尹志芳,刘卫,杨泱,陈星,廖惠怡.一步电沉积法制备Ni-Mo-Nd/NF复合电极及其析氢性能研究[J].表面技术,2024,53(6):214-221.
YIN Zhifang,LIU Wei,YANG Yang,CHEN Xing,LIAO Huiyi.One-step Electrodeposition of Ni-Mo-Nd/NF Electrodes and Their Hydrogen Evolution Performance[J].Surface Technology,2024,53(6):214-221 |
| 一步电沉积法制备Ni-Mo-Nd/NF复合电极及其析氢性能研究 |
| One-step Electrodeposition of Ni-Mo-Nd/NF Electrodes and Their Hydrogen Evolution Performance |
| 投稿时间：2023-02-10 修订日期：2023-07-08 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.06.020 |
| 中文关键词: 一步电沉积 Ni-Mo-Nd/NF 析氢反应 泡沫镍 |
| 英文关键词:one-step electrodeposition Ni-Mo-Nd/NF hydrogen evolution reaction nickel foam |
| 基金项目:益阳市银城科技人才托举工程项目(益人才办(2022)6号) |
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| Author | Institution |
| YIN Zhifang | College of Materials and Chemical Engineering, Hunan City University, Hunan Yiyang 413000, China |
| LIU Wei | College of Materials and Chemical Engineering, Hunan City University, Hunan Yiyang 413000, China;Yiyang Hongyuan Rare Earth Co., Ltd., Hunan Yiyang 413001, China |
| YANG Yang | Yiyang Hongyuan Rare Earth Co., Ltd., Hunan Yiyang 413001, China |
| CHEN Xing | Yiyang Hongyuan Rare Earth Co., Ltd., Hunan Yiyang 413001, China |
| LIAO Huiyi | College of Materials and Chemical Engineering, Hunan City University, Hunan Yiyang 413000, China |
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| 中文摘要: |
| 目的 采用一步恒电流沉积法在泡沫镍基底上制备出镍-钼-钕三元析氢电极，提高碱性条件下的析氢性能。方法 使用电化学工作站研究工艺参数对Ni-Mo-Nd/NF析氢电极性能的影响，同时制备Ni-Mo/NF析氢电极，使用扫描电镜(SEM)、X射线衍射分析仪(XRD)、能谱仪(EDS)和X射线光电子能谱(XPS)对合金镀层表面形貌、相结构、元素含量及成键状态进行表征。通过线性扫描伏安法(LSV)、循环伏安法(CV)及电化学阻抗技术(EIS)测试电极析氢性能。结果 最佳工艺参数为:pH=4.5，电流密度30 mA/cm2，沉积时间60 min，温度30 ℃。在1.0 mol/L KOH溶液中，Ni-Mo-Nd/NF电极在10 mA/cm2下的析氢过电位仅为73 mV，Tafel斜率为147 mV/dec，表明析氢反应机理遵循典型的Volmer-Heyrovsky步骤。此外，Ni-Mo-Nd/NF电极在长时电解24 h时电流密度保持稳定，2 000次循环伏安测试后，催化剂的活性衰减微小。结论 稀土元素Nd的掺杂，能够细化电极表面的球形颗粒并提高电极表面粗糙度，从而提升电极的比表面积，为析氢反应提供更多的活性位点，利于析氢反应效率的提高。由于三元合金的协同作用，与二元合金Ni-Mo/NF相比，Ni-Mo-Nd/NF三元合金电极显示出更优异的HER催化性能。 |
| 英文摘要: |
| Finding non-precious metal hydrogen evolution reaction (HER) electrocatalysts with high efficiency and low cost is a great challenge. One-step galvanostatic deposition method was used to prepare nickel-molybdenum-neodymium ternary hydrogen evolution electrode on nickel foam substrate and improve its hydrogen evolution performance under alkaline condition. The effects of process parameters on the performance of Ni-Mo-Nd/NF hydrogen evolution electrode were studied by electrochemical workstation, and the Ni-Mo/NF hydrogen evolution electrode was prepared simultaneously. Scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) were used to characterize the surface morphology, phase structure, element content and bonding state of the alloy coating. The hydrogen evolution performance was measured by linear sweep voltammetry (LSV), Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Throughout the electrodeposition experiment, the NF (10 mm×10 mm×0.3 mm), the graphite plate (20 mm×20 mm×5 mm) and the saturated calomel electrode (SCE) were used as working, counter, and reference electrodes, respectively. The results showed that the optimum process parameters were pH=4.5, current density 30 mA/cm2, deposition time 60 min and temperature 30 ℃. After electrochemical deposition, the surface of Ni-Mo/NF alloy coating presented cellular structure with relatively coarse particles. With the introduction of Nd element, the surface particles of Ni-Mo-Nd/NF coating increased, and the fine particles grew directly on the conductive substrate, which increased the specific surface area of the coating, provided more the active sites of hydrogen evolution, and helped to improve hydrogen evolution efficiency. According to Mapping, Ni, Mo and Nd were evenly distributed on the coating, and their mass percentages were 57.0%, 29.9% and 13.1% respectively. It could be seen from XRD that with the doping of Mo and Nd, the peak appeared negative shift, which might be due to the solid solution of Mo and Nd in Ni, and the Ni atom was replaced by the Nd atom with a larger radius, and the lattice changed. Ni 2p, Mo 3d and Nd 3d peaks could be clearly observed in the XPS total spectrum. In terms of electrochemical performance, the over potential of Ni-Mo-Nd/NF was only 73 mV at 10 mA/cm2 in alkaline medium, the Tafel slope was 147 mV/dec, the double-layer capacitance (Cdl) value was 4.39 mF/cm2, the charge transfer resistance was 1.352 Ω, compared with Ni-Mo/NF. The binary electrode decreased by 62 mV, 54 mV/dec, 0.35 Ω, and the double-layer capacitance (Cdl) value increased by 1.66 mF/cm2. In addition, the current density of Ni-Mo-Nd/NF electrocatalyst remained stable after prolonged electrolysis for 24 h, and the activity of the catalyst decreased slightly after 2 000 cycles of voltammetry. It is concluded that the doping of rare earth element Nd can increase and refine the crystal grains, thus increasing the specific surface area of the electrode, providing more active sites for hydrogen evolution reaction and improving the efficiency of hydrogen evolution reaction. Compared with the binary alloy Ni-Mo/NF, the Ni-Mo-Nd/NF ternary alloy electrode exhibits better HER catalytic performance due to the synergistic effect of the ternary alloy. |
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