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Facile synthesis of gold nanomaterials with unusual crystal structures

Nature Protocols volume 12, pages 2367–2376 (2017)Cite this article

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Abstract

Gold (Au) nanomaterials have attracted wide research attention, owing to their high chemical stability, promising catalytic properties, excellent biocompatibility, unique electronic structure and outstanding localized surface plasmon resonance (LSPR) absorption properties; all of which are closely related to their size and shape. Recently, crystal-phase-controlled synthesis of noble metal nanomaterials has emerged as a promising strategy to tune their physicochemical properties. This protocol describes the detailed experimental procedures for the crystal-phase-controlled syntheses of Au nanomaterials with unusual crystal structures under mild conditions. Briefly, pure hexagonal close-packed (hcp) Au square sheets (AuSSs) with a thickness of ∼2.4 nm are synthesized using a graphene-oxide-assisted method in which HAuCl4 is reduced by oleylamine in a mixture of hexane and ethanol. By using pure hexane as the solvent, well-dispersed ultrathin hcp/face-centered cubic (fcc) Au nanowires with a diameter of ∼1.6 nm on graphene oxide can be obtained. Meanwhile, hcp/fcc Au square-like plates with a side length of 200–400 nm are prepared via the secondary growth of Au on the hcp AuSSs. Remarkably, hexagonal (4H) Au nanoribbons with a thickness of 2.0–6.0 nm can be synthesized with a one-pot colloidal method in which HAuCl4 is reduced by oleylamine in a mixed solvent of hexane and 1,2-dichloropropane. It takes 17–37 h for the synthesis of these Au nanomaterials with unusual crystal structures. Transmission electron microscopy (TEM) and atomic force microscopy (AFM) are used to characterize the resultant Au nanomaterials, which could have many promising applications, such as biosensing, near-IR photothermal therapy, catalysis and surface-enhanced Raman scattering (SERS).

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Figure 1
Figure 2: Photographs of the experimental setup used for the synthesis of Au nanomaterials with unusual crystal structures.
Figure 3: TEM characterization of hcp AuSSs.
Figure 4: TEM characterization of hcp/fcc Au NWs.
Figure 5: A typical TEM image of hcp/fcc Au NWs synthesized in the presence of water in the reaction solution, leading to the formation of many spherical Au nanoparticles.
Figure 6: TEM and AFM characterizations of hcp/fcc AuSPs.
Figure 7: TEM characterization of 4H Au NRBs.

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Acknowledgements

This work was supported by the Singapore Ministry of Education (MOE) under Academic Research Fund (AcRF) Tier 2 (ARC 19/15, MOE2014-T2-2-093; MOE2015-T2-2-057; MOE2016-T2-2-103) and AcRF Tier 1 (2016-T1-001-147; 2016-T1-002-051), and by Nanyang Technological University (NTU) under a Start-Up Grant (M4081296.070.500000) in Singapore. It was also supported by the Joint Research Fund for Overseas Chinese, Hong Kong and Macao Scholars (51528201), the National Natural Science Foundation of China (51322202). We acknowledge the Facility for Analysis, Characterization, Testing and Simulation, Nanyang Technological University, Singapore, for use of its electron microscopy facilities.

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Authors and Affiliations

  1. Center for Programmable Materials, School of Materials Science and Engineering, Nanyang Technological University, Singapore, Singapore

    Zhanxi Fan, Ye Chen & Hua Zhang

  2. Key Laboratory of Flexible Electronics (KLOFE) and Institute of Advanced Materials (IAM), Jiangsu National Synergistic Innovation Center for Advanced Materials (SICAM), Nanjing Tech University, Nanjing, China

    Xiao Huang & Wei Huang

  3. Shaanxi Institute of Flexible Electronics (SIFE), Northwestern Polytechnical University (NPU), Xi'an, China

    Wei Huang

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Contributions

H.Z. proposed the research direction and guided the project. Z.F., X.H. and H.Z. developed the protocol. Z.F. and X.H. performed the experiments. Z.F., X.H., Y.C., W.H. and H.Z. drafted the manuscript. Y.C. performed some supporting experiments. All authors contributed to the manuscript.

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Correspondence to Hua Zhang.

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Fan, Z., Huang, X., Chen, Y. et al. Facile synthesis of gold nanomaterials with unusual crystal structures. Nat Protoc 12, 2367–2376 (2017). https://doi.org/10.1038/nprot.2017.097

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