Gold-silver nano cone array with body-enhanced Raman scattering effect as well as preparation method thereof and use thereof

A technology that enhances Raman scattering and silver nanometers. It is applied in Raman scattering, nanotechnology for materials and surface science, and nanotechnology. It can solve the problems of poor product stability, complicated preparation process, and poor uniformity. The method is simple, the signal repeatability is good, and the structure is stable.

Active Publication Date: 2020-07-28
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

Although this product has a certain volume-enhanced Raman scattering effect, there are unsatisfactory aspects of the product and its preparation method. First, the enhancement mode of the product is single, and only a high-intensity electromagnetic field is distributed in the hollow area of ​​​​the nanocone. The improvement of VERS activity is limited; secondly, because the high-intensity electromagnetic field is mainly concentrated on the upper end of the hollow nanocone with a pore size of about 100nm, the size of the analyte to be measured is limited due to the small range; thirdly, due to the restriction of the bowl-shaped substrate, by The uniformity of the array composed of nanocone holes is poor, which affects the repeatability of the detection signal; again, because the evaporated gold film is very thin and has no stable support, the stability of the product is poor; finally, the preparation process is more difficult. It is complicated, it is difficult to achieve large-scale production, and it is impossible to obtain a detection substrate with better volume-enhanced Raman scattering effect

Method used

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  • Gold-silver nano cone array with body-enhanced Raman scattering effect as well as preparation method thereof and use thereof
  • Gold-silver nano cone array with body-enhanced Raman scattering effect as well as preparation method thereof and use thereof
  • Gold-silver nano cone array with body-enhanced Raman scattering effect as well as preparation method thereof and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The specific steps of preparation are:

[0048] Step 1. Place the nickel imprint mold of the hexagonal array nano-pillar array with a period of 495nm, a diameter of 105nm and a height of 150nm on the aluminum sheet and place it at 8kN / cm. 2 The aluminum sheet with dents was obtained for 5 minutes under the same pressure. Then, anodize the aluminum sheet with dents for 3min, wet etching, 5min anodization, wet etching and 3min anodization in sequence; among them, the voltage of anodization is 200V, and the temperature of the electrolyte is A mixture of 100:100:2 ethylene glycol, 5wt% citric acid and 85wt% phosphoric acid with a volume ratio of 10°C. The etching solution for wet etching is a 5wt% phosphoric acid solution with a temperature of 45°C. The time is 80 minutes, and the inverted cone-shaped porous alumina template is obtained.

[0049] Step 2: Firstly, vapor-deposit a 70nm thick gold film on the inverted cone-shaped porous alumina template to obtain an inverted cone-...

Embodiment 2

[0052] The specific steps of preparation are:

[0053] Step 1. Place the nickel imprint mold of the hexagonal array nano-pillar array with a period of 498nm, a diameter of 103nm and a height of 163nm on the aluminum sheet, and place it at 9kN / cm. 2 The aluminum sheet with dents was obtained under a pressure of 4.5 min. Then the aluminum sheet with dents was subjected to 3.5min anodization, wet etching, 4.5min anodization, wet etching and 3.5min anodization in sequence; among them, the voltage of the anodization was 200V, and the electrolyte It is a mixture of ethylene glycol, 5wt% citric acid and 85wt% phosphoric acid at a temperature of 10℃ and a volume ratio of 100:100:1.7. The etching solution for wet etching is 5wt% phosphoric acid at a temperature of 48℃ Solution, soaking time is 75min, to obtain inverted cone-shaped porous alumina template.

[0054] In step 2, a gold film with a thickness of 75 nm is vapor-deposited on the inverted cone-shaped porous alumina template to obta...

Embodiment 3

[0057] The specific steps of preparation are:

[0058] Step 1. First, the nickel imprint mold of the hexagonal array nano-pillar array with a period of 500nm, a diameter of 100nm and a height of 175nm is attached to the aluminum sheet and placed at 10kN / cm 2 The aluminum sheet with dents was obtained for 4 minutes under the same pressure. Then, anodize the aluminum sheet with dents for 4 minutes, wet etching, 4 minutes anodization, wet etching, and 4 minutes anodization in sequence; among them, the voltage of anodization is 200V, and the temperature of the electrolyte is A mixture of 100:100:1.3 ethylene glycol, 5wt% citric acid and 85wt% phosphoric acid with a volume ratio of 10℃. The etching solution for wet etching is a 5wt% phosphoric acid solution with a temperature of 50℃. The time is 70 minutes, and the inverted cone-shaped porous alumina template is obtained.

[0059] In step 2, an 80nm thick gold film is vapor-deposited on the inverted cone-shaped porous alumina template ...

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Abstract

The invention discloses a gold-silver nano cone array with body-enhanced Raman scattering effect as well as a preparation method thereof and use thereof. The array is a nano cone ordered array with acone bottom diameter of 500-520 nm, a cone top diameter of 115-125 nm, bone height of 465-475 nm and spacing less than or equal to 10 nm between adjacent two cone bottoms, wherein the cone is formed by coating a silver nano film outside a gold nano film, and the cone is arranged on a flat plate shaped polymethyl methacrylate substrate. The method comprises the following steps: laminating a hexagonally arranged nano pillar array nickel coining die and an aluminum sheet, performing multi-time anode oxidizing and wet-process etching on the aluminum sheet with concave marks, evaporating a gold film on an obtained inverted-cone-shaped porous aluminum oxide template, coating a polymethyl methacrylate solution on the aluminum oxide template; etching off the aluminum oxide template which is sequentially coated with the gold film and polymethyl methacrylate in the inverted-cone-shaped porous aluminum oxide template, and then, sputtering a silver film on a gold nano cone ordered array on the polymethyl methacrylate substrate to obtain a target product. The gold-silver nano cone array can be used for trace detection of rhodamine or crystal violet or malachite green on a body-enhanced Raman scattering active substrate.

Description

Technical field [0001] The invention relates to a nano-cone array and a preparation method and application thereof, in particular to a gold-silver nano-cone array with volume-enhanced Raman scattering effect, and a preparation method and application thereof. Background technique [0002] Surface-enhanced Raman Scattering (SERS) spectroscopy with the advantages of high sensitivity, short detection time, fingerprint information characteristics, and no complicated sample pre-processing, etc., in the fields of environmental pollutant detection, reaction monitoring, food safety detection, and biosensing have a broad vision of application. At present, the "hot spot" mode based on the SERS substrate is single. In order to further improve the detection performance of the SERS substrate, people have made some useful attempts and efforts, such as the title "Volume-Enhanced Raman Scattering Detection of Viruses", Small, 2019, 15( 11):1805516. ("Volume Enhanced Raman Scattering for Virus De...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/18C23C14/16C23C14/24C23C14/34C25D11/12C25D11/16C23C14/02G01N21/65B82Y40/00B82Y30/00
CPCC23C14/18C23C14/24C23C14/3442C23C14/165C23C14/021C25D11/12C25D11/16G01N21/658B82Y30/00B82Y40/00
Inventor 孟国文闫思思陈斌黄竹林
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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