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Synthesis of Ag nanocubes 18-32 nm in edge length: the effects of polyol on reduction kinetics, size control, and reproducibility.

Journal of the American Chemical Society (2013-01-16)
Yi Wang, Yiqun Zheng, Cheng Zhi Huang, Younan Xia
ABSTRACT

This article describes a robust method for the facile synthesis of small Ag nanocubes with edge lengths controlled in the range of 18-32 nm. The success of this new method relies on the substitution of ethylene glycol (EG)--the solvent most commonly used in a polyol synthesis--with diethylene glycol (DEG). Owing to the increase in hydrocarbon chain length, DEG possesses a higher viscosity and a lower reducing power relative to EG. As a result, we were able to achieve a nucleation burst in the early stage to generate a large number of seeds and a relatively slow growth rate thereafter; both factors were critical to the formation of Ag nanocubes with small sizes and in high purity (>95%). The edge length of the Ag nanocubes could be easily tailored in the range of 18-32 nm by quenching the reaction at different time points. For the first time, we were able to produce uniform sub-20 nm Ag nanocubes in a hydrophilic medium and on a scale of ∼20 mg per batch. It is also worth pointing out that the present protocol was remarkably robust, showing good reproducibility between different batches and even for DEGs obtained from different vendors. Our results suggest that the high sensitivity of synthesis outcomes to the trace amounts of impurities in a polyol, a major issue for reproducibility and scale up synthesis, did not exist in the present system.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Ethylene glycol, spectrophotometric grade, ≥99%
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Ethylene glycol, ReagentPlus®, ≥99%
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Ethylene glycol, anhydrous, 99.8%
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Ethylene glycol, BioUltra, ≥99.5% (GC)
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Ethylene glycol, Pharmaceutical Secondary Standard; Certified Reference Material
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Ethylene glycol solution, NMR reference standard, 80% in DMSO-d6 (99.9 atom % D), NMR tube size 3 mm × 8 in.
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Ethylene glycol solution, NMR reference standard, 80% in DMSO-d6 (99.9 atom % D), NMR tube size 5 mm × 8 in.
Sigma-Aldrich
Ethylene glycol 5 M solution