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Silver nanodendrite surface enhanced Raman scattering (SERS) substrate, and preparation method and application thereof

A surface-enhanced Raman and silver nanotechnology, applied in Raman scattering, nanotechnology, material excitation analysis, etc., can solve the problem of high-concentration HF solution limiting the application range, metal activity limiting the use of substrate raw materials, and limiting large-scale applications and other problems, to achieve the effect of enhancing surface Raman scattering activity, fast and convenient preparation process, and adjustable size

Inactive Publication Date: 2012-11-07
WENZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Recently, the research group of Meng Guowen, Institute of Solid State Physics, Chinese Academy of Sciences (J. Appl. Phys., 2010, 107, 044315) also reported the rapid detection of tetrachlorobiphenyl based on the silver nano-"dendrite" SERS effect, and the detection limit can be very low, but the preparation process of its silver nanodendrite needs to use a higher concentration of HF solution, which limits its large-scale application
Foreign Maboudian et al. treated the surface of aluminum paper with a concentrated HF solution, used AgF as a precursor, and obtained three-dimensional silver dendrites after 24 hours of dark reduction, and used the substrate to detect compounds such as 2, 2'-dithiobipyridine, although they showed Higher SERS signal, but the longer preparation cycle and the use of high-concentration HF solution limit its application to some extent (J. Am. Chem. Soc. 2010, 132, 1476)
In addition, the three-dimensional silver dendrite structure can be obtained through controllable reduction of silver ions on the surface of active metal sheets by utilizing the reducibility of metals, such as Sn (Langmuir 2008;24:12010), Zn (J. Phys. Chem. C 2008, 112 , 16301), Cu (Mater. Lett., 2009, 63, 2306), although the method is simple, the requirement of metal activity limits the use of substrate materials to a certain extent

Method used

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  • Silver nanodendrite surface enhanced Raman scattering (SERS) substrate, and preparation method and application thereof
  • Silver nanodendrite surface enhanced Raman scattering (SERS) substrate, and preparation method and application thereof
  • Silver nanodendrite surface enhanced Raman scattering (SERS) substrate, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 8ml AgNO to a 10ml electrolytic cell 3 (0.02 mol·L -1 ) solution as the electrolyte, a small piece of ITO is inserted into the electrolytic cell as the working electrode, the effective part immersed in the electrolyte is 1 cm×0.5 cm, and the Pt wire is used as the reference electrode and the counter electrode. Turn on the working current and adjust it to 5 mA, silver nanodendrites grow on the surface of ITO, turn off the current after 14s, rinse the ITO substrate with water, and dry to obtain the SERS active substrate.

[0031] The above-mentioned active substrate with SERS effect on the surface was used as the Raman detection substrate, 2, 2’-dithiobipyridine was used as the probe molecule, and methanol was used as the solvent to prepare it at a concentration of 1 μmol L -1 solution, use a micro-syringe to measure 50 μl and drop it on the substrate, and do Raman detection after the solvent evaporates (JY-T64000 Raman spectrometer, excitation wavelength is 632.8 nm...

Embodiment 2

[0033] Add 8ml AgNO to a 10ml electrolytic cell 3 (0.02 mol·L -1 ) solution as the electrolyte, a small piece of ITO is inserted into the electrolytic cell as the working electrode, the effective part immersed in the electrolyte is 1 cm×0.5 cm, and the Pt wire is used as the reference electrode and the counter electrode. Turn on the working current and adjust it to 5 mA, silver nanodendrites grow on the surface of ITO, turn off the current after 10s, wash the ITO substrate with water, and dry to obtain the SERS active substrate.

[0034] The active substrate with the SERS effect obtained above was used as the Raman detection substrate, and 2,2'-dithiobipyridine was used as the probe molecule, and the Raman detection was performed according to the method in Example 1, and it was clearly observed that 2, The characteristic peak of 2'-dithiodipyridine, its Raman signal intensity is close to that of Example 1.

Embodiment 3

[0036] Add 8ml AgNO to a 10ml electrolytic cell 3 (0.02 mol·L -1 ) solution as the electrolyte, a small piece of ITO is inserted into the electrolytic cell as the working electrode, the effective part immersed in the electrolyte is 1 cm×0.5 cm, and the Pt wire is used as the reference electrode and the counter electrode. Turn on the working current and adjust it to 5 mA. Silver nanodendrites grow on the surface of ITO. After 30s, turn off the current, rinse the ITO substrate with water, and dry it to obtain the SERS active substrate.

[0037] The active substrate with the SERS effect obtained above was used as the Raman detection substrate, and 2,2'-dithiobipyridine was used as the probe molecule, and the Raman detection was performed according to the method in Example 1, and it was clearly observed that 2, The characteristic peak of 2'-dithiodipyridine, its Raman signal intensity is equivalent to that of Example 1.

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Abstract

The invention discloses a silver nanodendrite surface enhanced Raman scattering (SERS) substrate, and a preparation method and application thereof, relating to the technical field of nanomaterial science and Raman detection. The SERS active substrate is of silver dendrites which are distributed evenly, and the three-dimensional sizes of dendrites are adjustable. The preparation method of the invention is characterized in that the silver nanodendrites are electrically deposited on commercially available ITO (Indium-doped Tin Oxide) conductive glass by adopting a constant current deposition method and using a silver nitrate solution as electrolyte without adding any other auxiliary. The preparation method of the invention has the advantages of simple, convenient fast (30s) preparation process, low cost, small current and low voltage, and the silver dendrites can be transferred to any substrate (paper, other metal sheets or plastic sheets). The substrate obtained by the method disclosed by the invention has high stability and ordered and controllable structure, and exhibits quite high sensitivity in Raman spectrum detection.

Description

technical field [0001] The invention belongs to the technical field of laser Raman detection and nanomaterial science, and in particular relates to a silver nanodendritic surface-enhanced Raman scattering substrate and a preparation method thereof. Background technique [0002] Raman spectroscopy is a molecular structure characterization technology based on the Raman effect, which uses photons as probes and has the characteristics of real-time non-destructive and rapid detection. However, due to the low efficiency of ordinary Raman scattering and weak signal, increasing the laser intensity may cause side effects such as damage or photobleaching of the sample. The detection seems powerless, so other auxiliary enhancement methods are needed. Therefore, Surface Enhanced Raman Scattering Spectroscopy (SERS) emerged as a means of Raman enhancement. SERS technology originates from the adsorption of trace molecules on Cu, Au, Ag and other metal sols and electrode surfaces, and the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65C25D3/46B82Y40/00
Inventor 王舜陈锡安
Owner WENZHOU UNIV
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