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Ol. D. Zolotarenko, E. P. Rudakova, V. A. Lavrenko, N. Y. Akhanova, An. D. Zolotarenko, D. V. Shchur, Z. A. Matysina, M. T. Gabdullin, M. Ualkhanova, N. A. Gavrylyuk, O. D. Zolotarenko, M. V. Chymbai, and I. V. Zagorulko
Features of Electrochemical (Anode) Synthesis of Nickel and Copper Nanocrystalline Powder
0857–0873 (2022)
PACS numbers: 61.43.Gt, 68.70.+w, 81.05.Rm, 82.45.Cc, 82.45.Fk, 82.45.Gj, 82.45.Hk
Several methods of electrochemical synthesis of nickel (Ni) nanopowder are investigated. As shown, the most efficient and cost-effective method is the electrolysis of nickel sulphate (NiSO4) with appropriate impurities of nickel chloride II (NiCl2), boric acid (H3BO3) and thiourea ((NH4)2CS) using the P-5848 potentiostat as a power source. Ultrahigh-purity aluminium (Al) is used as the cathode, and a platinum plate is served as the anode. The synthesis is performed at temperatures of 45–65°C. After two hours of electrolysis at a current density of 1.0–3.3 A/dm2, nickel nanopowder with an average scale size (scaly particles) of 55 nm is obtained that is confirmed by high-resolution electron microscopy and Raman spectroscopy of high resolution, as well as modern adsorption methods. Electrochemical reactions take place at the cathode (Ni2+ + 2e = Ni) and at the anode (2H2O = O2↑ + 4H+ + 4e). Dendritic copper nanoparticles with high dispersion are also obtained with the possibility of regulating the synthesis of copper nanopowder with a bulk density of 0.4 g/cm3. For this purpose, electrolysis of an electrolyte solution with a relatively low copper content and a high sulphuric acid content is performed at a high cathode current density and a relatively low temperature of a copper sulphate solution (CuSO4). At the same time, a significant amount of copper sludge is removed from the cell by means of the periodic shocks, and the copper anode is shed to the bottom of the bath after 13.3 ampere-hours of current per 1 dm2 of the anode plane. The electrolysis process is continued at a current density of 15.6 A/dm2, and the direction of the current is changed every 20 minutes. In our case, the most appropriate mode of electrolysis is when the cathodes (copper plates) are placed at a distance of 0.8 cm from each other in the electrolyte with 45% H2SO4, 4% CuSO4 and 8% Na2SO4, and the current density at the cathode is of 15.3 A/dm2 at the temperature of 54°C and at the voltage between two copper plates of 0.775 V.
Key words: copper nanopowder, electrochemical synthesis, electrolysis, dendritic copper, nickel nanopowder, sulphuric acid (H2SO4), aluminium (Al) cathode, platinum (Pt) anode, potentiostat, nickel chloride II (NiCl2), boric acid (H3BO3), thiourea (NH4(NH4)2CS), sodium sulphate (Na2SO4), copper sulphate (CuSO4), nickel sulphate (NiSO4).
https://doi.org/10.15407/nnn.20.04.857
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