麦满芳,廖彬,曾珊,王金凤,郭燕玲,马信洲.基于超短电压脉冲的Cu2O微区电沉积研究[J].表面技术,2024,53(6):183-189.
MAI Manfang,LIAO Bin,ZENG Shan,WANG Jinfeng,GUO Yanling,MA Xinzhou.Localized Electrochemical Deposition of Cu2O with Ultrashort Voltage Pulses[J].Surface Technology,2024,53(6):183-189 |
| 基于超短电压脉冲的Cu2O微区电沉积研究 |
| Localized Electrochemical Deposition of Cu2O with Ultrashort Voltage Pulses |
| 投稿时间：2023-02-04 修订日期：2023-06-21 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.06.016 |
| 中文关键词: 微区电沉积 超短脉冲 Cu2O 微结构 |
| 英文关键词:localized electrochemical deposition ultrashort voltage pulses Cu2O microstructure |
| 基金项目:国家自然科学基金资助项目(11504242);广东省教育厅特色创新项目(2020KTSCX131);粤港澳智能微纳光电技术联合实验室(2020B1212030010);广东省基础与应用基础研究基金项目(2020B1515120097) |
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| Author | Institution |
| MAI Manfang | School of Physics and Optoelectronic Engineering,Guangdong Foshan 528225, China ;Guangdong-Hong Kong-Macao Joint Laboratory for Intelligent Micro-nano Optoelectronic Technology, Foshan University Guangdong Foshan 528225, China |
| LIAO Bin | School of Materials Science and Hydrogen Energy, Guangdong Foshan 528225, China |
| ZENG Shan | School of Materials Science and Hydrogen Energy, Guangdong Foshan 528225, China |
| WANG Jinfeng | School of Materials Science and Hydrogen Energy, Guangdong Foshan 528225, China |
| GUO Yanling | School of Materials Science and Hydrogen Energy, Guangdong Foshan 528225, China |
| MA Xinzhou | School of Materials Science and Hydrogen Energy, Guangdong Foshan 528225, China |
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| 中文摘要: |
| 目的 实现基于纳秒级超短电压脉冲的Cu2O微区电沉积。方法 开发了可视化超短电压脉冲微区电化学加工系统，通过脉冲发生器施加纳秒长的超短电压脉冲到微电极与工作电极之间使局部极化发生，采用原位倒置光学显微镜实时监控微区电沉积的动态过程。使用扫描电子显微镜对Cu2O微结构的微观形貌进行表征，研究不同加工参数，包括电极间距、脉冲长度和微电极运动速度对微区电沉积Cu2O的尺寸及微观形貌的影响。结果 电极间距、脉冲长度和微电极运动速度均对沉积的Cu2O微圆盘的直径和晶粒形貌有显著影响。电极间距的增大，使沉积的Cu2O微圆盘的直径和晶粒尺寸均有所减小。电压脉冲长度越小，Cu2O微圆盘的面积越小。微电极移动的速度越快，Cu2O微圆盘的直径越小，结晶性变差。电极间距为14 µm、脉冲长度为30~40 ns以及降低微电极运动速度能够获得轮廓清晰的微区电沉积结构。结论 基于纳秒级超短电压脉冲可视化微区电化学加工系统成功地在ITO导电玻璃表面沉积了直径为50~100 µm的Cu2O微圆盘，为高效率Cu2O基光电器件的微加工提供了简单有效的方法。 |
| 英文摘要: |
| Localized electrochemical deposition is a micromachining approach which exhibits great potential in fabrication of various microstructures due to its simplicity, low cost and reproducibility. Upon applying ultrashort voltage pulses, electrochemical reactions can be spatially confined with nanometer accuracy, which permits for high precision machining of electrochemical active materials including metals and semiconductors. Cu2O has been extensively investigated for its appealing electronic and optical properties, with a direct bandgap around 2.0 eV, a high absorption coefficient as well as abundance. Recently, more researches have focused on Cu2O-based optoelectronic and photochemical devices such as photocathodes for photoelectrochemical water splitting. Electrodeposition is a common method for the preparation of Cu2O, which has advantages of inexpensiveness, low reaction temperature and ease of control. However, Cu2O in micro-size can not be prepared by traditional electrodeposition. Using localized electrochemical deposition with ultrashort voltage pulses, Cu2O in micro-size can be fabricated. At present, Cu2O microstructures prepared by localized electrochemical deposition with ultrashort voltage pulses has not been reported yet. In this paper, Cu2O microdisks were successfully fabricated by localized electrochemical deposition with nanosecond ultrashort voltage pulses. A visualized processing system based on a four-electrode configuration for localized electrochemical deposition with ultrashort voltage pulses was developed. In a miniature cell, an indium tin oxide (ITO) covered glass was used as the working electrode. A Pt wire and an Ag/AgCl were functioned as the counter electrode and the reference electrode while a 50 μm diameter Pt/Ir wire with its front face polished was used as the microelectrode. Solution of 0.4 mol/L CuSO4+ 3 mol/L C3H6O3 with pH adjusting to 11 was used as electrolyte. Local polarization was induced through applying nanosecond ultrashort voltage pulses generated by a pulse generator between the microelectrode and the working electrode. The potential of the working electrode and the microelectrode were controlled by a Bi-potentiostat. An in situ inverted optical microscope was used to monitor the dynamic process of localized electrochemical deposition in real time. Morphology of Cu2O deposited with different conditions was characterized with a scanning electron microscopy (SEM). The effects of processing parameters, including electrodes interval, pulse length and microelectrode removed velocity on the size and morphology of the deposited Cu2O were investigated. The results in this paper showed that electrodes interval, pulse length and microelectrode removed velocity had significant effects on the diameter and morphology of the deposited Cu2O microdisks. As the electrodes interval increased, the diameter and the grain size of the deposited Cu2O microdisks both decreased. The shorter the voltage pulse length, the smaller the area of the Cu2O microdisks. The faster the microelectrode moved, the smaller the diameter of the Cu2O microdisks and the worse the crystallinity. Well-defined deposited Cu2O microstructures could be obtained using electrodes interval of 14 μm, pulse length of 30-40 ns and low microelectrode removed velocity. In conclusion, Cu2O microdisks with a diameter of 50-100 μm were successfully deposited on the surface of ITO substrates by localized electrochemical deposition with nanosecond ultrashort voltage pulses, which provides a simple and effective method for micromachining high-efficiency Cu2O-based optoelectronic devices. |
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