Application of Square-Wave Stripping Voltammetry for the Analysis of Electrodeposits Based on Lead-Bismuth

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Resumo

The possibility of targeted electrodeposition of coatings in the lead-bismuth binary system is discussed. The analysis of metal content in electrodeposits was performed using square-wave stripping voltammetry of solutions simultaneously containing lead and bismuth. The obtained results were supported by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and powder X-ray diffraction analysis. The electrodeposition conditions of obtaining Pb7Bi3 ε-phase, which is promising for the application in superconducting microelectronics, were found.

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Sobre autores

I. Voronin

Lomonosov Moscow State University

Email: kirill@inorg.chem.msu.ru
Rússia, Moscow

S. Sotnichuk

Lomonosov Moscow State University

Email: kirill@inorg.chem.msu.ru
Rússia, Moscow

I. Kolesnik

Lomonosov Moscow State University; Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: kirill@inorg.chem.msu.ru
Rússia, Moscow; Moscow

K. Napolsky

Lomonosov Moscow State University

Autor responsável pela correspondência
Email: kirill@inorg.chem.msu.ru
Rússia, Moscow

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2. Fig. 1. Types of voltammetryograms as a function of the duration of the electroconcentration stage, s: 60 (a), 150 (b), 300 (c)

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3. Fig. 2. Voltammetryograms obtained during the study of calibration solutions of different concentrations (a). Graduation dependences for bismuth concentration 2.5-9 μM and lead concentration 7-25 μM (b). The error of peak area determination does not exceed 3%. In the captions to the dependences: S - area under the peak of anodic dissolution of metal, normalised by the rate of potential sweep, C - metal concentration

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4. Fig. 3. Cyclic voltammetry obtained for Au/Si electrode in an electrolyte containing, mM: 18.4 Pb(NO3)2, 0.8 Bi(NO3)3, 24.6 EDTA-Na2 and 625 NaNO3. The potential sweep speed is 50 mV/s

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5. Fig. 4. Mole fraction of bismuth in the electrolytic precipitate as a function of the mole fraction of bismuth in the total lead and bismuth content in the electrolyte, determined by PCMA and IVA methods. The results of approximation according to equation (2) are presented by the dotted line

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6. Fig. 5. Phase diagram for Pb-Bi alloys (reproduced from [7]) and experimental points corresponding to the composition of precipitates obtained during this work. The composition of precipitates was determined by inversion voltammetry

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7. Fig. 6. Scanning electron microscopy images for samples containing Bi, at. %: 77 (a), 33 (b) and 22 (c)

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8. Fig. 7. SEM image of the surface of the precipitate containing 27 at. % Bi, formed from the electrolyte composition, mM: 18.4 Pb(NO3)2, 0.8 Bi(NO3)3, 24.6 EDTA-Na2 and 625 NaNO3, on a copper substrate at a deposition potential of -1.0 V (a); and its X-ray image (b)

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