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A surface-enhanced Raman scattering substrate and its preparation method

A surface-enhanced Raman and substrate technology, which is applied in Raman scattering, measurement devices, instruments, etc., can solve the problems of less explanation of SERS substrate enhancement mechanism, inaccurate qualitative and quantitative detection, and high cost in the detection process. The effect of field enhancement, rapid detection, and simple detection method

Active Publication Date: 2018-07-13
张志刚
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] There are two major problems in the detection of β-doping agents: one is that the qualitative and quantitative detection cannot be accurately performed, and the detection limit is too large; the other is that the cost of the detection process is too high
However, there are not many requirements for high-sensitivity detection, and there are few explanations for the enhancement mechanism of SERS substrates

Method used

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  • A surface-enhanced Raman scattering substrate and its preparation method
  • A surface-enhanced Raman scattering substrate and its preparation method
  • A surface-enhanced Raman scattering substrate and its preparation method

Examples

Experimental program
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Embodiment 1

[0040] Example 1: Preparation of Surface Enhanced Raman Scattering Substrate

[0041] (1) Firstly, the ultrasonically cleaned silicon wafer was activated for 6 minutes under a reactive ion etching system with a power of 80W, and then self-assembled single-layer PS spheres (polystyrene, diameter 500nm) were performed, and the rotation speed was controlled at a low speed of 500rpm. Coating time 10s, high speed 2500rpm, spin coating time 40s, then put the above-mentioned silicon wafer with PS ball template into a reactive ion etching system with a power of 80W to etch for 60s, O 2 The flow rate is 2.0L / min. Put the above sample into the magnetron sputtering equipment to sputter ZnO thin film, the power is 80W, the ratio of argon and oxygen is 1:1, the substrate is rotated without heating, the pressure is 1Pa, and the time is 24min, so that the thickness is 50nm. Annealing at 500° C. for 30 min in a nitrogen atmosphere to obtain a ZnO nanoparticle array with a spherical hollow sh...

Embodiment 2

[0045] Highly sensitive SERS detection of PATP (p-mercaptoaniline)

[0046] Using PATP molecule as the calibration reagent, the Raman enhancement factor is 10 9 , taking PATP as an example, the detection limit is about 0.01ng / ml (ppb)

[0047] (1) Firstly, a surface-enhanced Raman scattering substrate was prepared according to the specific preparation process of Example 1.

[0048] (2) Then configure different concentrations of PATP solutions, the concentration is 10 -4 , 10 -5 , 10 -6 , 10 -7 , 10 -8 , 10 -9 , 10 -10 M, M is the abbreviation of mol / L.

[0049] (3) Use a Renishaw Invia Raman spectrometer to collect signals on the SERS substrate dripped with the detection solution. The laser wavelength is 532nm, the laser power is 0.25mW, and the signal collection time is 1-10s. Concentration 10 -4 , 10 -5 , 10 -6 , 10 -7 , 10 -8 , 10 -9 , 10 -10 Raman spectrum of M.

[0050] (4) Then process the data with Origin software to obtain the corresponding detection l...

Embodiment 3

[0052] Example 3: Highly sensitive SERS detection of β-agonists

[0053] The highly sensitive SERS detection of β-agonists, the specific implementation steps are as follows:

[0054] (1) As described in Example 1, a highly sensitive SERS substrate based on the multipolar mode coupling resonance mechanism of the present invention was prepared.

[0055] (2) Preparation of detection solution: Prepare the standard powder samples of two kinds of β-agonists, clenbuterol and salbutamol, respectively with 99.99% methanol solution to obtain 1ng / L, 10ng / L, 100ng / L, 1ug / L , 10ug / L, 100ug / L, 1mg / L and 10mg / L detection solutions;

[0056] (3) Use a Renishaw Invia Raman spectrometer to collect signals on the SERS substrate dripped with the detection solution, and collect two kinds of β-excited signals under the conditions of laser wavelength of 532nm, laser power of 0.25mW, and signal collection time of 1-10s The Raman spectra of 8 concentrations of 1ng / L, 10ng / L, 100ng / L, 1ug / L, 10ug / L, ...

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Abstract

The invention relates to a surface enhanced raman scattering substrate and a preparation method thereof. The surface enhanced raman scattering substrate comprises a spherical empty shell and a film, wherein the film covers an upper half spherical surface of the spherical empty shell to form a composite micro-cavity structure, the spherical empty shell is the empty shell of any one of ZnO, TiO2, Al2O3, GaN and Al, and the film is an Ag film or an Au film. The preparation method of the substrate comprises the following steps: self-assembling an array template, adjusting the array template, depositing any one of ZnO, TiO2, Al2O3, GaN and Al on the array template, annealing the template in a nitrogen atmosphere, and depositing the Ag film or the Au film on the annealed array template. The multi-polar mode of the composite micro-cavity structure is coupled with a resonance mechanism, so that the advantages of simplicity in operation, rapidness in detection and high sensitivity can be realized, and the application prospect in the fields such as food security, stimulant detection and the like is wide.

Description

technical field [0001] The invention relates to metal surface plasmon resonance, dielectric cavity optical resonance, and the coupling technology of the two modes, in particular to a surface-enhanced Raman scattering substrate and a preparation method thereof. Background technique [0002] β-stimulants have the functions of promoting protein synthesis, accelerating fat metabolism, increasing carcass lean meat percentage, etc., and have been used as feed additives. Once people eat this type of animal food, it will cause poisoning, and long-term consumption will be even more harmful. Therefore, an accurate, rapid and convenient method for detecting β-agonists is of great significance for food safety. PATP, p-mercaptoaniline, can be used in Raman immunoassays. [0003] There are two major problems in the detection of β-doping agents: one is that the qualitative and quantitative detection cannot be performed accurately, and the detection limit is too large; the other is that t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65B82Y40/00
CPCB82Y40/00G01N21/658
Inventor 张志刚李静尹君吴敏班榕柽
Owner 张志刚
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