电化学扫描隧道显微术:以Cu在Au(111)表面初始阶段电沉积为例  

Electrochemical Scanning Tunneling Microscopy:Taking the Initial Stage of Cu Electrodeposition on Au(111)as an Example

作　　者：谭卓 李凯旋 毛秉伟[1] 颜佳伟[1] Zhuo Tan;Kai-Xuan Li;Bing-Wei Mao;Jia-Wei Yan(State Key Laboratory of Physical Chemistry of Solid Surfaces,Department of Chemistry,College of Chemistry and Chemical Engineering,Xiamen University,Xiamen 361005,Fujian,China)

机构地区：[1]厦门大学化学化工学院,固体表面物理化学国家重点实验室,福建厦门361005

出　　处：《电化学》2023年第7期30-35,共6页Journal of Electrochemistry

摘　　要：电化学扫描隧道显微术能在电解质溶液中获得随电位变化的电极表面高空间分辨率的结构信息及跟踪某些反应过程,为从高空间分辨率的角度理解界面结构和电极过程提供了一种强有力的手段。本文以电化学扫描隧道显微术研究Cu在Au(111)上电沉积初始阶段过程为例,与读者交流电化学扫描隧道显微术实验方面的经验,涉及实验装置、实验操作、实验步骤和注意事项等。Electrochemical scanning tunneling microscopy(ECSTM)plays an important role in the field of electrochemistry,which can obtain potential-dependent structural information of electrode surface with high spatial resolution and observe some reaction processes in electrolyte solutions,and provide a powerful way to understand the interfacial structure and electrode processes from the perspective of high spatial resolution.In this article,the study of electrodeposition of Cu on Au(111)by ECSTM is taken as an example to introduce the experimental methods required for ECSTM and share our experience with other electrochemical groups.Firstly,the working principle of STM is introduced so that readers can understand the imaging principle of STM.Secondly,we describe the process in detail and the points for attention during ECSTM experiments,which include the cleanings of the electrochemical cell and O-ring,the preparation and encapsulation of the ECSTM tip,the preparation and cleaning of the working electrode,and the selections of the counter electrode and reference electrode.Thirdly,the ECSTM study on the initial stage of Cu electrodeposition on Au(111)has been taken to demonstrate the experimental procedure of ECSTM,and shown its ability to obtain image with high spatial resolution.We have analyzed the two interfacial structures obtained by ECSTM at two different potential regions according to the cyclic voltammetric curve of Cu UPD on Au(111)electrode.The high-resolution atomic image obtained at a relatively positive potential is assigned to the image of Au atoms.Further,it has been demonstrated that the(√3×√3)R30°structure can be observed after the completion of the submonolayer of Cu on Au(111)in the sulfuric acid solution.However,the(√3×√3)R30°structure obtained between the two pairs of current peaks of cyclic voltammetric curve should be assigned to the adsorption of sulfate anions,which occupy the centers of honeycomb lattice formed by Cu adatoms.The ECSTM images demonstrate the ability of this technique to

关 键 词：扫描隧道显微术 电化学 铜电沉积 欠电位沉积 

分 类 号：TQ150.6[化学工程—电化学工业]