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A general protocol for precise syntheses of ordered mesoporous intermetallic nanoparticles

Nature Protocols volume 18, pages 3126–3154 (2023)Cite this article

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Abstract

Intermetallic nanomaterials consist of two or more metals in a highly ordered atomic arrangement. There are many possible combinations and morphologies, and exploring their properties is an important research area. Their strict stoichiometry requirement and well-defined atom binding environment make intermetallic compounds an ideal research platform to rationally optimize catalytic performance. Making mesoporous intermetallic materials is a further advance; crystalline mesoporosity can expose more active sites, facilitate the mass and electron transfer, and provide the distinguished mesoporous nanoconfinement environment. In this Protocol, we describe how to prepare ordered mesoporous intermetallic nanomaterials with controlled compositions, morphologies/structures and phases by a general concurrent template strategy. In this approach, the concurrent template used is a hybrid of mesoporous platinum or palladium and Korea Advanced Institute of Science and Technology-6 (KIT-6) (meso-Pt/KIT-6 or meso-Pd/KIT-6) that can be transformed by the second precursors under reducing conditions. The second precursor can either be a second metal or a metalloid/non-metal, e.g., boron/phosphorus. KIT-6 is a silica scaffold that is removed using NaOH or HF to form the mesoporous product. Procedures for example catalytic applications include the 3-nitrophenylacetylene semi-hydrogenation reaction, p-nitrophenol reduction reaction and electrochemical hydrogen evolution reaction. The synthetic strategy for preparation of ordered mesoporous intermetallic nanoparticles would take almost 5 d; the physical characterization by electron microscope, X-ray diffraction and inductively coupled plasma–mass spectrometry takes ~2 days and the function characterization depends on the research question, but for catalysis it takes 1–5 h.

Key points

  • Ordered mesoporous intermetallic compounds are generated by first hybridizing platinum or palladium with a silica scaffold (KIT-6), adding a second metal or metalloid/non-metal under reducing conditions, followed by removal of KIT-6 using either NaOH or HF.

  • Other synthetic approaches do not allow the preparation of ordered mesostructures. The advantage of creating ordered mesostructures is that it is easier to optimize the structure–activity profile of the resulting materials.

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Fig. 1: Traditional synthetic strategies.
Fig. 2: Comparisons of the concurrent template syntheses of ordered mesoporous intermetallic nanoparticles with traditional methods.
Fig. 3: Synthesis procedures.
Fig. 4: Morphological and structural characterizations of ordered meso-Pt (Pd)/KIT-6 (SBA-15) nanoparticles.
Fig. 5: Morphological and structural characterizations of ordered meso-i-PtSn nanoparticles.
Fig. 6: Crystalline structure characterizations of meso-i-PtSn nanoparticles.
Fig. 7: Characterizations of other meso-i-Pt/Pd-based nanoparticles.
Fig. 8: Characterization of meso-i-Pt1Sn1(SBA-15) nanobundles and h-meso-i-Pt1Sn1 nanoparticles.
Fig. 9: Characterization of ordered meso-i-PtZnCo trimetals.
Fig. 10: Characterization of ordered meso-i-Pd2B nanoparticles.
Fig. 11: Characterization of ordered meso-i-PtX2 and meso-i-Pt1-xMxP2 nanoparticles.
Fig. 12: Catalytic performance of ordered meso-i-PtSn nanoparticles in semi-hydrogenation reaction of 3-NPA.
Fig. 13: Catalytic performance of ordered meso-i-PtZnCo trimetals in electrocatalytic HER.
Fig. 14: Catalytic performance of ordered meso-i-Pd2B nanoparticles in hydrogenation reaction of p-NP.

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Data availability

The data supporting this work are included in the Extended Data and Supplementary Information as well as in refs. 36,42,63,68,70.

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Acknowledgements

B.L. acknowledges financial supports from the Natural Science Foundation of Sichuan Province (2023NSFC0080) and the Fundamental Research Funds for the Central Universities. Y.Y. thanks the supports from the JST-ERATO Yamauchi Materials Space-Tectonics Project (JPMJER2003) and the Queensland node of the NCRIS-enabled Australian National Fabrication Facility (ANFF). We thank Y. Huang (Center of Engineering Experimental Teaching, School of Chemical Engineering, Sichuan University) for the discussion of SEM images and F. Yang (the Comprehensive Training Platform of the Specialized Laboratory, College of Chemistry, Sichuan University) for the discussion of TEM images.

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Authors and Affiliations

  1. Key Laboratory of Green Chemistry and Technology of Ministry of Education, College of Chemistry, Sichuan University, Chengdu, China

    Hao Lv, Yanzhi Wang, Lizhi Sun & Ben Liu

  2. Australian Institute for Bioengineering and Nanotechnology (AIBN), The University of Queensland, Brisbane, Queensland, Australia

    Yusuke Yamauchi

  3. Department of Materials Process Engineering, Graduate School of Engineering, Nagoya University, Nagoya, Japan

    Yusuke Yamauchi

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  1. Hao Lv
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Contributions

B.L. conceived the idea and provided design guidelines. H.L., Y.Y. and B.L. developed the protocol and co-drafted the manuscript. Y.W. and L.S. contributed to the discussion and manuscript modification.

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Correspondence to Ben Liu.

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Key references using this protocol

Lv, H. et al. Angew. Chem. Int. Ed. 61, e202116179/1-8 (2022): https://doi.org/10.1002/anie.202116179

Wang, Y. et al. Adv. Energy Mater. 12, 2201478/1-8 (2022): https://doi.org/10.1002/aenm.202201478

Lv, H. et al. Angew. Chem. Int. Ed. 62, e202304420/1-8 (2023): https://doi.org/10.1002/anie.202304420

Key data used in this protocol

Wang, H. et al. J. Am. Chem. Soc. 133, 14526–14529 (2011): https://doi.org/10.1021/ja2058617

Lv, H. et al. Angew. Chem. Int. Ed. 61, e202116179/1-8 (2022): https://doi.org/10.1002/anie.202116179

Lv, H. et al. ACS Cent. Sci. 6, 2347–2353 (2020): https://doi.org/10.1021/acscentsci.0c01262

Wang, Y. et al. Adv. Energy Mater. 12, 2201478/1-8 (2022): https://doi.org/10.1002/aenm.202201478

Wang, Y. et al. CCS Chem. 5, 1896–1907 (2023): https://doi.org/10.31635/ccschem.022.202202451

Extended data

Extended Data Fig. 1 The comparison of soft and hard-templating method for the syntheses of mesoporous nanomaterials.

(a) Soft-templating method and (b) hard-templating method for the syntheses of mesoporous nanomaterials.

Extended Data Fig. 2 TEM images of mesoporous silica used in the Protocol.

TEM images of (a,b) KIT-6 and (c,d) SBA-15. Figure adapted with permission from ref. 36, American Chemical Society.

Extended Data Fig. 3 The schematic procedures of the other morphologies and compositions of mesoporous intermetallics.

The schematic procedures of the concurrent templates toward the syntheses of the mesoporous intermetallic nanoparticles of (a) meso-i-Pt1Sn1(SBA-15), (b) h-meso-i-Pt1Sn1, (c) meso-i-PtZnCo and (d) meso-i-Pd2B.

Extended Data Fig. 4 TEM images of meso-i-Pt1Sn1 nanoparticles with different nanoparticle size.

TEM images of meso-i-Pt1Sn1 nanoparticles with a nanoparticle size of (a) 121 nm, (b) 164 nm, and (c) 208 nm. Figure adapted with permission from ref. 42, Wiley.

Extended Data Fig. 5 STEM EDS mapping images of meso-i-PtX2.

STEM EDS mapping images of meso-i-PtP2, meso-i-PtS2, meso-i-PtSe2 and meso-i-PtTe2. Figure adapted with permission from ref. 70, Chinese Chemical Society.

Extended Data Fig. 6 STEM/TEM and STEM EDX images of meso-i-Pt1Sn1, meso-i-Pt3Sn1, and meso-Pt nanoparticles after catalysis.

STEM/TEM and STEM EDX images of (a,b) meso-i-Pt1Sn1, (c,d) meso-i-Pt3Sn1, and (e–h) meso-Pt nanoparticles after catalysis. All the nanoparticles retained their structure/morphology and composition, indicating a good catalytic stability. Figure adapted with permission from ref. 42, Wiley.

Extended Data Fig. 7 PXRD patterns of meso-Pt, meso-i-Pt3Sn1, and meso-i-Pt1Sn1 nanoparticles after catalytic stability tests.

All samples retained PXRD peaks well, indicating they are chemically stable for catalysis. Figure adapted with permission from ref. 42, Wiley.

Extended Data Fig. 8 EDS mapping images of meso-i-PtZnCo after ADT.

EDS mapping images of meso-i-PtZnCo after the (a) 5000, (b) 10000, (c) 30000, (d) 50000 CV cycles. Figure adapted with permission from ref. 68, Wiley.

Extended Data Fig. 9 TEM images of Commercial Pt/C after ADT.

TEM images of Commercial Pt/C after the (a) 1, (b) 5000, (c) 10000, (d) 20000 CV cycles. Figure adapted with permission from ref. 68, Wiley.

Supplementary information

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Lv, H., Wang, Y., Sun, L. et al. A general protocol for precise syntheses of ordered mesoporous intermetallic nanoparticles. Nat Protoc 18, 3126–3154 (2023). https://doi.org/10.1038/s41596-023-00872-1

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