Preparation method of silver nanoparticle/graphene composite material

A composite material and graphene technology, which is applied in the field of preparation of SERS active substrates, can solve the problems of reducing the SERS activity of silver/graphene nanocomposite materials, impairing the superior characteristics of graphene, and damaging the chemical enhancement effect of graphene, etc. The effect of promoting the use on a large scale, preventing self-agglomeration, and being easy to operate

Inactive Publication Date: 2012-07-11
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, graphene that is first oxidized and then reduced will have a large number of defects, which seriously damages the superior characteristics of graphene itself, and also damages the chemical enhancement effect of graphene, greatly reducing the SERS activity of silver / graphene nanocomposites.

Method used

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  • Preparation method of silver nanoparticle/graphene composite material
  • Preparation method of silver nanoparticle/graphene composite material
  • Preparation method of silver nanoparticle/graphene composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Preparation of graphene NMP solution: Dissolve 0.2g of PVP in 20ml of NMP solution, ultrasonically disperse it evenly, add 0.001g of expanded graphite into the NMP solution, and ultrasonically for 40min, thus obtaining dispersion in the NMP solution Better monolayer graphene solutions. This solution is dripped on the copper grid and observed under the transmission electron microscope, and the transmission electron microscope picture obtained is as follows: figure 1 shown. from figure 1 It can be seen that the length of the as-prepared graphene sheets is about 5 μm. The obtained graphene solution is spin-coated on a silicon wafer, and tested with a confocal Raman spectrometer, and the obtained Raman spectrum is shown in figure 2 . In the figure, the ordinate represents the peak intensity, and the abscissa represents the Raman shift. from figure 2 It can be seen that the peak is at -1580cm -1 The G peak and its peak position are at -2700cm -1 The 2D peaks ...

Embodiment 2

[0024] (1) Preparation of graphene NMP solution: Dissolve 0.4g of PVP in 20ml of NMP solution, and disperse it evenly by ultrasonication, add 0.001g of expanded graphite into the NMP solution, and ultrasonicate for 50min, thus obtaining dispersion in the NMP solution Better monolayer graphene.

[0025] (2) Preparation of silver / graphene nanocomposite material: Take 10ml of the above graphene NMP solution for use. Prepare 10ml each of 0.01M tannic acid and silver nitrate solutions, first use a micropipette to take 1ml of silver nitrate solution, drop it into 10ml graphene NMP solution, and shake gently; after mixing evenly, use a micropipette Liquid container gets 3ml tannic acid solution, slowly adds dropwise in the above-mentioned solution, and now in this solution, the mass ratio of silver nitrate and graphene is 34, does not stop stirring; Continue to make it react 40min after dripping completely, obtains The silver particle is a silver / graphene solution of 20-30 nm.

[0...

Embodiment 3

[0029] (1) Preparation of graphene NMP solution: Dissolve 0.8g of PVP in 20ml of NMP solution, ultrasonically disperse it evenly, add 0.002g of expanded graphite into the NMP solution, and ultrasonically for 60min, thus obtaining dispersion in the NMP solution better monolayer graphene.

[0030] (2) Preparation of silver / graphene nanocomposite material: Take 10 ml of the above graphene NMP solution for use. Prepare 10ml of 0.01M tannic acid and silver nitrate solutions, first use a micropipette to take 2ml of silver nitrate, drop it into 10ml of graphene NMP solution, and shake gently; after mixing evenly, use a micropipette Take 8ml of tannic acid solution, slowly add it dropwise to the above solution, and keep stirring; after the dropwise addition is complete, continue to react for 50min to obtain a silver / graphene solution with silver particles of 20-30nm. Carry out at room temperature. The prepared solution is centrifuged and washed three times with deionized water to ob...

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Abstract

The invention relates to a preparation method of SERS active substrates and in particular relates to a preparation method of a silver nanoparticle / graphene composite material. The preparation method comprises the following steps: (1) graphene NMP solution preparation: adding expanded graphite into a NMP solution, and dispersing uniformly by ultrasonic wave to obtain a NMP solution of single layergraphene, wherein the PVP concentration is 0.01 g / mL to 0.05 g / mL and the graphene content is 0.02 g / L to 0.1 g / L; (2) silver nanoparticle / graphene solution preparation: adding dropwise equal concentrations of silver nitrate aqueous solution and tannic acid aqueous solution into the NMP solution of single layer graphene, controlling the silver nitrate / graphene mass ratio within the range of 10 to100, and stirring to obtain a silver nanoparticle / graphene solution in which the silver particles have a particle size of 20 nm to 30 nm; and (3) centrifugally washing with deionized water to obtain the silver / graphene composite nanomaterial. The silver nanoparticle / graphene composite material has the physical enhancement effect of silver particles as well as the chemical enhancement effect of graphene, and is excellent in SERS activity. According to the preparation method, tannic acid is used as a reducer and is environment-friendly. The preparation method is simple and easy to operate and is favorable to large-range generalization and application.

Description

technical field [0001] The invention relates to a preparation method of a SERS active substrate, in particular to a preparation method of a nano-silver / graphene composite material SERS active substrate. Background technique [0002] Surface enhanced Raman scattering (surface enhanced Ramanscattering, SERS) is an abnormal surface optical phenomenon discovered in the application of laser Raman spectroscopy to surface science research. Its generation mechanism can be divided into electromagnetic field enhancement and chemical enhancement. Among them, the electromagnetic field enhancement mode has been widely recognized. Some literature points out that electromagnetic field enhancement plays a major role in the enhancement effect of SERS. Since SERS has a very high gain factor, even up to a million times or even higher, it has great development potential in the application of detectors and single-molecule detection. The surface plasmons of metal nanoparticles have a strong lo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24
Inventor 王秀娟孟国文朱储红
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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