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The Anodic Behaviour of Bulk Copper in Ethaline and 1-Butyl-3-Methylimidazolium Chloride

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The Anodic Behaviour of Bulk Copper in Ethaline and 1-Butyl-3-Methylimidazolium Chloride applied sciences Article The Anodic Behaviour of Bulk Copper in Ethaline and 1-Butyl-3-Methylimidazolium Chloride Wrya O. Karim 1,2, Shujahadeen B. Aziz 3,4,* , Mohamed. A. Brza 1,5, Ranjdar M. Abdullah 1 and Mohd. F. Z. Kadir 6 1 Department of Chemistry, College of Science, University of Sulaimani, Qlyasan Street, Sulaimani 46001, Kurdistan Regional Government-Iraq; [email protected] (W.O.K.); [email protected] (M.A.B.); [email protected] (R.M.A.) 2 Department of Chemistry, University of Leicester, Leicester LE1 7RH, UK 3 Prof. Hameeds Advanced Polymeric Materials Research Lab., Department of Physics, College of Science, University of Sulaimani, Qlyasan Street, Sulaimani 46001, Kurdistan Regional Government-Iraq 4 Komar Research Center (KRC), Komar University of Science and Technology, Sulaimani 46001, Kurdistan Regional Government-Iraq 5 Faculty of Engineering, International Islamic University of Malaysia, Kuala Lumpur, Gombak 53100, Malaysia 6 Centre for Foundation Studies in Science, University of Malaya, Kuala Lumpur 50603, Malaysia; [email protected] * Correspondence: [email protected] or [email protected] Received: 23 August 2019; Accepted: 11 October 2019; Published: 17 October 2019 Abstract: The anodic dissolution of bulk metallic copper was conducted in ionic liquids (ILs)—a deep eutectic solvent (DES) ((CH3)3NC2H4OH) comprised of a 1:2 molar ratio mixture of choline chloride Cl (ChCl), and ethylene glycol (EG)—and imidazolium-based ILs, such as C4mimCl, using electrochemical techniques, such as cyclic voltammetry, anodic linear sweep voltammetry, and chronopotentiometry.To investigate the electrochemical dissolution mechanism, electrochemical impedance spectroscopy (EIS) was used. In addition to spectroscopic techniques, for instance, UV-visible spectroscopy, microscopic techniques, such as atomic force microscopy (AFM), were used. The significant industrial importance of metallic copper has motivated several research groups to deal with such an invaluable metal. It was confirmed that the speciation of dissolved copper from 2 the bulk phase at the interface region is [CuCl3]− and [CuCl4] − in such chloride-rich media, and the EG determine the structure of the interfacial region in the electrochemical dissolution process. A super-saturated solution was produced at the electrode/solution interface and CuCl2 was deposited on the metal surface. Keywords: copper electrodissolution; (choline chloride-based IL) ethaline eutectic solvent; butyl-3-methylimidazolium chloride ionic liquid; linear sweep voltammetry; electrochemical impedance spectroscopy; electropolishing 1. Introduction The electrodeposition of copper has been investigated for a variety of applications, and the anodic dissolution of metallic copper has been thoroughly studied in ionic liquid (IL) and deep eutectic solvent (DES) media [1–10]. Previously, the anodic dissolution of metallic copper has been thoroughly examined in aqueous media [11–13]. This invaluable metal has wide applications, including electronics, decorating, pre-coating, and electro-catalysis [14–19]. Appl. Sci. 2019, 9, 4401; doi:10.3390/app9204401 www.mdpi.com/journal/applsci Appl. Sci. 2019, 9, 4401 2 of 15 Gu et al. studied electrodeposition and the corrosion behaviour of copper in a choline chloride-ethylene glycol DES. In the electrodeposition process, a rough surface was obtained with the addition of ethylene diamine; the corrosion decreased and a relatively uniform surface was gained [5]. Many research groups have tried to deal with the physical properties of ethaline (choline chloride–ethylene glycol). it was found that the mass transport could be increased with an increasing temperature; when the temperature was increased to 50 ◦C, the viscosity decreased by 65% [7]. Concerning the physical properties of the electrolyte, such as conductivity and viscosity, it was found that it is insensitive to metal-salt addition but strongly temperature dependent [9]. The speciation of 2 2 copper is well-defined in choline-based DESs. It was determined to be [CuCl3] − and [CuCl4] − for Cu(I) and Cu(II), respectively [20]. The dissolution of bulk copper was studied previously in these media, in the present work attempt was directed to deal with copper in more detail [21]. Deep eutectic solvents (DESs) are attracting significant research interest as electrochemical media, especially for electrodeposition, as they share many of the useful properties of ILs, but are typically greener and cheaper [22]. The influence of water and the changing potential on the interfacial region between a platinum electrode and a DES were studied. It was found that the nanostructural feature of interface decreased in the presence of small amount of water and was also strongly potential dependent [23]. The aim of this work is to investigate the dissolution mechanism of copper in a DES and its comparable IL and compare it to the aqueous system. This is important for counter-electrode processes during electrodeposition, for electropolishing, and also to understand whether metallic copper corrodes in the DESs. 2. Experimental The DES was prepared by mixing choline chloride (ChCl) (Aldrich, 99%) and EG (Aldrich, >99%) in a stoichiometric molar ratio of 1:2 (ChCl:EG). Then, it was heated to 60◦C with continuous stirring until a clear liquid was produced. The IL one was purchased from (Aldrich, 99%). The 1-Butyl-3-methylimidazolium chloride, (C4mim)(Cl), was dried under vacuum before use, but had a water content of ca. 0.1 wt.% (thermogravimetric analysis, Mettler Toledo TGA/DSC1 STARe system) which enabled it to be liquid at 70◦C.The copper wire was purchased from Alfa Aesar (99.9% purity). Regarding electrochemical measurements, both cyclic voltammetry and linear sweep voltammetry were conducted by means of both stationary and rotating disk electrodes. The galvanostatic and the AC impedance were performed using an Autolab PGSTAT 12: controlling by GPES software and then fitting with an FRA impedance module. The impedance spectra acquisition was in the frequency range of 1–65,000 Hz with small amplitude of 10 mV of the AC signal. All electrochemical measurements were carried out in a three electrode cell system involving a 1 mm diameter metal disc Cu working electrode, sealed in glass; a platinum flag (1 cm2 area) as a counter electrode; and Ag/AgCl (0.1 M in 1:2ChCl:EG) as the reference electrode. All measurements are performed at 20◦C and 70◦C at a 5 mV s 1 scan rate except for the determination of time considered necessary for copper electrode to · − reach passivation. The sweep rate was changed from 5 up to 50.5 mV s 1. · − The UV spectra were recorded by means of a Shimadzu model Uv-1601 spectrophotometer with a cell path length of 10 mm. The morphological examinations were conducted using atomic force microscopy (AFM). The acquisition of images was by means of a Digital Instruments Nanoscope IV Dimension 300 (Veeco) atomic force microscope with a 100 mm scanning head contact mode. The controlling software was Nanoscope version 6.13 during image acquisition in air. Appl. Sci. 2019, 9, 4401 3 of 15 3. Results and Discussion 3.1. Anodic Dissolution Mechanism Cyclic and Linear Sweep Voltammetry Figure1a exhibits the cyclic voltammetric response a of metallic, copper disc electrode in choline chloride-based IL at 20 ◦C. Within the anodic potential range, two oxidation processes can be clearly seen. The anodic current begins to increase at 0.3 V, peaking at ca. 0 V. The current sharply drops Appl. Sci. 2019, 9, x FOR PEER REVIEW − 3 of 14 in a manner which is a characteristic of a quasi-passivation process. This might be due primarily to presencepresence of of EG, EG, and and partly, partly, the the chloride chloride ion. ion. The The second second anodic anodic current current rises rises to a to peak a peak at +0.3 at + V0.3 and V and fallsfalls down down to to a a steady steady state state cu currentrrent of of approximately approximately 23 23 mA·cm mA cm−2. The2. The second second anodic anodic peak peak beyond beyond · − +0.25+0.25 V V could could be be linked linked to to extra extra oxidation oxidation of ofcopper copper from from Cu(I) Cu(I) to Cu(II). to Cu(II). The The other other ting ting peaks peaks are are artefactsartefacts that that might might be be linked linked to to complexity complexity of of di dissolutionssolution process process of of bulk bulk copper copper metal metal within within such such a aviscous viscous liquid.liquid. 50 40 a b 40 30 ) ) -2 -2 30 20 20 ( mA cm ( mA ( mA cm ( mA j 10 j 10 0 0 -10 -10 -1.0 -0.5 0.0 0.5 1.0 1.5 -1.0 -0.5 0.0 0.5 1.0 1.5 E (V) vs. Ag/AgCl E (V) vs. Ag/AgCl FigureFigure 1. 1. CyclicCyclic voltammetric voltammetric responses responses of ofa Cu a Cu disc disc (solid (solid line) line) and and 0.1 0.1M CuCl M CuCl2·2H22HO (dashedO (dashed line) line) 2· 2 inin choline choline chloride-based chloride-based ionic ionic liquid liquid (IL) (IL) on ona platinum a platinum electrode electrode at 20 at °C 20 (◦aC(), anda), and a Cu a Cudisc disc (solid (solid line)line) and and 0.2 0.2 M M CuCl CuCl2·2H2H2O Oin inimidazolium-based imidazolium-based IL (dashed IL (dashed line) line) at 70 at °C 70 (bC(), allb), at all a atsweep a sweep rate rateof of 2· 2 ◦ 55 mV·s mV −s1. 1. · − OnOn the the cathodic cathodic scan, scan, the the current current was was approximately approximately constant constant until until ca. ca.0.2 V, 0.2 when V, when a noisy a noisy phenomenonphenomenon occurred occurred at at the the same same potential potential that that pass passivationivation film film formation formation occurred: occurred: on the on reversed the reversed sweep.sweep.
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