Preparation method of surface-enhanced Raman scattering substrate of metal particle array

A surface-enhanced Raman and metal particle technology, applied in Raman scattering, material excitation analysis, etc., can solve problems such as easy oxidation, poor time stability, etc.

Inactive Publication Date: 2012-09-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First of all, the use of a three-dimensional composite SERS substrate to replace a two-dimensional planar substrate is to increase the specific surface area of ​​the substrate, which in turn can greatly increase the density of SERS "hot spots" to achieve the purpose of improving Raman signal intensity and sensitivity; second, precious metals Due to its large plasmon resonance frequency (2.5 eV), silver has become the material of choice for the preparation of high SERS enhancement capabilities, but a major disadvantage of metallic silver is that it is easily oxidized in air, resulting in poor SERS performance. Stability, which is also one of the main problems that need to be solved urgently in the application of SERS

Method used

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  • Preparation method of surface-enhanced Raman scattering substrate of metal particle array
  • Preparation method of surface-enhanced Raman scattering substrate of metal particle array

Examples

Experimental program
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Effect test

Embodiment 1

[0017] (1) Place an n or p-type single crystal silicon wafer with a resistivity of 2 Ω?cm in the reactor, and fill it with 10% HF and 0.005mol / L AgNO 3 and H with a mass fraction of 0.5% 2 o 2 The composition of the etching solution, the solution volume filling degree of the reaction kettle is 80%, and it is etched at a temperature of 50°C for 15 minutes. After the above-mentioned metal-assisted chemical etching method, the porous silicon nanowire array of the substrate material required for the substrate can be prepared. ;

[0018] (2) Put the porous silicon nanowire array in 0.01mol / L AgNO 3 Immerse in the solution for 2 minutes, remove and wash with N 2 Blow dry to obtain the metal particle array-based surface-enhanced Raman scattering substrate;

[0019] (3) Drop the rhodamine 6G solution onto the surface of the substrate in the form of a hanging drop, put it into a Raman spectrometer for analysis, and the detection limit can be as low as 10 -16 mol / L.

Embodiment 2

[0021] (1) Place an n-type (111) oriented monocrystalline silicon wafer with a resistivity of 0.001Ω·cm in a reactor, and fill it with 1% HF and 0.001mol / L AgNO 3 and H with a mass fraction of 0.1% 2 o 2 The composition of the etching solution, the solution volume filling degree of the reaction kettle is 40%, and it is etched at a temperature of 10°C for 2 hours. After the above-mentioned metal-assisted chemical etching method, the porous silicon nanowire array of the substrate material required for the substrate can be prepared. ;

[0022] (2) Put the porous silicon nanowire array in 40% HF and 1mol / L AgNO 3 After immersing in the mixed solution for 1 second, take it out and dry it naturally to obtain a metal particle array-based surface-enhanced Raman scattering substrate;

[0023] (3) Drop the pesticide Thiram solution onto the surface of the substrate in the form of hanging drops, put it into a Raman spectrometer for analysis, and the detection limit can be as low as 10...

Embodiment 3

[0025] (1) A p-type (100) oriented single crystal silicon wafer with a resistivity of 50 Ω cm was placed in a reactor, filled with 40% HF and 1mol / L AgNO 3 and H with a mass fraction of 10% 2 o 2 The composition of the etching solution, the solution volume filling degree of the reaction kettle is 90%, and it is etched at a temperature of 100 ° C for 1 minute. After the above-mentioned metal-assisted chemical etching method, the porous silicon nanowire array of the substrate material required for the substrate can be prepared. ;

[0026] (2) Put the porous silicon nanowire array in 0.0001mol / L HAuCl 4 Immerse in the solution for 1 hour, take it out and wash it in N 2 Blow-dry in medium to obtain the metal particle array-based surface-enhanced Raman scattering substrate;

[0027] (3) Soak the substrate in Rhodamine 6G solution for 1 hour, take it out, dry it, put it into a Raman spectrometer for analysis, the detection limit can be as low as 10 -12 mol / L.

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Abstract

The invention provides a preparation method of a surface-enhanced Raman scattering substrate of a metal particle array. The preparation method comprises the following steps of: preparing a porous silicon nanometer wire array (PSNWA) as a substrate material through a metal-assisted chemical corrosion method; reducing metal ions in a metal salt solution to elementary substance through an impregnation-reduction method, and obtaining the surface-enhanced Raman scattering substrate after uniformly depositing the elementary substance on the surface of the PSNWA in a nanometer particle manner; and inducing a substance to be detected into an active substrate surface through an infiltration or titration method, namely carrying out Raman spectrum detection. The preparation method provided by the invention has the advantages of low cost, simple process, simplicity and convenience in operation, high sensitivity of SERS (Surface-Enhanced Raman Scattering) signals, and good repeatability; and an SERS light spectrum has very good stability and repeatability. The invention provides a molecule detection and trace quantity analysis method with high speed, high sensitivity and high reliability. The preparation method provided by the invention needs extremely less sample amount, is suitable for various liquid samples, and has wide application prospects of rapid identification of clinical biological molecules, trace quantity chemical substance detection, biological sample analysis and the like.

Description

technical field [0001] The invention belongs to the technical field of Raman spectroscopic molecular detection, and relates to a method for preparing a surface-enhanced Raman scattering active substrate with the characteristics of low cost, simple process, easy operation, Raman signal enhancement effect and good repeatability. Background technique [0002] Since the phenomenon of Surface-enhanced Raman Scattering (SERS) was first observed on the surface of a rough silver electrode adsorbed with pyridine molecules in 1974, SERS research has developed rapidly. Using SERS technology, the Raman scattering signal can be greatly enhanced when the molecule to be tested is adsorbed on a rough metal surface, which can give information at the single-molecule level, has very high sensitivity, and has fast test speed and mild test conditions. The molecules to be tested are not destructive, and at the same time, they can be portable for real-time and on-site detection and analysis. These...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
Inventor 许海军苏雷廛宇飞张常兴孙晓明
Owner BEIJING UNIV OF CHEM TECH
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