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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

XRD patterns of Ag NPs: a sample T14, b sample T9, c silver reference (ICSD card 01-071-6549)
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Fig8: XRD patterns of Ag NPs: a sample T14, b sample T9, c silver reference (ICSD card 01-071-6549)

Mentions: In this respect, worth noting are the pronounced diffraction peaks clearly seen in XRD patterns of T9 and T14 (cf. Fig. 8). The results indicate the crystalline structure of the Ag NPs with observed peaks closely matching those of pure silver (ICSD card 01-071-6549, reflections at 2θ = 38.12°, 44.31°, 64.45°, 77.41°, and 81.56°). They correspond, respectively, to the (1 1 1), (2 0 0), (2 2 0), (3 1 1), and (2 2 2) crystallographic planes of face-centered cubic Ag crystals. The size of crystalline particles calculated from Scherrer equation (d = Kλ/βcos(θ) where d is the average crystal grain size, λ is the wavelength of the X-rays, β is the broadening of reflection due to crystallite size effect, θ is the diffraction angle of a particular reflection, K = 0.9), was of an average diameter in the range of about 13–15 nm for both T9 and T14 sample. These estimates are in good agreement with the maxima of PSDs obtained from TEM and DLS analyses of T14 (cf. Figs. 5, 7).Fig. 8


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)

XRD patterns of Ag NPs: a sample T14, b sample T9, c silver reference (ICSD card 01-071-6549)
© Copyright Policy - OpenAccess
Related In: Results  -  Collection

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

Fig8: XRD patterns of Ag NPs: a sample T14, b sample T9, c silver reference (ICSD card 01-071-6549)
Mentions: In this respect, worth noting are the pronounced diffraction peaks clearly seen in XRD patterns of T9 and T14 (cf. Fig. 8). The results indicate the crystalline structure of the Ag NPs with observed peaks closely matching those of pure silver (ICSD card 01-071-6549, reflections at 2θ = 38.12°, 44.31°, 64.45°, 77.41°, and 81.56°). They correspond, respectively, to the (1 1 1), (2 0 0), (2 2 0), (3 1 1), and (2 2 2) crystallographic planes of face-centered cubic Ag crystals. The size of crystalline particles calculated from Scherrer equation (d = Kλ/βcos(θ) where d is the average crystal grain size, λ is the wavelength of the X-rays, β is the broadening of reflection due to crystallite size effect, θ is the diffraction angle of a particular reflection, K = 0.9), was of an average diameter in the range of about 13–15 nm for both T9 and T14 sample. These estimates are in good agreement with the maxima of PSDs obtained from TEM and DLS analyses of T14 (cf. Figs. 5, 7).Fig. 8

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