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Mono- and bi-functional arenethiols as surfactants for gold nanoparticles: synthesis and characterization.

Vitale F, Fratoddi I, Battocchio C, Piscopiello E, Tapfer L, Russo MV, Polzonetti G, Giannini C - Nanoscale Res Lett (2011)

Bottom Line: Stable gold nanoparticles stabilized by different mono and bi-functional arenethiols, namely, benzylthiol and 1,4-benzenedimethanethiol, have been prepared by using a modified Brust's two-phase synthesis.Nanocrystals diameters have been tuned in the range 2 ÷ 9 nm by a proper variation of Au/S molar ratio.In particular, the formation of networks has been observed with interconnected gold nanoparticles containing 1,4-benzenedimethanethiol as ligand.

View Article: PubMed Central - HTML - PubMed

Affiliation: ENEA (Italian National Agency for New Technologies, Energy and the Sustainable Economic Development), UTTMATB (Technical Unit of Materials Technologies - Brindisi), Brindisi Research Centre, S,S, 7 Appia km, 706, 72100 Brindisi, Italy. floriana.vitale@enea.it.

ABSTRACT
Stable gold nanoparticles stabilized by different mono and bi-functional arenethiols, namely, benzylthiol and 1,4-benzenedimethanethiol, have been prepared by using a modified Brust's two-phase synthesis. The size, shape, and crystalline structure of the gold nanoparticles have been determined by high-resolution electron microscopy and full-pattern X-ray powder diffraction analyses. Nanocrystals diameters have been tuned in the range 2 ÷ 9 nm by a proper variation of Au/S molar ratio. The chemical composition of gold nanoparticles and their interaction with thiols have been investigated by X-ray photoelectron spectroscopy. In particular, the formation of networks has been observed with interconnected gold nanoparticles containing 1,4-benzenedimethanethiol as ligand.

No MeSH data available.


Scheme 1. Reaction scheme of the modified two-phase synthesis, based on the Brust's procedure, to obtain benzylthiol-capped gold nanoparticles (synthesis i, sample A).
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Figure 1: Scheme 1. Reaction scheme of the modified two-phase synthesis, based on the Brust's procedure, to obtain benzylthiol-capped gold nanoparticles (synthesis i, sample A).

Mentions: The reaction route leading to the benzylthiol-capped gold nanoparticles is shown in Scheme 1 (Figure 1, sample A). Using the Au/S ratio 0.75:1 as an example: HAuCl4·3H2O (0.350 g, 0.88 mmol) was dissolved in 30 ml of H2O and added to a solution of BzT (0.145 g, 1.17 mmol) in 80 ml of CH2Cl2, dichloromethane. The gold ions were transferred from the aqueous phase into CH2Cl2 upon addition of 1.6 g of tetraoctylammonium bromide (TOAB), and the mixture was vigorously stirred at RT. The gold was reduced upon addition of 22.3 ml of a 0.4 M aqueous solution of NaBH4, added over a period of 1 min to the vigorously stirring solution. The solution was left stirring for a further 3 h. Then, 50 ml of H2O and 50 ml of CH2Cl2 were added, and the organic phase was separated and dried over anhydrous sodium sulfate. The drying agent and any insoluble materials were removed by filtration and the solution was reduced to a solid, in vacuum. The dark brown residue was resuspended in methanol with the aid of sonication and stirred for 2 h. The suspension was filtered over Celite and subsequently washed with 400 ml of methanol and 400 ml of acetonitrile to remove any excess of arenethiolate, TOAB, and by-products. The product was obtained by washing off the Celite with CH2Cl2, then solvent was removed in vacuum, and the pure product was dried overnight. The yield for sample A1 was 87% (0.3045 g of obtained product).


Mono- and bi-functional arenethiols as surfactants for gold nanoparticles: synthesis and characterization.

Vitale F, Fratoddi I, Battocchio C, Piscopiello E, Tapfer L, Russo MV, Polzonetti G, Giannini C - Nanoscale Res Lett (2011)

Scheme 1. Reaction scheme of the modified two-phase synthesis, based on the Brust's procedure, to obtain benzylthiol-capped gold nanoparticles (synthesis i, sample A).
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC3211147&req=5

Figure 1: Scheme 1. Reaction scheme of the modified two-phase synthesis, based on the Brust's procedure, to obtain benzylthiol-capped gold nanoparticles (synthesis i, sample A).
Mentions: The reaction route leading to the benzylthiol-capped gold nanoparticles is shown in Scheme 1 (Figure 1, sample A). Using the Au/S ratio 0.75:1 as an example: HAuCl4·3H2O (0.350 g, 0.88 mmol) was dissolved in 30 ml of H2O and added to a solution of BzT (0.145 g, 1.17 mmol) in 80 ml of CH2Cl2, dichloromethane. The gold ions were transferred from the aqueous phase into CH2Cl2 upon addition of 1.6 g of tetraoctylammonium bromide (TOAB), and the mixture was vigorously stirred at RT. The gold was reduced upon addition of 22.3 ml of a 0.4 M aqueous solution of NaBH4, added over a period of 1 min to the vigorously stirring solution. The solution was left stirring for a further 3 h. Then, 50 ml of H2O and 50 ml of CH2Cl2 were added, and the organic phase was separated and dried over anhydrous sodium sulfate. The drying agent and any insoluble materials were removed by filtration and the solution was reduced to a solid, in vacuum. The dark brown residue was resuspended in methanol with the aid of sonication and stirred for 2 h. The suspension was filtered over Celite and subsequently washed with 400 ml of methanol and 400 ml of acetonitrile to remove any excess of arenethiolate, TOAB, and by-products. The product was obtained by washing off the Celite with CH2Cl2, then solvent was removed in vacuum, and the pure product was dried overnight. The yield for sample A1 was 87% (0.3045 g of obtained product).

Bottom Line: Stable gold nanoparticles stabilized by different mono and bi-functional arenethiols, namely, benzylthiol and 1,4-benzenedimethanethiol, have been prepared by using a modified Brust's two-phase synthesis.Nanocrystals diameters have been tuned in the range 2 ÷ 9 nm by a proper variation of Au/S molar ratio.In particular, the formation of networks has been observed with interconnected gold nanoparticles containing 1,4-benzenedimethanethiol as ligand.

View Article: PubMed Central - HTML - PubMed

Affiliation: ENEA (Italian National Agency for New Technologies, Energy and the Sustainable Economic Development), UTTMATB (Technical Unit of Materials Technologies - Brindisi), Brindisi Research Centre, S,S, 7 Appia km, 706, 72100 Brindisi, Italy. floriana.vitale@enea.it.

ABSTRACT
Stable gold nanoparticles stabilized by different mono and bi-functional arenethiols, namely, benzylthiol and 1,4-benzenedimethanethiol, have been prepared by using a modified Brust's two-phase synthesis. The size, shape, and crystalline structure of the gold nanoparticles have been determined by high-resolution electron microscopy and full-pattern X-ray powder diffraction analyses. Nanocrystals diameters have been tuned in the range 2 ÷ 9 nm by a proper variation of Au/S molar ratio. The chemical composition of gold nanoparticles and their interaction with thiols have been investigated by X-ray photoelectron spectroscopy. In particular, the formation of networks has been observed with interconnected gold nanoparticles containing 1,4-benzenedimethanethiol as ligand.

No MeSH data available.