Citation: XIA Hai-Lun, HUA Xin, LONG Yi-Tao. Coupled Time-of-Flight Secondary Ion Mass Spectrometry-Electrochemical Analysis of Electrode-Electrolyte Interface at High Vacuum of 10^-5 Pa[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(12): 1887-1892. doi: 10.19756/j.issn.0253-3820.191449 shu

Coupled Time-of-Flight Secondary Ion Mass Spectrometry-Electrochemical Analysis of Electrode-Electrolyte Interface at High Vacuum of 10^-5 Pa

XIA Hai-Lun ^1, ,
HUA Xin ¹ ,
LONG Yi-Tao ^1,2

1.
School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237, China;
2.
State Key Laboratory of Analytical Chemistry for Life Science, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China

Received Date: 27 July 2019
Revised Date: 23 August 2019

Fund Project: This work was supported by the National Natural Science Foundation of China (Nos. 21834001, 21705046).

Electrode-electrolyte interface, where the electrochemical reaction happens, plays an important role in the investigation of electrochemical mechanism. The traditional electrochemical techniques pay more attention on the charge transfer process happened on the electrode. However, they cannot provide information of the electrode-electrolyte interface at molecular level. How to realize the in-situ electrochemical monitoring of the intermediates on the electrode-electrolyte interface during redox reaction is of great significance to the study of electrochemical mechanism. In this work, electrochemical reaction of coenzyme Q₀ (CoQ₀) on the gold electrode was studied by time-of-flight secondary ion mass spectrometry (ToF-SIMS). A high vacuum compatible microfluidic electrochemical cell was fabricated for the electrochemical study of CoQ₀. Then, a micro-hole with diameter of 2 μm was fabricated on the electrochemical cell by the primary ion beam of ToF-SIMS for the subsequent analysis. To evaluate the feasibility of ToF-SIMS for liquid sample measurement, the chemical distribution of CoQ₀ and the SiN^- around the micro-hole were measured. The stable distribution of CoQ₀ and the SiN^- during the ToF-SIMS measurement indicated that the microfluidic electrochemical cell was compatible for the in-situ detection of the electrode-electrolyte interface in high vacuum environment (1×10^-5 Pa). Electrochemical behavior of CoQ₀ in the electrochemical cell was further studied. The variations of CoQ₀, CoQ₀H₂ and related intermediate at different potentials agreed well with the electrochemical reaction of CoQ₀ in aqueous solution, which showed that the direct molecular evidence of the electrode-electrolyte interface was obtained. The direct monitoring of electrode-electrolyte interface by ToF-SIMS revealed the electrochemical evolution on the electrode at molecular level, which was of great potential for the detailed understanding of the electrochemical reaction mechanism.
- Coenzyme Q₀,
- Electrode-electrolyte interface,
- In-situ electrochemical monitoring,
- Time of flight secondary ion mass spectrometry
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Coupled Time-of-Flight Secondary Ion Mass Spectrometry-Electrochemical Analysis of Electrode-Electrolyte Interface at High Vacuum of 10-5 Pa

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通讯作者: 陈斌, bchen63@163.com

Coupled Time-of-Flight Secondary Ion Mass Spectrometry-Electrochemical Analysis of Electrode-Electrolyte Interface at High Vacuum of 10^-5 Pa