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Method for preparing surface-enhanced Raman scattering substrate by solution method and application

A surface-enhanced Raman and solution method, applied in Raman scattering, material excitation analysis, etc., can solve the problems of inability to obtain SERS active substrate, unable to prepare with SERS substrate, and lack of surface-enhanced "hot spots" to achieve uniformity Good, reproducible, and low-cost effects

Active Publication Date: 2013-10-09
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2011, a domestic scientific research team used the capillary effect-assisted method to realize the preparation of randomly distributed SERS substrates of gold nano-islands (Adv. Therefore, the uniformity of large-area preparation is difficult to control
However, the spacing of gold nano-islands obtained by this technique is greater than 10nm, and there is no surface-enhanced "hot spot" on the substrate, so it cannot be used for the preparation of SERS substrates.
[0004] The purpose of the present invention is to solve the problem that the SERS active substrate cannot be obtained by the solution method preparation technology, using gold nanoparticles modified with low-boiling thiol ligands as raw materials, and providing a solution of gold nano-island films with a clean surface and enhanced "hot spots" method of preparation

Method used

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  • Method for preparing surface-enhanced Raman scattering substrate by solution method and application
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  • Method for preparing surface-enhanced Raman scattering substrate by solution method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1) Synthesis of gold nanoparticles with a diameter of 1-5nm;

[0037] (1) Dissolve 1.5g tetraoctyl ammonium bromide in 80ml toluene, then add 0.32g HAuCl 4 ·H 2 O and 1ml of pure water. Toluene phase changes to brownish yellow.

[0038] (2) Under stirring, 3mmol hexanethiol was added thereto, and the brownish-yellow solution quickly became colorless, and the stirring was continued for 10min at room temperature.

[0039] (3) Add 20 ml of an aqueous solution of 0.28 g of sodium borohydride into the solution under stirring, and the organic phase turns black. After continuous stirring for 4h, the reaction was stopped.

[0040] (4) The organic phase was separated, and the toluene was evaporated under reduced pressure with a rotary evaporator.

[0041] (5) Collect black gold nanoparticles, ultrasonically disperse them in methanol, wash away impurities in the product, centrifuge the product after washing 5 times, and vacuum dry to obtain metal nanoparticles with a diamete...

Embodiment 2

[0050] 1) Synthesis of gold nanoparticles with a diameter of 1-5nm;

[0051] (1) Dissolve 1.5g tetraoctyl ammonium bromide in 80ml toluene, then add 0.32g HAuCl 4 ·H 2 O and 1ml of pure water. Toluene phase changes to brownish yellow.

[0052] (2) Under stirring, 3 mmol of pentanethiol was added thereto, and the brown-yellow solution quickly became colorless, and the stirring was continued for 10 min at room temperature.

[0053] (3) Add 20 ml of an aqueous solution of 0.28 g of sodium borohydride into the solution under stirring, and the organic phase turns black. After continuous stirring for 2 h, the reaction was stopped.

[0054] (4) The organic phase was separated, and the toluene was evaporated under reduced pressure with a rotary evaporator.

[0055] (5) Collect black gold nanoparticles, ultrasonically disperse them in methanol, wash away impurities in the product, centrifuge the product after washing 5 times, and vacuum dry to obtain metal nanoparticles with a dia...

Embodiment 3

[0063] 1) Synthesis of gold nanoparticles with a diameter of 1-5nm;

[0064] (1) Dissolve 1.5g tetraoctyl ammonium bromide in 80ml toluene, then add 0.32g HAuCl 4 ·H 2 O and 1ml of pure water. Toluene phase changes to brownish yellow.

[0065] (2) Under stirring, 3mmol octyl mercaptan was added thereto, the brownish yellow solution quickly became colorless, and the stirring was continued for 10min at room temperature.

[0066] (3) Add 20 ml of an aqueous solution of 0.28 g of sodium borohydride into the solution under stirring, and the organic phase turns black. After continuous stirring for 4h, the reaction was stopped.

[0067] (4) The organic phase was separated, and the toluene was evaporated under reduced pressure with a rotary evaporator.

[0068] (5) Collect black gold nanoparticles, ultrasonically disperse them in methanol, wash away impurities in the product, centrifuge the product after washing 5 times, and vacuum dry to obtain metal nanoparticles with a diamete...

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Abstract

The invention relates to a method for preparing surface-enhanced Raman scattering (SERS) substrate by a solution method and application, and belongs to the technical field of SERS substrates. The method comprises the following steps: preparing hydrocarbyl mercaptan modified metal nanoparticles with the diameter of 1 to 5 nm; dissolving the metal nanoparticles with the diameter of 1 to 5 nm into an organic solvent to prepare metal nanoparticle sol of 60 to 100 mg / ml; and coating the metal nanoparticle sol on a substrate, placing a sample coated with a metal colloid film in a precise muffle furnace or a tube furnace, heating to 140 to 250 DEG C within 5 minutes, maintaining for 5 to 30 minutes, and cooling to room temperature. When the SERS substrate obtained by the method is applied to detection of rhodamine 6G and 4-mercaptopyridine, the enhancement factor is 107, and the relative standard difference of Raman signal intensity distribution at different positions is 5%.

Description

technical field [0001] The invention belongs to the technical field of surface-enhanced Raman substrates, and relates to the preparation of metal nanostructures based on surface-enhanced Raman scattering effects, in particular to a large-area, low-cost preparation method for Raman scattering-enhanced substrates based on gold nanomaterials, and using this A substrate was used to detect rhodamine 6G molecules and 4-mercaptopyridine molecules in solution. Background technique [0002] Surface-enhanced Raman scattering (SERS) spectroscopy has been proven to be an ultrafast and versatile analytical technique with a detection limit of single molecular weight and carrying fingerprint vibration information of the measured molecule. This technology is an important means to solve a series of social problems, such as: food safety detection, early diagnosis of diseases, environmental pollution detection, terrorist threats, and has broad application prospects. With the improvement of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
Inventor 刘红梅张新平
Owner BEIJING UNIV OF TECH
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