Molecular Oxygen as Mediator in the Metal Nanoparticles’ Electrosynthesis in N,N-Dimethylformamide


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Abstract

Ultra-fine gold (<2 nm), silver (5 ± 2 nm), and palladium (<1–2 nm) nanoparticles stabilized in polyvinylpyrrolidone shell were synthesized in N,N-dimethylformamide, using molecular oxygen dissolved in the electrolyte as mediator, by the reduction of the metals’ ions and complexes at the controlled potential of the oxygen reduction to its radical-anion. Pd-nanoparticles showed high catalytic activity in the reactions of p-nitrophenol reduction and Suzuki cross-coupling. Long-term ageing of spherical Ag-nanoparticles for 60 days in the post- electrolysis solution resulted in their consolidation (up to 17 ± 5 nm; the average size of crystallites 7.5 (3) nm). Upon similar exposure of Au-nanoparticles for 15 days, V-shaped nanoparticles were formed (length 112 ± 53 nm, width 58 ± 22 nm, crystallites 20(2)–31(1) nm); upon the isolation, dispersing into ethanol, and exposure for 48 h, hexagonal nanoparticles (105 ± 29 nm) and polygons (56 ± 25 nm, crystallites 24(2)–51(1) nm; upon dispersing into water and exposure for 8 h, spherical nanoparticles (13 ± 8 nm, crystallites 7(1)–13.4(5) nm). Thus obtained nanoparticles are characterized by methods of cyclic voltammetry, dynamic light scattering, scanning and high resolution transmission electron microscopy, and X-ray powder diffraction.

About the authors

V. V. Yanilkin

Arbuzov Institute of Organic and Physical Chemistry

Author for correspondence.
Email: yanilkin@iopc.ru
Russian Federation, ul. Lenina 18, Kazan, 420008

N. V. Nastapova

Arbuzov Institute of Organic and Physical Chemistry

Email: yanilkin@iopc.ru
Russian Federation, ul. Lenina 18, Kazan, 420008

R. R. Fazleeva

Arbuzov Institute of Organic and Physical Chemistry

Email: yanilkin@iopc.ru
Russian Federation, ul. Lenina 18, Kazan, 420008

G. R. Nasretdinova

Arbuzov Institute of Organic and Physical Chemistry

Email: yanilkin@iopc.ru
Russian Federation, ul. Lenina 18, Kazan, 420008

E. D. Sultanova

Arbuzov Institute of Organic and Physical Chemistry

Email: yanilkin@iopc.ru
Russian Federation, ul. Lenina 18, Kazan, 420008

A. Yu. Ziganshina

Arbuzov Institute of Organic and Physical Chemistry

Email: yanilkin@iopc.ru
Russian Federation, ul. Lenina 18, Kazan, 420008

A. T. Gubaidullin

Arbuzov Institute of Organic and Physical Chemistry

Email: yanilkin@iopc.ru
Russian Federation, ul. Lenina 18, Kazan, 420008

A. I. Samigullina

Arbuzov Institute of Organic and Physical Chemistry

Email: yanilkin@iopc.ru
Russian Federation, ul. Lenina 18, Kazan, 420008

V. G. Evtyugin

Interdisciplinary Center “Analytical Microscopy,”

Email: yanilkin@iopc.ru
Russian Federation, ul. Kremlevskaya 18, Kazan, 420018

V. V. Vorob’ev

Interdisciplinary Center “Analytical Microscopy,”

Email: yanilkin@iopc.ru
Russian Federation, ul. Kremlevskaya 18, Kazan, 420018

Yu. N. Osin

Interdisciplinary Center “Analytical Microscopy,”

Email: yanilkin@iopc.ru
Russian Federation, ul. Kremlevskaya 18, Kazan, 420018

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