Working electrode for electrochemical onsite surface enhanced Raman scattering (SERS) spectrum in-situ cell as well as preparation method and application thereof

A working electrode, spectroscopic in-situ technology, used in Raman scattering, material excitation analysis, etc., can solve the problems of poor signal stability and reproducibility, and achieve improved accuracy and reliability, easy processing, stability and reproducibility. good effect

Inactive Publication Date: 2012-08-15
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In view of the problems existing in the above-mentioned background technology, the present invention proposes a working electrode for an electrochemical field SERS spectrum in-situ cell, a preparation method of the working electrode and an in-situ cell using the work

Method used

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  • Working electrode for electrochemical onsite surface enhanced Raman scattering (SERS) spectrum in-situ cell as well as preparation method and application thereof
  • Working electrode for electrochemical onsite surface enhanced Raman scattering (SERS) spectrum in-situ cell as well as preparation method and application thereof
  • Working electrode for electrochemical onsite surface enhanced Raman scattering (SERS) spectrum in-situ cell as well as preparation method and application thereof

Examples

Experimental program
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Example Embodiment

[0037] Example 1:

[0038] (1) Put the ITO glass sheet with the resistance value of 100Ω in acetone, isopropanol and ultrapure water for 20 minutes, and then use deionized water and hydrogen peroxide (30wt%) with a volume ratio of 5:0.5:0.5 , Ammonia water (25wt%) mixed solution boiling treatment for 30min;

[0039] (2) Place the cleaned ITO glass sheet at 0.18mol·L -1 Soak in the APTMS aqueous solution for 12h, take it out, rinse with ultrapure water, blow dry with nitrogen, and then treat it at 100℃ for 30min;

[0040] (3) At room temperature, immerse the silanized ITO glass sheet into 0.45×10 -7 The diameter of mmol / L is 30-50nm in gold sol for 6 hours, and the metal nanoparticles are assembled on the surface of the silanized ITO glass sheet through the electrostatic interaction between the silanized surface protonated amino groups and the metal nanoparticles;

[0041] (4) Immerse the ITO glass sheet into 1mmol / L HAuCl 4 And 0.1mol / L NaClO 4 In the mixed solution composed, use CHI7...

Example Embodiment

[0042] Example 2:

[0043] (1) Place the ITO glass sheet with a resistance value of 100Ω in acetone, isopropanol and ultrapure water for 25 minutes, and then use deionized water and hydrogen peroxide (30wt%) with a volume ratio of 5:1:1 , Ammonia (25wt%) mixed solution boiling treatment for 35min;

[0044] (2) Place the cleaned ITO glass sheet at 0.20mol·L -1 Soak in the 3-MPTMS aqueous solution for 24h, take it out and rinse with ultrapure water, blow dry with nitrogen, and then treat it at 105℃ for 35min;

[0045] (3) At room temperature, immerse the silanized ITO glass sheet into 0.45×10 -7 The particle size of mmol / L is 50-70nm in gold sol for 10 hours. The metal nanoparticles are assembled on the surface of the silanized ITO glass sheet through the chemical bonding between the sulfhydryl groups on the silanized surface and the metal nanoparticles.

Example Embodiment

[0046] Example 3:

[0047] (1) Place the ITO glass sheet with the resistance value of 100Ω in acetone, isopropanol and ultrapure water for 15 minutes, and then use deionized water and hydrogen peroxide (30wt%) with a volume ratio of 5:2:2. , Ammonia (25wt%) mixed solution boiling treatment for 25min;

[0048] (2) Place the cleaned ITO glass sheet at 0.25mol·L -1 Soak in the 3-MPTMS aqueous solution for 1 hour, take it out, rinse with ultrapure water, blow dry with nitrogen, and then treat it at 110°C for 25min;

[0049] (3) At room temperature, immerse the silanized ITO glass sheet into 0.50×10 -7 The particle size of mmol / L is 50~70nm in silver sol for 12 hours, and the metal nanoparticles are assembled on the surface of the silanized ITO glass sheet through the electrostatic interaction between the silanized surface protonated amino groups and the metal nanoparticles.

[0050] The gold or silver sols in the foregoing embodiments were prepared by the citrate reduction method proposed...

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Abstract

The invention discloses a working electrode for an electrochemical onsite surface enhanced Raman scattering (SERS) spectrum in-situ cell, a preparation method of the working electrode and an in-situ cell using the working electrode. The electrode comprises an indium tin oxide (ITO) glass substrate which is silanized and assembled with nanoscale Au or Ag particles orderly. The working electrode disclosed by the invention breaks through the limitation that only gold and sliver rod-shaped metal electrodes are used as the working electrodes in the traditional electrochemical onsite SERS spectrum in-situ cell, and can be used for effectively solving a long-standing puzzle that the reproducibility and stability of an SERS spectrum are poor; in addition, the working electrode disclosed by the invention has the advantages of convenience in purchasing process materials, easiness for processing, convenience in use and operation, wide applicable object range, strong SERS spectrum signal, and good stability and reproducibility; and the preprocessing time of the working electrode can be effectively reduced and fussy repetitive experimental works are avoided, therefore the efficiency of study works and the accuracy and reliability of work achievements are greatly improved.

Description

technical field [0001] The invention belongs to the field of spectroscopic instrument detection, and in particular relates to a working electrode for an electrochemical on-site SERS spectrum in-situ pool, a preparation method and application thereof. Background technique [0002] Electrochemical on-site surface-enhanced Raman spectroscopy (SERS) technology generally uses a specially designed and fabricated spectroelectrochemical in-situ cell placed in a Raman spectrometer, while performing electrochemical processes on the surface of the working electrode, with the help of laser probes and The surface-enhanced Raman scattering effect generated between the adsorbed species on the electrode surface characterizes the species and structure of the adsorbed species on the electrode surface with the change of electrochemical parameters such as potential. It has become a very important characterization and analysis technique in the research fields of material science, surface science...

Claims

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Application Information

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IPC IPC(8): G01N21/65
Inventor 曹晓卫李欣然邓卫琴
Owner SHANGHAI NORMAL UNIVERSITY
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