High Yield Synthesis of Pure Alkanethiolate-Capped Silver Nanoparticles

Abstract

One-phase, one-pot synthesis of Ag(0) nanoparticles capped with alkanethiolate molecules has been optimized to easily achieve a pure product in quantitative yield. We report the synthesis of dodecanethiolate-capped silver particles and the chemophysical, structural, and morphologic characterization performed by way of UV-vis, (1)H NMR, and X-ray photoelectron (XPS) spectroscopies, X-ray powder diffraction (XRD) and X-ray absorption fine structure analysis (XFAS), electron diffraction and high-resolution transmission electron microscopy (HR-TEM), and scanning and transmission electron microscopy (SEM and TEM). Depending on the molar ratio of the reagents (dodecylthiosulphate/Ag(+)), the mean Ag(0) particle size D(XRD) is tuned from 4 to 3 nm with a narrow size distribution. The particles are highly soluble, very stable in organic solvents (hexane, toluene, dichloromethane, etc.), and resistant to oxidation; the hexane solution after one year at room temperature does not show any precipitation or formation of oxidation byproducts.

Facile Synthesis of Silver Nanoparticles Using a Novel Benzenethiol Derivative: Addition Effect of Cationic Surfactants

“…Substantial research is underway to achieve monodispersity and stability of silver nanoparticles without perturbing the desired properties [14,15]. Alkane thiols are widely explored as reductive stabilizer of metal nanoparticles [16][17][18]. However, much attention has not been paid to the formation of AgNps using short-chain benzene thiol derivatives.…”

Formation of Ag(I) Thiolate‐layered Materials and Thiol‐capped Ag Nanoparticles by the Reduction of Silver Nitrate with Sodium Borohydride in the Presence of Thiol: Control of the Selectivity by the Ag+ to Thiol Mole Ratio

“…Especially, the metal to thiol mole ratio is frequently mentioned as an important factor to control the average mean size of thiol-capped metal NPs. 8,10 This suggests that the reduction/nucleation/growth of crystal and passivation processes compete in this reaction. We modified the one-phase method to prevent the initial formation of Ag(I) thiolatelayered material from the mixtures of AgNO 3 and thiols.…”

“…9 However, tetraalkylammonium salt is difficult to remove from thiol-capped Ag NPs and produces disorder in the self-assembly of the alkanethiolate onto the Ag NPs. 10 In order to these problems, a one-phase method for thiol-capped Au and Ag NPs has been explored. 11,12 In this method, sodium borohydride solution is added to the mixtures of AgNO 3 and thiols in ethanol to produce thiol-capped Ag NPs.…”

“…However, it has been reported that Ag(I) thiolate-layered material is generated as a byproduct in this reaction and that the workup process is time-consuming and gives a low yield. 10 It has been proposed that Ag(I) thiolate-layered material is formed when Ag + ions are exposed to thiols in the presence of highly polar solvents. 5 We decided to explore the experimental conditions for the generation of thiol-capped Ag NPs and Ag(I) thiolate-layered material in one-phase method.…”

“…The synthetic method of this work for the preparation of thiol-capped Ag NPs is more simple and has advantage over the methods of the two phase using tetraalkyl ammonium ion and one phase using alkylthiosulfate and ascorbic acid. 10,11 The dimension of the thiol-capped Ag NPs varied between 10 and 20 nm, as determined by high-resolution TEM and XRD. The distributions of thiol-capped Ag NPs and Ag(I) thiolate-layered materials were affected by the Ag + to thiol mole ratio and also by the nature of the thiol used.…”