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Rapid continuous microwave-assisted synthesis of silver nanoparticles to achieve very high productivity and full yield: from mechanistic study to optimal fabrication strategy.

Dzido G, Markowski P, Małachowska-Jutsz A, Prusik K, Jarzębski AB - J Nanopart Res (2015)

Bottom Line: Systematic studies of silver nanoparticle synthesis in a continuous-flow single-mode microwave reactor using polyol process were performed, revealing that the synthesis is exceptionally effective to give very small metal particles at full reaction yield and very high productivity.Owing to its much higher reactivity, silver acetate was shown to be far superior substrate for the synthesis of small (10-20 nm) spherical silver nanoparticles within a few seconds.The performed studies indicate an optimal strategy for the high-yield fabrication of metal particles using polyol method.

View Article: PubMed Central - PubMed

Affiliation: Department of Chemical Engineering and Process Design, Faculty of Chemistry, Silesian University of Technology, Ks. M. Strzody 7, 44-100 Gliwice, Poland.

ABSTRACT

Systematic studies of silver nanoparticle synthesis in a continuous-flow single-mode microwave reactor using polyol process were performed, revealing that the synthesis is exceptionally effective to give very small metal particles at full reaction yield and very high productivity. Inlet concentration of silver nitrate or silver acetate, applied as metal precursors, varied between 10 and 50 mM, and flow rates ranged from 0.635 to 2.5 dm(3)/h, to give 3-24 s reaction time. Owing to its much higher reactivity, silver acetate was shown to be far superior substrate for the synthesis of small (10-20 nm) spherical silver nanoparticles within a few seconds. Its restricted solubility in ethylene glycol, applied as the solvent and reducing agent, appeared to be vital for effective separation of the stage of particle growth from its nucleation to enable rapid synthesis of small particles in a highly loaded system. This was not possible to obtain using silver nitrate. All the observations could perfectly be explained by a classical LaMer-Dinegar model of NPs' formation, but taking into account also nonisothermal character of the continuous-flow process and acetate dissolution in the reaction system. The performed studies indicate an optimal strategy for the high-yield fabrication of metal particles using polyol method.

No MeSH data available.


Related in: MedlinePlus

Voltamograms of liquids with specified concentrations of silver ions
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Fig2: Voltamograms of liquids with specified concentrations of silver ions

Mentions: DPV method applied to determine silver ions content in the suspension on the reactor’s exit made use of the selective ion oxidation at the working electrode (glassy carbon), with silver/silver chloride (Ag/AgCl) and platinum electrode being a reference and an auxiliary electrode, respectively. A mixture of Britton-Robinson buffer (pH 4.10) with ethylene glycol (99/1, v/v) was used as a supporting electrolyte. Figure 2 shows the voltamograms obtained from the liquids with a specified concentration of silver ions. The areas under the curves are proportional to the concentration of Ag+ ions. In this way, a calibration curve could be developed, to be later applied to determine Ag+, and hence Ag0 content, to give the reaction yield. The accuracy of analytic determinations ranged from 0.4 to 3.6 %.Fig. 2


Rapid continuous microwave-assisted synthesis of silver nanoparticles to achieve very high productivity and full yield: from mechanistic study to optimal fabrication strategy.

Dzido G, Markowski P, Małachowska-Jutsz A, Prusik K, Jarzębski AB - J Nanopart Res (2015)

Voltamograms of liquids with specified concentrations of silver ions
© Copyright Policy - OpenAccess
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4300398&req=5

Fig2: Voltamograms of liquids with specified concentrations of silver ions
Mentions: DPV method applied to determine silver ions content in the suspension on the reactor’s exit made use of the selective ion oxidation at the working electrode (glassy carbon), with silver/silver chloride (Ag/AgCl) and platinum electrode being a reference and an auxiliary electrode, respectively. A mixture of Britton-Robinson buffer (pH 4.10) with ethylene glycol (99/1, v/v) was used as a supporting electrolyte. Figure 2 shows the voltamograms obtained from the liquids with a specified concentration of silver ions. The areas under the curves are proportional to the concentration of Ag+ ions. In this way, a calibration curve could be developed, to be later applied to determine Ag+, and hence Ag0 content, to give the reaction yield. The accuracy of analytic determinations ranged from 0.4 to 3.6 %.Fig. 2

Bottom Line: Systematic studies of silver nanoparticle synthesis in a continuous-flow single-mode microwave reactor using polyol process were performed, revealing that the synthesis is exceptionally effective to give very small metal particles at full reaction yield and very high productivity.Owing to its much higher reactivity, silver acetate was shown to be far superior substrate for the synthesis of small (10-20 nm) spherical silver nanoparticles within a few seconds.The performed studies indicate an optimal strategy for the high-yield fabrication of metal particles using polyol method.

View Article: PubMed Central - PubMed

Affiliation: Department of Chemical Engineering and Process Design, Faculty of Chemistry, Silesian University of Technology, Ks. M. Strzody 7, 44-100 Gliwice, Poland.

ABSTRACT

Systematic studies of silver nanoparticle synthesis in a continuous-flow single-mode microwave reactor using polyol process were performed, revealing that the synthesis is exceptionally effective to give very small metal particles at full reaction yield and very high productivity. Inlet concentration of silver nitrate or silver acetate, applied as metal precursors, varied between 10 and 50 mM, and flow rates ranged from 0.635 to 2.5 dm(3)/h, to give 3-24 s reaction time. Owing to its much higher reactivity, silver acetate was shown to be far superior substrate for the synthesis of small (10-20 nm) spherical silver nanoparticles within a few seconds. Its restricted solubility in ethylene glycol, applied as the solvent and reducing agent, appeared to be vital for effective separation of the stage of particle growth from its nucleation to enable rapid synthesis of small particles in a highly loaded system. This was not possible to obtain using silver nitrate. All the observations could perfectly be explained by a classical LaMer-Dinegar model of NPs' formation, but taking into account also nonisothermal character of the continuous-flow process and acetate dissolution in the reaction system. The performed studies indicate an optimal strategy for the high-yield fabrication of metal particles using polyol method.

No MeSH data available.


Related in: MedlinePlus