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High-distribution density nanometer-spaced ordered array as well as preparation method and application thereof

A technology of distribution density and nano-gap, which is applied in the field of high-density distribution nano-gap ordered array and its preparation, can solve the problems of nanostructure unit gap control, uneven distribution of active sites, poor signal stability and reproducibility, etc. Achieve the effects of increased local electromagnetic field strength, improved sensitivity, and low cost

Inactive Publication Date: 2018-12-11
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

[0005] In order to solve the technical problems of the existing SERS substrates, such as uneven distribution of active sites, poor signal stability and reproducibility, and difficulty in controlling the gap between adjacent nanostructure units at the optimal gap distance, the present invention provides a A high-density nano-gap ordered array and its preparation method and application can control the gap between adjacent nano-structure units at the optimal gap distance, not only the distribution of active sites is uniform, the SERS sensitivity is high, the signal is stable and reproducible Good performance, and the preparation process is simple, fast and efficient, low cost, environmental protection and pollution-free, suitable for large-scale industrial production

Method used

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  • High-distribution density nanometer-spaced ordered array as well as preparation method and application thereof
  • High-distribution density nanometer-spaced ordered array as well as preparation method and application thereof
  • High-distribution density nanometer-spaced ordered array as well as preparation method and application thereof

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preparation example Construction

[0034] Specifically, the method for preparing an ordered array of nano-gap with high distribution density in the present invention includes the following steps:

[0035] (1) Step A. Place the precious metal nanoparticle array together with the substrate in a reactive ion etching machine for etching. The vacuum degree of the reactive ion etching machine is 150mT, the power is 50~200w, and the etching time is 2~ 30min, gas flow is CF 4 / O 2 =45 / 5Sccm (that is, the gas uses FC 4 With O 2 Mixed gas, and FC 4 The flow rate is 45Sccm, O 2 The gas flow rate is 5 Sccm), so as to prepare a high-distribution density nano-gap ordered columnar array template.

[0036] Among them, the substrate is preferably silicon wafer, quartz wafer or silicon dioxide wafer. The noble metal nano-particle array is an ordered single-layer noble metal nano-particle array that is uniformly grown on a substrate and arranged in a hexagonal tight arrangement, and the particle size of the noble metal nano-particles ...

Embodiment 1

[0049] A high-distribution density nano-gap ordered array, and its preparation method includes the following steps:

[0050] Step a1. Add chloroauric acid, diethylene glycol phthalate diacrylate (PDDA) and hydrochloric acid to the ethylene glycol solution, then heat to 195°C in an oil bath, keep it for 30 minutes, and then use a small amount of hydrochloric acid to wet By chemical etching, a monodisperse colloidal solution of gold ball nanoparticles is prepared.

[0051] Step b1. Centrifugal separation of the gold ball nanoparticle colloidal solution, the centrifugal separation speed is 10000-12000 rpm, the centrifugal separation treatment time is 10-30 minutes, remove the upper layer of the centrifuge tube, and repeat the centrifugation three times Separate, and then disperse the precipitate after centrifugation into the n-butanol solution, thereby preparing the n-butanol dispersion of gold ball nanoparticles.

[0052] Step c1: Use a gas-liquid interface self-assembly method to sel...

Embodiment 2

[0056] A high-distribution density nano-gap ordered array, and its preparation method includes the following steps:

[0057] Step a2. Add chloroauric acid, diethylene glycol diacrylate (PDDA) and hydrochloric acid to the ethylene glycol solution, then heat to 195°C in an oil bath, keep it for 30 minutes, and then use a small amount of hydrochloric acid to wet By chemical etching, a monodisperse colloidal solution of gold ball nanoparticles is prepared.

[0058] Step b2. Centrifugal separation of the gold ball nanoparticle colloidal solution, the centrifugal separation speed is 10000-12000 rpm, the centrifugal separation processing time is 10-30 minutes, the upper liquid of the centrifuge tube is removed, and the centrifugation is repeated three times Separate, and then disperse the precipitate after centrifugation into the n-butanol solution, thereby preparing the n-butanol dispersion of gold ball nanoparticles.

[0059] Step c2: Use the gas-liquid interface self-assembly method to ...

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Abstract

The invention discloses a high-distribution density nanometer-spaced ordered array as well as a preparation method and application thereof. The high-distribution density nanometer-spaced ordered arrayis an ordered columnar array with uniform morphology size, is in a hexagonal non-close arrangement manner, and uniformly grows on a substrate. In the ordered columnar array, the spacing between adjacent nano pillars is 5-30nm. The preparation method comprises the following steps: etching a precious metal nanoparticle array and the substrate in a reactive ion etching machine together, and coatingthe film, thereby obtaining the high-distribution density nanometer-spaced ordered array. The high-distribution density nanometer-spaced ordered array can directly serve as an SERS (Surface Enhanced Raman Scattering) substrate, and is used for detecting 4-ATP. The spacing between adjacent nano structured units can be controlled at the optimum spacing distance, the high-distribution density nanometer-spaced ordered array is uniform in active site distribution, high in SERS sensitivity, stable in signal and excellent in reproducibility, and the preparation process is simple, rapid, high-efficiency, low in cost, environmental-friendly and pollution-free and is suitable for large-scale industrial production.

Description

Technical field [0001] The invention relates to the technical field of surface enhanced Raman scattering substrate materials, in particular to a high-distribution density nano-gap ordered array and a preparation method and application thereof. Background technique [0002] Surface enhanced Raman scattering (SERS) effect, as a highly sensitive spectroscopic analysis technology, can provide rich fingerprint information of molecular structure and realize the detection of single molecular weight samples. It is widely used in food and medicine safety, Many fields such as biomedical analysis and environmental testing. [0003] The SERS substrate constructed based on the precious metal nanostructure unit has the advantages of simple preparation, easy storage, controllable active site distribution (in the prior art, the active site usually tends to the tip of the structure), etc., and has significant effects on many molecules The SERS enhancement effect of this product is widely favored b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65B82Y40/00
CPCB82Y40/00G01N21/658
Inventor 李越温路路孙一强蔡伟平
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI