A kind of reusable Raman enhanced substrate and its preparation method and application

A substrate and Raman technology, applied in Raman scattering, nanotechnology for sensing, nanotechnology for materials and surface science, etc., can solve the problem that uniformity affects the quality of SERS substrate, the uniformity of nanoparticles, The problem of high cost of physical methods can achieve the effect of improving SERS performance, improving optical absorption performance, and improving SERS performance

Active Publication Date: 2022-04-08
SOUTH CHINA NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, although these physical methods greatly improve the preparation efficiency of the substrate, the uniformity of the particles greatly affects the quality of the SERS substrate.
At the same time, due to the limitations imposed by the technology, these physical methods lead to the accumulation of nanoparticles in the vertical direction, so that the "hot spot" area between the nanoparticles is covered, thereby reducing the hot spot density on the entire substrate.
In addition, the disadvantages of physical methods such as high cost, harsh experimental conditions, and easy damage to the array structure have also brought great challenges to the development of the experiment.
It can be seen that there are three main problems in the construction process of the three-dimensional SERS substrate: 1. The uniformity of nanoparticles; 2. The density of hot spots caused by the accumulation of nanoparticles; 3. The limitation of experimental conditions

Method used

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  • A kind of reusable Raman enhanced substrate and its preparation method and application
  • A kind of reusable Raman enhanced substrate and its preparation method and application
  • A kind of reusable Raman enhanced substrate and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0050] A protocol for the preparation of a novel reusable Raman-enhanced substrate.

[0051] (1) ZnO seed crystal preparation: magnetron sputtering method, 1) with P(111) type single crystal silicon wafer as the substrate, P(111) type single crystal silicon wafer (1×1cm 2 ) Ultrasonic cleaning with acetone for 15 minutes before sputtering, rinse with deionized water, ultrasonic cleaning with absolute ethanol for 15 minutes, rinse with deionized water, and ultrasonic cleaning with deionized water for 15 minutes to ensure that the surface ions are completely removed. After cleaning, use nitrogen flow Blow dry and store in a vacuum. 2) Sputtering A ZnO ceramic target with a purity higher than 99.99% is used, and pre-sputtering is performed on it for 10 minutes to remove surface impurities. 3) Vacuum degree 3×10 -5 Torr, the vacuum atmosphere is Ar and O with a purity better than 99% 2 Gas mixture, the flow rate is 10:10 (sccm), the sputtering pressure is about 1Pa, the sputter...

Embodiment 2

[0058] The SERS performance of the new three-dimensional substrate was evaluated by using crystal violet and rhodamine B molecules.

[0059] (1) Prepare 5×10 -4 M crystal violet aqueous solution, take 10 μL and drop it on ZnO array, ZnO / AuNPs substrate, ZnO / Au / Ag 152 The surface of the three-dimensional SERS substrate was dried for SERS detection (the Raman spectrometer was Derbyshire, and the excitation wavelength was 785nm). see test results Image 6 , by comparison, it can be found that the deposition of AuNPs has greatly improved the SERS signal intensity of the three-dimensional ZnO array. Subsequently, Ag 152 (SCH 2 CH 2 Ph) 60 With the deposition of nanoclusters, the intensity of SERS signal was further enhanced. It can be seen that the nanoclusters have greatly enhanced the SERS performance of the substrate.

[0060] (2) Prepare 5×10 -3 to 5×10 -12Rhodamine B aqueous solution of M for testing ZnO / AuNPs substrates and ZnO / Au / Ag 152 Detection limits for 3D SER...

Embodiment 3

[0067] The recyclability of the novel 3D substrate was evaluated using rhodamine 6G molecule.

[0068] (2) Prepare 1×10 -6 M of rhodamine 6G aqueous solution, take 2mL of the solution in a cuvette, use an ultraviolet absorbance photometer (UV-6300, MAPADA) to detect the absorbance, and record. Subsequently, under the assisted condition of ZnO / AuNPs substrate, the degradation reaction was carried out for 90min under the ultraviolet light (~254nm, 8w), and the absorbance of the solution was detected every ten minutes, and recorded. Such as Figure 9 As shown, with the prolongation of the ultraviolet radiation time, the absorbance of rhodamine 6G aqueous solution gradually decreases. At the same time, it can be seen in the inserted figure that the color of rhodamine 6G aqueous solution gradually becomes lighter, which also shows that rhodamine 6G molecules are assisted on the ZnO / AuNPs substrate. gradually degrades under these conditions.

[0069] (2) Using the same experiment...

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Abstract

The invention discloses a reusable Raman enhanced substrate, a preparation method and application thereof. The method comprises the following steps: ZnO seed crystal preparation; ZnO array preparation; ZnO / AuNPs substrate preparation; ZnO / Au / Ag 152 Preparation of 3D SERS substrates. Due to Ag 152 (SCH 2 CH 2 Ph) 60 The particle size of nanoclusters is extremely small, not only will not cover the hot spots on the original AuNPs film during the deposition process, but will further increase the hot spot density on its surface; greatly improving the SERS performance of the original substrate. The substrate of the present invention has good uniformity and signal reproducibility (RSD=6.95%), and can realize trace detection of analyte (5×10 ‑12 M), the enhancement factor can reach 6.48×10 9 , and can achieve cyclic detection. The method has the advantages of simple preparation process, low cost, high sensitivity, recyclable use and the like, and is suitable for mass production.

Description

technical field [0001] The invention belongs to the technical field of functionalized nanometer materials, and in particular relates to a reusable Raman enhanced substrate and its preparation method and application. Background technique [0002] Since surface-enhanced Raman scattering (SERS) can perform trace detection and provide unique fingerprint peaks for analytes, it has been widely used in various fields. SERS is mainly derived from the near field of surface plasmon polaritons generated by the interaction between the laser source and the SERS substrate. Therefore, the quality of the SERS substrate will directly affect the sensitivity and accuracy of detection. Usually, the construction of the substrate is a process of establishing SERS active sites (called "hot spots"). The "hot spots" mainly exist in the gaps between the metal nanoparticles and are accompanied by extremely high electric field enhancement. Therefore, the number of "hot spots" has a great influence o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65C01G9/02C01G9/03C23C14/35C23C14/08C23C14/58B22F9/24B22F1/054B82Y30/00B82Y40/00B82Y15/00
CPCG01N21/658C01G9/02C01G9/03C23C14/35C23C14/086C23C14/5806B22F9/24B82Y30/00B82Y40/00B82Y15/00B22F1/054
Inventor 胡勇军王俊杰余星星庄秀眉王琪胡婕妤
Owner SOUTH CHINA NORMAL UNIVERSITY
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