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Surface-enhanced Raman scattering substrate and preparation method and application thereof

A surface-enhanced Raman and substrate technology, applied in Raman scattering, measuring devices, instruments, etc., can solve the problems of difficult to obtain the deposition layer of nano-silver particles, high cost of SERS substrate preparation, and inability to use SERS detection, etc., to achieve performance Superior, high sensitivity, low cost effect

Active Publication Date: 2021-06-25
BEIJING CENT FOR DISEASE PREVENTION & CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main reasons that restrict the development of this technology to practical application are that the preparation cost of this SERS substrate is high, the technical operation is difficult, and it is difficult to obtain a deposition layer that can form uniform and dense nano-silver particles in a large area.
[0005] In addition, although SERS technology has the advantages of low cost, high sensitivity, and rapid analysis time, it cannot be detected by SERS for substances with weak SERS signals, and substances with small Raman scattering cross-sections or even no Raman vibrations.

Method used

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  • Surface-enhanced Raman scattering substrate and preparation method and application thereof
  • Surface-enhanced Raman scattering substrate and preparation method and application thereof
  • Surface-enhanced Raman scattering substrate and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Preparation of surface-enhanced Raman scattering substrate:

[0067] S1. NAAO@TA / Fe 3+ Preparation of the NAAO film: Soak the NAAO film in an aqueous solution of tannic acid at pH=7 for 1 hour, take it out, wash off the excess tannic acid on the surface with ultrapure water, and obtain NAAO@TA, and place the NAAO@TA in a 0.001mol / L FeCl 3 Incubate in an aqueous solution, take it out after 1 min, and soak it again in an aqueous solution of tannic acid at pH=7, so that Fe 3+ Complexation with tannic acid to obtain NAAO@TA / Fe 3+ ;

[0068] S2. Preparation of silver ammonia solution: 0.17gAgNO 3 Dissolve in 9.7mL water, add 0.3mL ammonia solution dropwise to obtain 0.1mol / L transparent silver ammonia solution;

[0069] S3. Preparation of surface-enhanced Raman scattering substrate: the NAAO@TA / Fe 3+ Soaked in 2mL 0.1mol / L silver ammonia solution, deposited in situ at 60°C for 4h to form NAAO@AgNS1.

Embodiment 2

[0071] Preparation of surface-enhanced Raman scattering substrate:

[0072] S1. NAAO@TA / Fe 3+ Preparation of the NAAO film: Soak the NAAO film in an aqueous solution of tannic acid at pH=7 for 1 hour, take it out, wash off the excess tannic acid on the surface with ultrapure water, and obtain NAAO@TA, and place the NAAO@TA in a 0.001mol / L FeCl 3 Incubate in an aqueous solution, take it out after 1 min, and soak it again in an aqueous solution of tannic acid at pH=7, so that Fe 3+ Complexation with tannic acid to obtain NAAO@TA / Fe 3+ ;

[0073] S2. Preparation of silver ammonia solution: 0.17gAgNO 3 Dissolve in 9.7mL water, add 0.3mL ammonia solution dropwise to obtain 0.1mol / L transparent silver ammonia solution;

[0074] S3. Preparation of silver growth medium: add 1mL 5mmol / L silver ammonia solution, 0.5mL 50mmol / L ascorbic acid, 0.5mL 1% (w / v) sodium citrate aqueous solution into 12.5mL water, mix well to obtain silver growth medium ;

[0075] S4. Preparation of surf...

Embodiment 3

[0089] Example 3 Surface-enhanced Raman scattering substrate NAAO@AgNS2 for testing fluoroacetic acid

[0090] S1. After incubating the surface-enhanced Raman scattering substrate NAAO@AgNS2 prepared in Example 2 with 0.001mol / L KSCN aqueous solution for 30min, the SCN - As internal standard, take it out, wash with pure water, and carry out quantitative determination;

[0091]S2. Add 0.01μmol / L-0.6μmol / L standard solution of fluoroacetic acid and 0.6μmol / L thiosalicylic acid into 0.2mL buffer solution containing 1.0mmol / L NaOH and 1.0mmol / L KI, at 90℃ After reacting for 30 minutes, the solution was transferred to a circular quartz measurement cell with a surface-enhanced Raman scattering substrate NAAO@AgNS2. After incubation for 1 hour, a random area on the surface-enhanced Raman scattering substrate film was selected under a microscope, and it was found that the There is basically no change in the Mann intensity, indicating that the substrate has a large area of ​​uniform...

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Abstract

The invention provides a surface-enhanced Raman scattering substrate and a preparation method and application thereof, and belongs to the technical field of surface-enhanced Raman scattering films, the surface-enhanced Raman scattering substrate comprises a substrate and a three-dimensional noble metal nanostructure; and the substrate is an NAAO film, and the noble metal is Ag. The preparation method comprises the following steps: complexing Fe < 3 + > and tannic acid (TA) on the surface of an NAAO film to obtain NAAO (at) TA / Fe < 3 + >, and further performing in-situ deposition in a silver-containing solution to form the surface-enhanced Raman scattering substrate. A step-by-step assembly method is adopted, a metal polyphenol coordination polymerization network is used for coating an NAAO film, a TA / Fe < 3 + > complex on the surface deposits a large-area uniform silver nanostructure (AgNS) on the NAAO substrate in situ, the surface enhanced Raman scattering substrate is prepared, the surface enhanced Raman scattering substrate has the advantages of uniformity, large area, high sensitivity and the like, and on-site detection of trace fluoroacetic acid can be achieved.

Description

technical field [0001] The invention relates to the technical field of surface-enhanced Raman scattering detection, in particular to a surface-enhanced Raman scattering substrate and a preparation method and application thereof. Background technique [0002] Fluoroacetic acid is a prohibited highly toxic rodenticide, which is widely used in agriculture. Because of its high acute toxicity and good chemical stability, it has caused many serious food poisoning incidents. Among them, the most famous one is the 2009 incident of Fonterra Group's commercial milk supply contaminated by fluoroacetic acid, which caused a huge panic and caused serious economic losses at that time. Although fluoroacetic acid has been banned and strictly regulated, it can still be used illegally for deliberate physical assault and terrorist activities. As a food precautionary measure, developing a rapid, low-cost, and convenient method for the detection of fluoroacetic acid in food and biological sample...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 孙洁芳邵兵张晶
Owner BEIJING CENT FOR DISEASE PREVENTION & CONTROL
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