Composite SERS substrate and preparation method and application thereof

A technology of substrate and composite material, applied in the field of composite SERS substrate and its preparation, can solve the problems of easy agglomeration of MOF and noble metal particles, difficult to distribute evenly of noble metal nanoparticles, complicated and complicated post-modification, etc., so as to improve SERS performance and signal strength. , excellent surface plasmon performance, improved sensitivity and reproducibility

Pending Publication Date: 2022-01-14
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The MOF-metal nanoparticle composite SERS substrate prepared by the ex-situ method needs cumbersome and complicated post-modification, and the charged MOF and noble metal particles are easy to agglomerate, and the dispersion is greatly reduced.
Modified molecules or polymers are easy to block the pores of MOF materials and affect the performance of MOF
In addition, the exposed unsaturated group sites of MOF are limited, the modification effect is not satisfactory, and it is often difficult to achieve a uniform distribution of noble metal nanoparticles.
Greatly affects the performance of the composite SERS substrate, poor reproducibility
In addition, the combination of pesticides and organic dyes with traditional noble metal materials is weak and the detection signal is poor, which limits the application of composite SERS substrates in the detection of pesticides and organic dyes.

Method used

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  • Composite SERS substrate and preparation method and application thereof
  • Composite SERS substrate and preparation method and application thereof
  • Composite SERS substrate and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] The composite material in this example includes MOF materials and gold and silver nanoparticles, the gold and silver nanoparticles are loaded in situ on the surface of the MOF material, the gold and silver nanoparticles have a core-shell structure, and the core of the gold and silver nanoparticles is Au Nanoparticles, the shell of gold and silver nanoparticles is Ag nanoparticles.

[0089] In this example, the composite material is prepared by the following preparation method, including the following steps:

[0090] (1) Preparation of two-dimensional Ni-MOF:

[0091] Dissolve 360mg of terephthalic acid and 250mg of nickel chloride into the DMF-ethanol-deionized water mixture with a volume ratio of 30:2:2 (v / v / v). After fully dissolving, add 2mL of triethylamine , sonicated for 6h, the product was centrifuged, washed with DMF and ethanol several times, and dried in vacuum at 60°C for 12h to obtain a two-dimensional Ni-MOF powder. The morphology of the obtained two-dimen...

Embodiment 2

[0102] The composite SERS substrate in this example includes the composite material prepared in Example 1 with the noble metal core AuNPs having a particle size of 91 nm and the gold and silver nanoparticles having a particle size of 149 nm.

[0103] The preparation method of the composite SERS substrate in this example is the same as that of the composite material in Example 1.

Embodiment 3

[0105] The application of the composite SERS substrate obtained in embodiment 2 in the detection of pesticide thiram comprises the following steps:

[0106] Configure different concentrations of thiram detection solution, the specific concentration of thiram solution is: 50μg / L, 100μg / L, 250μg / L, 500μg / L, 1mg / L, 2.5mg / L, 5mg / L, 10mg / L, 25mg / L. Take 30 μL of thiram to be tested and add it to a 200 μL centrifuge tube, add 30 μL of the composite SERS substrate suspension obtained in Example 2 to each centrifuge tube, mix evenly, and let it stand for 60 minutes to obtain the detection solution, from the bottom of the centrifuge tube Pipette 30 μL of the detection solution onto the silicon wafer, and perform Raman detection after the water evaporates. The wavelength of the Raman detection laser is 785nm, the power is 25mW, and the integration time is 5s. For specific results, see Figure 7 , Figure 7 is the SERS spectrum of different concentrations of thiram on the composite SE...

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Abstract

The invention discloses a composite SERS substrate and a preparation method and application thereof.The composite SERS substrate comprises a composite material, the composite material comprises an MOF composite material with the surface loaded with precious metal nanoparticles, the precious metal nanoparticles are of a core-shell structure, and the precious metal nanoparticles are loaded on the surface of the MOF material through an in-situ growth method. The precious metal nanoparticles are gold and silver nanoparticles of a core-shell structure. According to the composite SERS substrate, effective combination of the MOF and the metal nanoparticles of the core-shell structure is achieved through in-situ reduction and growth, and the composite material combines the performance that the MOF material is large in specific surface area and can effectively adsorb and enrich to-be-detected molecules and the excellent surface plasma performance of the metal nanoparticles, so that the detection sensitivity and reproducibility of the composite SERS substrate are obviously improved.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a composite SERS substrate and its preparation method and application. Background technique [0002] With the continuous improvement of people's living standards, the attention to food safety has also continued to increase. Pesticide residues on vegetables, fruits and other foods, especially some systemic pesticides that are not easy to remove, have brought huge risks to human health. It is easy to cause genotoxicity, induce cancer, affect liver function, nerve spasm and other adverse consequences. Therefore, it is particularly important to develop a fast and accurate detection method for pesticide residues. Conventional detection methods include high performance liquid chromatography, liquid chromatography-mass spectrometry, gas chromatography-mass spectrometry, ion exchange chromatography, and fluorescence spectroscopy. Although these methods have high sensitivity, the pretreat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65B22F1/18B22F9/24B82Y30/00B82Y40/00
CPCG01N21/658B22F9/24B82Y40/00B82Y30/00
Inventor 李攻科赖华圣张卓旻
Owner SUN YAT SEN UNIV
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