Thin-layer flow electrolytic cell applicable to electrochemical in-situ Raman spectrum detection

An in-situ Raman and spectral detection technology, applied in the field of Raman spectroscopy detection and analysis, can solve the problems of low Raman light collection efficiency and low detection sensitivity of electrochemical Raman spectroscopy, so as to improve the collection efficiency and detection sensitivity, reduce the Differences and the effect of improving collection efficiency

Active Publication Date: 2016-03-16
UNIV OF SCI & TECH OF CHINA
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Problems solved by technology

[0004] The prior art discloses a variety of electrolytic cells for electrochemical in-situ Raman spectroscopy detection. The windows used are generally flat quartz windows, and the solution is usually in a static state. The thickness of the liquid layer between the window and the working electrode is required Thicker (~several millimeters thick) to avoid reaction distortion due to limited mass transfer. Flat windows and thick liquid layers lead to low Raman light collection efficiency and low detection sensitivity of electrochemical Raman spectroscopy

Method used

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  • Thin-layer flow electrolytic cell applicable to electrochemical in-situ Raman spectrum detection
  • Thin-layer flow electrolytic cell applicable to electrochemical in-situ Raman spectrum detection
  • Thin-layer flow electrolytic cell applicable to electrochemical in-situ Raman spectrum detection

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Embodiment 1

[0071] Raman spectra of Pd-C and C=O saturated with CO adsorbed on an electrode composed of 55nm Au2MLPd core-shell nanoparticles:

[0072]The 55nm Au2MLPd core-shell nanoparticles were synthesized according to the literature method and made into thin film electrodes on glassy carbon electrodes. Put the electrode into the O ring whose inner diameter is almost the same as its own diameter, use the left cell body with the first left groove and the second left groove and the right cell body with the first right groove and the second right groove Press it tightly so that the electrode is located in the space formed by the first left groove and the first right groove; then cover the electrode with a hollow silicone pad with a thickness of 0.5mm and a hemispherical window in the middle, the silicone pad and the window are positioned in the space formed by the second left groove and the second right groove, meanwhile, the bottom of the hemispherical window, the hollow part of the sil...

Embodiment 2

[0074] The Raman spectra of Pt-C and C=O saturated with adsorbed CO were obtained on 55nmAu1MLPt, 55nmAu2MLPt core-shell nanoparticles and Pt(111) electrodes:

[0075] The procedure on 55nmAu1MLPt and 55nmAu2MLPt core-shell nanoparticles is consistent with that in Example 1. A Pt(111) single crystal electrode was prepared according to the literature. The shape of the electrode is hemispherical, and the surface of the hemisphere has only a flat surface, which is the surface we want to study, and only this surface can contact the solution. Put the cleaned single crystal electrode into the O ring whose inner diameter is almost the same as its own diameter, use the left cell body with the first left groove and the second left groove and the first right groove and the second right groove The right cell body of the groove presses it tightly so that the electrode is located in the space formed by the first left groove and the first right groove; then cover the electrode with a hollow...

Embodiment 3

[0077] Raman spectra of saturated CO adsorbed on rough Pt thin film electrodes obtained by SHINERS technology at different temperatures:

[0078] First of all, temperature correction should be carried out: put the thermometer head into the O ring whose inner diameter is almost the same as its own diameter, use the left pool body with the first left groove and the second left groove and the first right groove and the second right groove. The right cell body of the groove presses it tightly so that the electrode is located in the space formed by the first left groove and the first right groove; then cover the electrode with a hollow, 0.5mm thick silicone pad and a hemispherical middle The window, the silica gel pad and the window are located in the space formed by the second left groove and the second right groove, meanwhile, the bottom of the hemispherical window, the hollow part of the silica gel pad and the upper surface of the electrode form a solution cavity, and The spheri...

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Abstract

The invention provides a thin-layer flow electrolytic cell applicable to electrochemical in-situ Raman spectrum detection. The thin-layer flow electrolytic cell employs the design of a semispherical window; and a solution flows in a right solution channel, a solution chamber and a left solution channel, thereby forming the flow electrolytic cell. Through introduction of the flowing function, the thickness of a solution layer between a working electrode and the window can be substantially reduced, so collection efficiency and detection sensitivity of Raman scattered light are greatly improved while electrochemical measurement is not influenced. Meanwhile, the design of the semispherical window can eliminate the refraction effect of an interface of air and the quartz window, reduce difference between the focus of a laser optical path and the focus of an optical imaging optical path and decreases divergence angles of light, so acquisition efficiency and detection sensitivity of Raman spectra are improved. The thin-layer flow electrolytic cell can monitor dynamic changes of surface adsorbed species in the process of an electrochemical reaction in situ in a wide temperature range and obtains inherent information of surface adsorbed substances related to parameters of reaction kinetics.

Description

technical field [0001] The invention relates to the technical field of Raman spectrum detection and analysis, in particular to a thin-layer flow electrolytic cell suitable for electrochemical in-situ Raman spectrum detection. Background technique [0002] Raman spectroscopy is an important fingerprint technology for the characterization of physical properties in the fields of chemistry, materials, biology, and the environment. However, because the probability of Raman scattering is too low (several orders of magnitude lower than that of infrared spectroscopy), the sensitivity of Raman detection is low, and due to the low sensitivity of Raman spectroscopy, it leads to serious problems such as difficult quantification and poor reproducibility. This restricts the wide application of Raman spectroscopy. These shortcomings are particularly prominent in Raman spectroscopy studies of electrode / electrolyte interfaces. In the electrochemical spectroscopy experiment, the spectroelec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65G01N27/28
CPCG01N21/65G01N27/28
Inventor 陈艳霞郑勇力陈微张普
Owner UNIV OF SCI & TECH OF CHINA
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