孙海静,王贺,杨帅,付旭,战充波,张润佳,周欣,陈国亮,孙杰.氯化胆碱-尿素低共熔溶剂中锌的电沉积研究[J].表面技术,2022,51(2):268-275, 305.
SUN Hai-jing,WANG He,YANG Shuai,FU Xun,ZHAN Chong-bo,ZHANG Run-jia,ZHOU Xin,CHEN Guo-liang,SUN Jie.Electrodeposition Studies of Zinc in Choline Chloride-Urea Deep Eutectic Solvents[J].Surface Technology,2022,51(2):268-275, 305 |
| 氯化胆碱-尿素低共熔溶剂中锌的电沉积研究 |
| Electrodeposition Studies of Zinc in Choline Chloride-Urea Deep Eutectic Solvents |
| 投稿时间：2021-04-02 修订日期：2021-07-21 |
| DOI：10.16490/j.cnki.issn.1001-3660.2022.02.026 |
| 中文关键词: 低共熔溶剂 离子液体 电沉积 锌 形核机制 微观形貌 耐蚀性 |
| 英文关键词:deep eutectic solvent ionic liquid electrodeposition zinc nucleation mechanism micro-morphology corrosion resistance |
| 基金项目:辽宁省教育厅青年科技人才“育苗”项目(LG201928);辽宁省-沈阳材料科学国家研究中心联合研发基金项目(2019JH3/30100021) |
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| Author | Institution |
| SUN Hai-jing | School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang 110159, China |
| WANG He | School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang 110159, China |
| YANG Shuai | School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang 110159, China |
| FU Xun | School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang 110159, China |
| ZHAN Chong-bo | School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang 110159, China |
| ZHANG Run-jia | School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang 110159, China |
| ZHOU Xin | School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang 110159, China |
| CHEN Guo-liang | School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang 110159, China |
| SUN Jie | School of Environmental and Chemical Engineering, Shenyang Ligong University, Shenyang 110159, China |
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| 中文摘要: |
| 目的 研究锌在氯化胆碱-尿素低共熔溶剂(ChCl-Urea DES)中的电化学行为、电结晶机理、电沉积历程和耐蚀性。方法 采用循环伏安(CV)和计时电流技术(CA)，研究了锌在玻碳电极上的电化学行为和电结晶机理。采用扫描电子显微镜(SEM)和X射线衍射技术(XRD)对锌镀层的微观形貌和物相组成进行了表征。采用动电位极化曲线和电化学阻抗谱，对比研究了ChCl-Urea DES和水溶液中锌镀层的耐蚀性。结果 CV测试表明，在Zn(Ⅱ)的氧化还原过程中仅出现了一对氧化还原峰，这说明Zn(Ⅱ)在ChCl-Urea DES中为一步还原及氧化，且还原峰电位为‒1.207 V(vs. Ag)。不同扫描速度下的CV曲线表明，还原峰和氧化峰的峰值电位Ep和峰值电流Ip均随扫描速率v的变化而有规律的偏移，这符合不可逆电极反应的特征。对Ip和v1/2的关系进行了线性拟合，发现Ip与v1/2之间符合线性关系，故可认为Zn(Ⅱ)的还原反应是受扩散控制的，进一步计算出扩散系数DZn(Ⅱ)为6.67×10‒8 cm2/s。在–1.141 ~ –1.147 V下测定CA曲线，通过对比拟合CA曲线和理论曲线发现，Zn(Ⅱ)在ChCl-Urea DES中的形核方式不符合三维瞬时成核和三维连续成核，是一种具有两种形核方式特征的混合形核。SEM结果表明，不同沉积时间下锌镀层的微观形貌相差较大。随着沉积时间的增加，锌晶粒由细小、粒径均一的颗粒逐渐变化成大小颗粒交叠存在的六方形立体结构，然后又变成线状或棒状的结构，最终转变为六方形的片状晶粒。XRD表明，锌镀层由六方晶相的多晶锌构成。动电位极化曲线测试和电化学阻抗图谱表明，在没有任何添加剂的情况下，ChCl-Urea DES可获得与水溶液中耐蚀性相当的锌镀层，且ChCl-Urea DES中锌镀层的沉积速率略高于水溶液。结论 Zn(Ⅱ)在ChCl-Urea DES中的电沉积过程是受扩散控制的不可逆电极过程，形核方式不符合三维瞬时成核和三维连续成核，是一种具有两种形核方式特征的混合形核。锌镀层是由六方晶相的多晶锌构成的。在ChCl-Urea DES中可获得与水溶液中耐蚀性相当的锌镀层，且沉积速率略高于水溶液。 |
| 英文摘要: |
| The work aims to study the electrochemical behavior, electrocrystallization mechanism, electrodeposition process of zinc and corrosion resistance in the Choline Chloride-Urea deep eutectic solvent (ChCl-Urea DES). The electrochemical behavior and electrocrystallization mechanism of zinc on glass-carbon electrode were studied by Cyclic Voltammetry (CV) and chronoamperometry (CA). The micro-morphology and phase composition of zinc coatings were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). Comparative study of the corrosion resistance and electrochemical impedance spectroscopy of zinc plating in ChCl-Urea DES and aqueous solutions using dynamic potential polarization curves. The CV test shows that only one pair of redox peaks appears in the whole redox process, which indicates that Zn(II) is a one-step reduction and oxidation in ChCl-Urea DES, and the reduction peak potential (vs. Ag) is ‒1.207 V. The CV curves at different scan rates show that the peak potentials of both the reduction and oxidation peaks are regular with the scan rate v. The positive shift, and the regular decrease of both peak currents Ip with increasing scan rate v, are consistent with the irreversible electrode reaction. The relationship between Ip and v1/2 was fitted linearly, and the relationship between Ip and v1/2 was found to be good, so the reduction reaction of Zn(II) in ChCl-Urea DES could be considered to be controlled by diffusion, and the diffusion coefficient DZn(II) was further calculated to be 6.67×10‒8 cm2/s. The nucleation mode of Zn(II) in ChCl-Urea DES is neither three-dimensional instantaneous nucleation nor three-dimensional continuous nucleation, but a hybrid nucleation with two nucleation modes. The microscopic morphology of zinc coatings varies considerably depending on the deposition time. The XRD shows that the coating is composed of polycrystalline zinc with hexagonal crystalline phase. Potentiodynamic polarization curve test and electrochemical impedance spectroscopy showed that without any additives, the corrosion resistance of zinc coating in CHCl urea DES was equivalent to that in aqueous solution, and the formation rate of zinc coating in CHCl urea DES was slightly higher than that in aqueous solution. The electrodeposition of Zn(II) in ChCl-Urea DES is a diffusion-controlled irreversible electrode process with a nucleation mode that is neither three-dimensional instantaneous nor three-dimensional continuous, but rather a hybrid nucleation mode characterized by two nucleation modes. The zinc coating is composed of polycrystalline zinc with a hexagonal crystal phase. Comparable corrosion resistance can be obtained in ChCl-Urea DES as in aqueous solutions. |
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