.
Fig. 14: ORR performance of the mesoporous carbon superparticles.

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All data generated or analyzed during this study are included in this published article.

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Acknowledgements

This work was supported by the National Key R&D Program of China (nos. 2022YFA1503501 (W.L.) and 2018YFA0209401 (D.Z.)), National Nature Science Foundation of China (nos. 22105041 (D.Z.), 21733003 (D.Z.), U21A20329 (W.L.), 51975502 (D.Z.), 21975050 (W.L.), 22365021 (Y.Z.) and 22305132 (Z.Z.)), Program of Shanghai Academic Research Leader (no. 21XD1420800 (W.L.)), Shanghai Pilot Program for Basic Research-Fudan University 21TQ1400100 (no. 21TQ008 (W.L.)) and Science and Technology Commission of Shanghai Municipality (no. 22JC1410200 (D.Z.)), ‘Junma’ Program of Inner Mongolia University (10000-23112101/045 (Z.Z.)), Inner Mongolia Natural Science Foundation Youth Fund (2023QN02014 (Z.Z.)), ‘Young academic talents’ Program of Inner Mongolia University (23600-5233706 (Y.Z.)), Natural Science Basic Research Program of Shaanxi (no. 2023-JC-QN-0498 (Y.X.)), Key Research and Development Plan of Shaanxi (no. 2023-YBGY-173, (Y.X.)) and Science and Technology Plan Project of Xi’an (no. 2022JH-RYFW-0137 (Y.X.)).

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Authors and Affiliations

  1. College of Energy Materials and Chemistry, College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot, China

    Zaiwang Zhao, Pengfei Zhang, Yujuan Zhao & Dongyuan Zhao

  2. College of Chemistry and Materials, Department of Chemistry, Laboratory of Advanced Materials, Fudan University, Shanghai, China

    Lipeng Wang, Jie Zhang, Fanxing Bu, Wanhai Zhou, Ruizheng Zhao, Xingmiao Zhang, Zirui Lv, Yupu Liu, Wei Zhang, Tiancong Zhao, Dongliang Chao, Wei Li & Dongyuan Zhao

  3. School of Materials Science and Engineering, Xi’an Shiyou University, Xi’an, China

    Yuan Xia

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Contributions

Z.Z., W.L. and D.Z. developed the protocol and co-drafted the manuscript. P.Z., Y.Z., L.W. and J.Z. contributed to the discussion and manuscript modification. F.B., W.Zhou, R.Z., X.Z. and Z.L. analyzed morphologies. Y.L., Y.X., W.Zhang, T.Z. and D.C. did formal analysis. All authors contributed to the manuscript.

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Correspondence to Zaiwang Zhao, Wei Li or Dongyuan Zhao.

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Key references

Zhao, Z. et al. Adv. Mater. 33, 2100820 (2021): https://doi.org/10.1002/adma.202100820

Zhao, Z. et al. Sci. Adv. 8, eabo0283 (2022): https://doi.org/10.1126/sciadv.abo0283

Zhao, Z. et al. J. Am. Chem. Soc. 26, 11767–11777 (2022): https://doi.org/10.1021/jacs.2c03814

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Zhao, Z., Zhang, P., Zhao, Y. et al. Versatile synthesis of uniform mesoporous superparticles from stable monomicelle units. Nat Protoc 20, 1310–1351 (2025). https://doi.org/10.1038/s41596-024-01073-0

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