| SUN Hai-jing,YANG Shuai,DING Ming-yu,SUN Jie.Electrochemical Behavior of Copper Electroplating Progress in ChCl-OxA Eutectic Solvent[J],50(11):313-320 |
| Electrochemical Behavior of Copper Electroplating Progress in ChCl-OxA Eutectic Solvent |
| Received:May 29, 2020 Revised:August 21, 2020 |
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| DOI：10.16490/j.cnki.issn.1001-3660.2021.11.033 |
| KeyWord:deep eutectic solvent oxalic acid copper electrodeposition electrochemical behavior nucleation mechanism |
| Author | Institution |
| SUN Hai-jing |
School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang , China |
| YANG Shuai |
School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang , China |
| DING Ming-yu |
School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang , China |
| SUN Jie |
School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang , China |
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| Abstract: |
| The work aims to study the electrochemical behavior, electro-crystallization mechanism and electrodeposition process of copper in the Choline Chloride-Oxalic Acid (ChCl-OxA) eutectic solvent system. The electrochemical behavior of copper in the ChCl-OxA eutectic solvent system was studied by cyclic voltammetry (CV). The electro-crystallization mechanism of copper at different potential steps was investigated by chronoamperometry (CA). The micro-morphology and phase composition of copper coatings were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The electrochemical stability window of the ChCl-OxA eutectic solvent was 2.10 V. The copper ion was reduced to copper after two successive electrochemical steps, and the two reduction peak potentials (vs. Ag) were respectively 0.686 V (Cu2+/Cu+) and 0.365 V (Cu+/Cu0). The reduction potentials were all located in the positive potential region, indicating that the copper ion had strong reducibility. The cyclic voltammetry curves of different scanning velocities showed that Eptrended to shift to negative value when the scanning velocities were increasing, which conforms to the characteristics of irreversible reactions. Therefore, it could be judged that Cu(Ⅱ) in the ChCl-OxA eutectic solvent was the process of irreversible reactions. The relationship between Ipand v1/2 was linearly fitted, and it was found that the relationship between Ipand v1/2 was linear. Therefore, the two reduction reactions of copper ions were controlled by diffusion. After calculation, the diffusion coefficient of DCu(Ⅱ), DCu(Ⅰ)were 7.27×10–9cm2/sand 5.70×10–9cm2/s. The third oxidation peak was found in the oxidation process, which was speculated to be the oxidation process of chloride ion (at a higher concentration). The chronoamperometry measured at –0.60~ –0.68 V showed that the electro-crystallization process of Cu(Ⅱ) in the ChCl-OxA system was found to conform to the Scharifker-Hill three- dimensional nucleation model through the comparison between the chronoelectric curve and the theoretical curve. The results for micro-morphologies showed that different micro-morphologies could be formed, such as spherical shape, short bar shape, and square shape. Uniform and fine copper coatings could be obtained in the ChCl-OxA system. The results for phase composition showed that copper coating consisted of Face-Centered Cubic (FCC) phase and the optimal crystal surface was (111). The electrodepositing process of copper(Ⅱ) in the ChCl-OxA eutectic solvent is an irreversible electrochemical process controlled by diffusion, and the nucleation mechanism is the three-dimensional instantaneous nucleation. The fine and uniform nanocrystalline copper coating with an average particle size of 45.34 nm can be obtained. |
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