Abstract
The electrodeposition of tin, bismuth, and tin–bismuth alloys from SnII and BiIII chlorometalate salts in the choline chloride/ethylene glycol (1:2 molar ratio) deep eutectic solvent was studied on glassy carbon and gold by cyclic voltammetry, rotating disc voltammetry, and chronoamperometry. The SnII‐containing electrolyte showed one voltammetric redox process corresponding to SnII/Sn0. The diffusion coefficient of [SnCl3]−, detected as the dominating species by Raman spectroscopy, was determined from Levich and Cottrell analyses. The BiIII‐containing electrolyte showed two voltammetric reduction processes, both attributed to BiIII/Bi0. Dimensionless current/time transients revealed that the electrodeposition of both Sn and Bi on glassy carbon proceeded by 3D‐progressive nucleation at a low overpotential and changed to instantaneous at higher overpotentials. The nucleation rate of Bi on glassy carbon was considerably smaller than that of Sn. Elemental Sn and Bi were electrodeposited on Au‐coated glass slides from their respective salt solutions, as were Sn–Bi alloys from a 2:1 SnII/BiIII solution. The biphasic Sn–Bi alloys changed from a Bi‐rich composition to a Sn‐rich composition by making the deposition potential more negative.
Highlights
Tin and its alloys are commonly used as lead-free soft solder layers in the mass production of electronic components.[1]
The electrochemistry of bismuth was previously studied in a Lewis acidic type 1 deep eutectic electrolyte of AlCl3/N-(n-butyl)pyridinium chloride containing 1 mm BiCl3.[30]. In this medium, the cathodic reduction of BiIII was shown to proceed via the low-valence state intermediate Bi53+
On the basis of the ratio of the anodic/cathodic charge, the coulombic efficiency for the SnII/0 reduction of all three cycles is around 92 %, if complete anodic stripping of Sn is assumed. This value is considerably higher than the 70 % efficiency for the electrodeposition of tin from the same tin salt on gold in a CH2F2 supercritical fluid.[5]
Summary
Tin and its alloys are commonly used as lead-free soft solder layers in the mass production of electronic components.[1]. The electrodeposition of p-block elements, including bismuth and tin, from tetrabutylammonium chlorometalate salts of the elements in dichloromethane and in supercritical fluids was reported.[4,5] These reagents are crystalline solids, easy to handle, and not highly water or oxygen sensitive. The electrodeposition of Sn from the type 1[10] deep eutectic solvents AlCl3/1-ethyl-3-methylimidazolium chloride[11] and ZnCl2/1-ethyl-3-methylimidazolium chloride[12] was previously reported For both studies, it was indicated that the speciation of SnII depended on the Lewis acidity of the electrolyte. The electrochemistry of bismuth was previously studied in a Lewis acidic type 1 deep eutectic electrolyte of AlCl3/N-(n-butyl)pyridinium chloride containing 1 mm BiCl3.[30] In this medium, the cathodic reduction of BiIII was shown to proceed via the low-valence state intermediate Bi53+. We describe the electrodeposition of Sn, Bi, and their alloys from their corresponding tetrabutylammonium chlorometalate salts in 12CE and characterization of the metallic deposits
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