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Preparation method of nano-silver/graphene derivative surface enhanced Raman substrate

A surface-enhanced, Raman matrix technology, applied in the field of molecular spectroscopic analysis and detection, can solve the problems of decreased sensitivity and accuracy, impact on performance, high energy consumption, etc., and achieve improved surface-enhanced Raman performance and strong surface-enhanced Raman performance , The effect of simple preparation method

Active Publication Date: 2015-01-07
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] 1. Some chemical solvents, surfactants, and reducing agents used in the synthesis process are toxic and have great environmental pollution problems;
[0007] 2. The synthesis process may be performed at a higher temperature and for a longer time, and consumes a lot of energy;
[0008] 3. It is difficult to control the size of nano-silver particles in the composite matrix, and it is impossible to achieve the optimal size that meets the performance
[0009] 4. The matrix material of some composite films, such as organic matrix, will affect the performance of surface-enhanced Raman, reducing its sensitivity and accuracy;
[0010] 5. The distance between nano-silver particles in the composite film is difficult to control, which affects its performance
[0011] 5. For the current nano-silver / graphene composite matrix, the influence of graphene on performance cannot be optimized

Method used

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  • Preparation method of nano-silver/graphene derivative surface enhanced Raman substrate
  • Preparation method of nano-silver/graphene derivative surface enhanced Raman substrate
  • Preparation method of nano-silver/graphene derivative surface enhanced Raman substrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Graphene derivative films help to adsorb sugar reducing agents and provide sites for the growth of nano silver particles. Therefore, graphene derivatives play a vital role; Example 1 refers to previous experience without graphene A silver mirror reaction is used to prepare a nano-silver film on the quartz substrate of the derivative film. The experimental steps are as follows:

[0044] 1) Pretreatment of the quartz substrate: The quartz substrate was ultrasonically cleaned in acetone, ethanol, and deionized water for 5 minutes, and then dried with nitrogen.

[0045] 2) The quartz substrate in step 1) is vertically immersed in a 10 mg / mL glucose aqueous solution for 20 minutes, then taken out, and dried with nitrogen.

[0046] 3) The configuration of silver ammonia solution: The configuration of silver ammonia solution: Under stirring conditions, add 2% aqueous ammonia solution dropwise to 0.4 mol / L concentration of silver salt aqueous solution until the precipitate is complet...

Embodiment 2

[0051] The difference between Example 2 and Example 1 is that the substrate is first coated with a graphene derivative film. Specific steps are as follows:

[0052] a) Preparation of graphene derivatives-graphene oxide film:

[0053] (1) Add graphene oxide powder to deionized water, add 0.1 mg graphene oxide per mL, and ultrasound for 2 h to obtain a graphene oxide colloidal solution.

[0054] (2) Add deionized water to PDDA with a mass fraction of 20%, and the volume ratio of deionized water to 20% PDDA is 4:1.

[0055] (3) Pretreatment of the quartz substrate: The quartz substrate was ultrasonically cleaned in acetone, ethanol, and deionized water for 5 minutes, and then dried with nitrogen.

[0056] (4) The pretreated quartz substrate was immersed in the graphene oxide solution for 20 minutes, then rinsed with deionized water, dried with nitrogen, immersed in the PDDA sol for 20 minutes, and rinsed with deionized water. Repeat this step once.

[0057] b) Put the graphene oxide film o...

Embodiment 3

[0064] The difference from embodiment 2 is that step a) in step (4) of embodiment 3 repeats this step twice.

[0065] image 3 (A) is the AFM image of the composite film. It can be clearly seen from the figure that the nano-silver particles uniformly cover the entire surface of the quartz substrate, and the size of the nano-particles has increased to 75 nm.

[0066] image 3 (B) It is the surface enhanced Raman diagram of crystal violet molecules of the composite film. It can be seen from the figure that the performance of the film has been greatly improved, and the surface Raman enhancement factor has been increased to 1.2*10 8 .

[0067] Example 3 once again proves that the graphene oxide film affects the growth of nano silver particles; comparing Examples 1 and 2, the performance of the composite film of Example 3 is greatly improved. This is not only because the size and number of nano-silver particles have increased, and the distance between the particles has decreased, but also...

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Abstract

The invention discloses a preparation method of a nano-silver / graphene derivative surface enhanced Raman substrate. The preparation method is characterized by uniformly adsorbing a reducing agent such as glucose on the surface of a graphene derivative ultrathin film through the adsorption of the graphene derivative ultrathin film, and growing a nano-silver thin film on the surface of the graphene derivative ultrathin film through the silver mirror reaction. The growth of the nano-silver thin film and the particle size and distribution of nano-silver are regulated and controlled by controlling the number of layers of the graphene derivative thin film and the concentration of a silver ammonia solution. The surface Raman enhanced performance of a composite film is regulated and controlled through the number of layers of the graphene derivative thin film and the morphology of the nano-silver thin film. Finally, a technological parameter of the optimal Raman enhanced performance is obtained.

Description

technical field [0001] The invention relates to the field of molecular spectrum analysis and detection, in particular to a method for preparing a nano-silver / graphene derivative surface-enhanced Raman matrix. Background technique [0002] Raman spectroscopy belongs to molecular vibration spectroscopy, which is the fingerprint of material molecules. Raman spectrometers made according to the Raman effect can be used to accurately and qualitatively identify samples. The analysis method of Raman spectroscopy generally does not require pretreatment of the sample, and it is easy to operate during the analysis process and the measurement time is short. It is a technology that can simultaneously perform qualitative and quantitative analysis of the sample. , food and other fields have extremely broad application prospects. But its disadvantage is low sensitivity, especially when detecting complex biological samples. At lower concentrations, ordinary Raman spectroscopy is insensitiv...

Claims

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Application Information

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IPC IPC(8): B22F9/24C23C18/44G01N21/65B82Y40/00
Inventor 周亚洲杨娟程晓农赵南马双彪郑思辉
Owner JIANGSU UNIV
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