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Composite material of graphene oxide/ nanometer precious metal with surface enhanced Raman effect and preparation thereof

A technology of surface-enhanced Raman and composite materials, applied in the field of nanomaterials, can solve problems such as complex preparation methods, difficult surface modification, and limited applications, and achieve the effects of flexible and adjustable components, mild reaction conditions, and large specific surface area

Active Publication Date: 2012-11-14
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The Chinese patent with the publication number CN102285629A discloses a method for preparing a surface-enhanced Raman spectroscopy active substrate, which includes spreading a single-layer polystyrene nano-bead array on the water surface, and using reactive plasma etching technology to prepare spaced polystyrene Nano-bead arrays are used to prepare surface-enhanced Raman spectroscopy active substrates. The substrates prepared by this method have high uniformity, but the preparation method is more complicated, and the enhancement of Raman spectroscopy signals is not obvious
[0005] The Chinese patent with the publication number CN102507530A discloses a method for preparing nano-silver surface-enhanced Raman spectroscopic substrates by gamma radiation. In this method, the glass substrate is placed in a radiation solution and irradiated with gamma-rays to obtain nano-silver surface-enhanced Raman spectroscopy. Spectral substrate, the preparation method of the substrate is simple, but the enhancement of the Raman spectral signal is not obvious enough
[0006] Graphene is a carbon atom with sp 2 The hybrid orbitals form a hexagonal planar film with a honeycomb lattice, which has unique physical and chemical properties. Applying graphene to the enhancement of Raman signals will have better results (green surface-enhanced Raman spectroscopy technology based on graphene ; Xu Weigao, Ling Xi, Zhang Jin; Abstracts of 2011 China Materials Symposium; 2011, P441), but there are strong intermolecular forces between the layers of graphene, it is difficult to stably disperse in solvents, and the surface It is inert and difficult to modify the surface, these factors limit its application in the field of Raman spectroscopy enhancement

Method used

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  • Composite material of graphene oxide/ nanometer precious metal with surface enhanced Raman effect and preparation thereof
  • Composite material of graphene oxide/ nanometer precious metal with surface enhanced Raman effect and preparation thereof
  • Composite material of graphene oxide/ nanometer precious metal with surface enhanced Raman effect and preparation thereof

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Experimental program
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Effect test

Embodiment 1

[0035] (1) Measure 20mL 10 -2 M AgNO 3 Solution, 80mL deionized water, 20mL 1% trisodium citrate solution, mix and stir for 15min at room temperature, add 100mL freshly prepared 10 -2 M NaBH 4 Solution, continue to stir the reaction for 1h. The prepared Ag sol was aged at 50°C for 2h before use;

[0036](2) Weigh 30 mg of graphene oxide and disperse it in 300 mL of ethanol solution with a volume fraction of 1% 3-mercaptopropylethoxysilane, stir continuously at room temperature for 24 hours, then wash and separate the mercapto-modified graphite oxide vinyl material;

[0037] (3) Disperse 1 mg of mercapto-modified graphene oxide material in 1 mL of water, mix evenly with 60 mL of the Ag sol prepared in step (1) and 20 mL of water, stir continuously at room temperature for 18 hours, wash and separate, and obtain a graphene oxide material with excellent surface enhancement. Mann effect graphene oxide / nano-Ag composite;

[0038] (4) the graphene oxide / nano-Ag composite prepar...

Embodiment 2

[0041] (1) Mix and stir 96mL deionized water and 4mL 1% chloroauric acid solution, heat to boiling, add 9.2mL 1% trisodium citrate solution, and continue to react for 20min to prepare Au sol;

[0042] (2) Weigh 30mg graphene oxide and disperse it in 300mL volume fraction of 1% methanol solution of 3-aminopropylethoxysilane, stir continuously at room temperature for 24h, then wash and separate the amino-modified graphene oxide Material;

[0043] (3) Disperse 1 mg of amino-modified graphene oxide material in 1 mL of water, mix evenly with 40 mL of the Au sol prepared in step (1), stir continuously at room temperature for 18 hours, wash and separate, and obtain an oxide with excellent surface-enhanced Raman effect. Graphene / nano-Au composite;

[0044] (4) the graphene oxide / nanometer Au composite that step (3) is prepared is redispersed in water, and concentration is 0.1mg / mL (in terms of the content of graphene), and 10 -6 The 4-mercaptopyridine aqueous solution of M was mixed...

Embodiment 3

[0046] (1) Mix and stir 96mL deionized water and 4mL 1% chloroauric acid solution, heat to boiling, add 9.2mL 1% trisodium citrate solution, and continue to react for 20min to obtain Au sol, and wait for it to cool naturally to room temperature After that, add 3mL 10 -1 M of ascorbic acid, stirred for 10min, added 7.5mL10 -2 M of AgNO3 solution, stirred for 20min. Obtain AuAg sol;

[0047] (2) Weigh 30mg graphene oxide and disperse it in 300mL volume fraction of 1% ethanol solution of 3-carboxypropylethoxysilane, stir continuously at room temperature for 24h, then wash and separate the carboxy-modified graphene oxide Material;

[0048] (3) Disperse 1mg of carboxy-modified graphene oxide material in 1mL of water, mix evenly with 40mL of AuAg sol prepared in step (1), stir continuously at room temperature for 18h, wash and separate, and obtain an oxidized material with excellent surface-enhanced Raman effect. Graphene / nano-AuAg composite;

[0049] (4) the graphene oxide / nan...

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Abstract

The invention discloses a preparation method of a composite material of graphene oxide / nanometer precious metal with a surface enhanced Raman effect. The preparation method comprises the following steps of: dispersing the graphene oxide into alcoholic solution of silane coupling agent; reacting to obtain a graphene oxide material grafted by the silane coupling agent; mixing the graphene oxide material with precious metalsol according to a certain proportion; and adsorbing and gathering precious metal nano-particles on the surface of graphene oxide to form the composite material of graphene oxide / nanometer precious metal. The method is simple to operate and has moderate reaction condition, and the size, the shape and the ingredients of the precious metal nano-particles can be adjusted flexibly. The invention simultaneously discloses the composite material of graphene oxide / nanometer precious metal prepared by the method, and the material has good water-solubility, large specific surface area, and can enrich target molecules in water to realize ultra-sensitive detection.

Description

technical field [0001] The invention relates to the field of nanomaterials, in particular to a graphene oxide / nano precious metal composite with surface-enhanced Raman effect. Background technique [0002] Raman spectroscopy can provide detailed structural information about the characteristic groups and stacking modes of molecules, and is not affected by solvent water. It can also select different wavelengths of excitation light according to different characteristics of the sample. As a conventional analysis and testing technology, it has It is widely used in the qualitative and quantitative analysis of chemical molecules. However, the Raman scattering cross-sectional area is small, requiring a relatively high concentration of the detected substance. [0003] Surface-enhanced Raman scattering (SERS) is a surface optical effect, and its discovery greatly improves the sensitivity of Raman spectroscopy: when molecules are adsorbed on the surface of nanoscale noble metals, due ...

Claims

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Application Information

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IPC IPC(8): B22F9/24C01B31/04B82Y40/00B82Y30/00C01B32/198
Inventor 钱志江程昱川郭建军王彪孙爱华许高杰刘丰华
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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