Ultrasound-Assisted Hydrazine Reduction Method for the Preparation of Nickel Nanoparticles, Physicochemical Characterization and Catalytic Application in Suzuki-Miyaura Cross-Coupling Reaction

Adél Anna Ádám; Márton Szabados; Gábor Varga; Ádám Papp; Katalin Musza; Zoltán Kónya; Ákos Kukovecz; Pál Sipos; István Pálinkó

doi:10.3390/nano10040632

Ultrasound-Assisted Hydrazine Reduction Method for the Preparation of Nickel Nanoparticles, Physicochemical Characterization and Catalytic Application in Suzuki-Miyaura Cross-Coupling Reaction

Nanomaterials (Basel). 2020 Mar 28;10(4):632. doi: 10.3390/nano10040632.

Authors

Adél Anna Ádám^{1

2}, Márton Szabados^{1

2}, Gábor Varga^{1

2}, Ádám Papp², Katalin Musza^{1

2}, Zoltán Kónya^{3

4}, Ákos Kukovecz³, Pál Sipos^{2

5}, István Pálinkó^{1

2}

Affiliations

¹ Department of Organic Chemistry, University of Szeged, Dóm tér 8, H-6720 Szeged, Hungary.
² Material and Solution Structure Research Group, and Interdisciplinary Excellence Centre, Institute of Chemistry, University of Szeged, Aradi Vértanúk tere 1, H-6720 Szeged, Hungary.
³ Department of Applied and Environmental Chemistry, University of Szeged, Rerrich B. tér 1, H-6720 Szeged, Hungary.
⁴ MTA-SZTE Reaction Kinetics and Surface Chemistry Research Group, Rerrich B tér 1, H-6720 Szeged, Hungary.
⁵ Department of Inorganic and Analytical Chemistry, University of Szeged, Dóm tér 7, H-6720 Szeged, Hungary.

Abstract

In the experimental work leading to this contribution, the parameters of the ultrasound treatment (temperature, output power, emission periodicity) were varied to learn about the effects of the sonication on the crystallization of Ni nanoparticles during the hydrazine reduction technique. The solids were studied in detail by X-ray diffractometry, dynamic light scattering, thermogravimetry, specific surface area, pore size analysis, temperature-programmed CO₂/NH₃ desorption and scanning electron microscopy. It was found that the thermal behaviour, specific surface area, total pore volume and the acid-base character of the solids were mainly determined by the amount of the nickel hydroxide residues. The highest total acidity was recorded over the solid under low-power (30 W) continuous ultrasonic treatment. The catalytic behaviour of the nanoparticles was tested in a Suzuki-Miyaura cross-coupling reaction over five samples prepared in the conventional as well as the ultrasonic ways. The ultrasonically prepared catalysts usually performed better, and the highest catalytic activity was measured over the nanoparticles prepared under low-power (30 W) continuous sonication.

Keywords: acid-base properties; activities in the Suzuki-Miyaura cross-coupling reaction; nickel nanoparticles; sonocrystallization; structural and morphology characterization.