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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

Experimental set-up of the microwave apparatus applied in synthesis of silver nanoparticles
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Related In: Results  -  Collection


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Fig1: Experimental set-up of the microwave apparatus applied in synthesis of silver nanoparticles

Mentions: The continuous synthesis of AgNP was realized in a set-up schematically shown in Fig. 1 using a commercial 2 kW single-mode microwave system (ERTEC, Poland) operating at 2.45 GHz frequency. Microwaves were transferred from the magnetron, through a microwave isolator and EH tuner, to the microwave applicator, i.e., a cavity with a PTFE tubular reactor (8 mm i.d., 42 mm length of irradiated section) mounted inside. The reactants mixture was fed continuously using a fine metering pump, at controlled flow rates of 0.318, 0.635, 1.27, and 2.5 dm3/h, to achieve the preset values of residence time (3, 6, 12 and 24 s) in the irradiation zone. The power was supplied continuously, and not intermittently as had been applied previously. Its value was controlled to achieve the preset outlet temperatures (in the range of 90–170 ± 1 °C depending on Ag precursor) and was measured by a thermocouple mounted at the reagents’ outlet. The diameter of tubing outside the reactor was reduced to 2-mm i.d. to speed up the reactants transport to a well-cooled collection cup.Fig. 1


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)

Experimental set-up of the microwave apparatus applied in synthesis of silver nanoparticles
© Copyright Policy - OpenAccess
Related In: Results  -  Collection

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

Fig1: Experimental set-up of the microwave apparatus applied in synthesis of silver nanoparticles
Mentions: The continuous synthesis of AgNP was realized in a set-up schematically shown in Fig. 1 using a commercial 2 kW single-mode microwave system (ERTEC, Poland) operating at 2.45 GHz frequency. Microwaves were transferred from the magnetron, through a microwave isolator and EH tuner, to the microwave applicator, i.e., a cavity with a PTFE tubular reactor (8 mm i.d., 42 mm length of irradiated section) mounted inside. The reactants mixture was fed continuously using a fine metering pump, at controlled flow rates of 0.318, 0.635, 1.27, and 2.5 dm3/h, to achieve the preset values of residence time (3, 6, 12 and 24 s) in the irradiation zone. The power was supplied continuously, and not intermittently as had been applied previously. Its value was controlled to achieve the preset outlet temperatures (in the range of 90–170 ± 1 °C depending on Ag precursor) and was measured by a thermocouple mounted at the reagents’ outlet. The diameter of tubing outside the reactor was reduced to 2-mm i.d. to speed up the reactants transport to a well-cooled collection cup.Fig. 1

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