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Facile synthesis of Ag nanocubes and Au nanocages


This protocol describes a method for the synthesis of Ag nanocubes and their subsequent conversion into Au nanocages via the galvanic replacement reaction. The Ag nanocubes are prepared by a rapid (reaction time < 15 min), sulfide-mediated polyol method in which Ag(I) is reduced to Ag(0) by ethylene glycol in the presence of poly(vinyl pyrrolidone) (PVP) and a trace amount of Na2S. When the concentration of Ag atoms reaches supersaturation, they agglomerate to form seeds that then grow into Ag nanostructures. The presence of both PVP and Na2S facilitate the formation of nanocubes. With this method, Ag nanocubes can be prepared and isolated for use within approximately 3 h. The Ag nanocubes can then serve as sacrificial templates for the preparation of Au nanocages, with a method for their preparation also described herein. The procedure for Au nanocage preparation and isolation requires approximately 5 h.

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Figure 1: Schematic illustration summarizing how hollow nanostructures with various porosities evolve from Ag nanocubes with increasing amounts of HAuCl4 solution added to the reaction.
Figure 2: Photographs of the experimental setup used to prepare Ag nanocubes.
Figure 3: A schematic of a custom-made vial holder, compatible with a 100 mm × 50 mm crystallization dish.
Figure 4: A photograph of the experimental setup used to prepare Au nanocages via the galvanic replacement reaction.
Figure 5: Photographs of Ag nanocubes at various stages of preparation.
Figure 6: Scanning electron microscope (SEM) images of Ag nanocubes.
Figure 7: Characterization of Au nanocages.
Figure 8: A scanning electron microscope image (insert: transmission electron microscope image) of Au nanocages prepared through the galvanic replacement reaction between Ag nanocubes and HAuCl4 aqueous solution (scale bars are 100 nm for both images).

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This work was supported in part by a Director's Pioneer Award (5DP1OD000798 to Y.X.) from National Institutes of Health (NIH), a grant from National Science Foundation (NSF) (DMR-0451788 to Y.X.), a grant from NIH (5R01CA120480 to X.L.), a DARPA-DURINT subcontract from Harvard University, and a fellowship from David and Lucile Packard Foundation. Y.X. is an Alfred P. Sloan Research Fellow (2000–2005) and a Camille Dreyfus Teacher Scholar (2002–2007). L.A. thanks the UW Center for Nanotechnology for an IGERT Student Fellowship jointly sponsored by NSF and National Cancer Institute (NCI). Part of the work was performed at the UW Nanotech User Facility (NTUF), a member of the National Nanotechnology Infrastructure Network (NNIN) funded by NSF.

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Correspondence to Younan Xia.

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Skrabalak, S., Au, L., Li, X. et al. Facile synthesis of Ag nanocubes and Au nanocages. Nat Protoc 2, 2182–2190 (2007).

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