CN112229829A - Surface-enhanced Raman substrate and preparation method and application thereof - Google Patents

Surface-enhanced Raman substrate and preparation method and application thereof Download PDF

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Publication number
CN112229829A
CN112229829A CN202011058622.1A CN202011058622A CN112229829A CN 112229829 A CN112229829 A CN 112229829A CN 202011058622 A CN202011058622 A CN 202011058622A CN 112229829 A CN112229829 A CN 112229829A
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China
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enhanced raman
metal matrix
detection
substrate
mesh
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Inventor
莫文雄
乔胜亚
李光茂
熊俊
王勇
朱晨
杨森
陈莎莎
周鸿铃
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Guangzhou Power Supply Bureau of Guangdong Power Grid Co Ltd
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Guangzhou Power Supply Bureau of Guangdong Power Grid Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The invention relates to a surface-enhanced Raman substrate and a preparation method and application thereof. The surface-enhanced Raman substrate comprises a metal matrix and a metal nano structure modified on the surface of the metal matrix, wherein the metal matrix is of a mesh structure. According to the invention, the metal matrix with the mesh structure is selected, so that the surface-enhanced Raman substrate can realize positioning and marking; in the Raman detection, the position of the surface enhanced Raman substrate is screened and marked to obtain a detection site, and the Raman detection is carried out on the marked site, so that the enhancement effect of the surface enhanced Raman substrate is consistent, and the repeatability of the detection result is good. The surface-enhanced Raman substrate obtained by modifying the surface of the metal matrix has the advantages of uniform surface nanostructure size, good compactness and good Raman enhancement effect. The surface-enhanced Raman substrate provided by the invention is good in signal enhancement effect when applied to furfural detection, high in detection repeatability and beneficial to realizing in-situ furfural detection.

Description

Surface-enhanced Raman substrate and preparation method and application thereof
Technical Field
The invention relates to the field of power transformers, in particular to a surface-enhanced Raman substrate and a preparation method and application thereof.
Background
The Raman scattering spectroscopy is an efficient and nondestructive detection method and is widely applied to various fields. Raman spectroscopy based on raman scattering effects allows for the determination of the structure and content of a substance. The qualitative and quantitative analysis of the substance can be carried out through the Raman scattering spectrogram. However, the cross section of the Raman scattering is small, so that the development of the Raman scattering in the field of trace substance detection is limited. The Surface-Enhanced Raman Scattering (SERS) effect refers to a phenomenon that in a specially prepared metal good conductor Surface or sol, in an excitation region, a Raman Scattering signal of an adsorbed molecule is greatly Enhanced compared with a Normal Raman Scattering (NRS) signal due to enhancement of an electromagnetic field on the Surface or near the Surface of a sample. The Surface Enhanced Raman Spectroscopy (SERS) technology improves the sensitivity of Raman detection and solves the problem of low sensitivity of trace substance detection to a certain extent. However, the enhancement effect of different SERS substrates is different, and the effect on the raman detection result is large.
The operation condition of the power transformer is related to the safety and stability of the operation of a power grid, and the furfural is an important index for evaluating the oil paper insulation aging of the transformer. Therefore, the method can accurately detect the furfural dissolved in the transformer oil, so as to judge the aging degree of the oil paper insulating material of the transformer, and is the key for ensuring the stable operation of the power transformer, preventing the large-area accident of the power grid and ensuring the safety and the stability of the power grid. The surface appearance uniformity and the enhancement effect of different positions of the existing chemically prepared SERS substrate have certain difference, the position screening of the substrate and the fixed-point positioning detection of furfural at different positions are difficult to realize, and a preparation method of the SERS substrate with good Raman enhancement effect and high consistency is sought for realizing the accurate, rapid and efficient in-situ detection of furfural in transformer oil. Therefore, the preparation of the SERS substrate is the key for developing the surface enhanced Raman spectroscopy technology, and the SERS substrate has important significance for Raman in-situ detection of furfural in transformer oil.
Disclosure of Invention
Therefore, a surface-enhanced raman substrate with good raman enhancement effect and high consistency, a preparation method thereof and a raman spectrum detection method are needed to be provided.
The invention provides a surface-enhanced Raman substrate which comprises a metal matrix and a metal nano structure modified on the surface of the metal matrix, wherein the metal matrix is in a mesh structure.
In some of these embodiments, the metal matrix has a mesh opening size of 200 to 400 mesh.
In some of these embodiments, the mesh of the metal matrix is circular, pentagonal, or hexagonal.
In some of these embodiments, the metal matrix has a mesh that is distributed in an array.
In some embodiments, the metal substrate is made of gold, silver or copper.
In some of these embodiments, the metal nanostructures are nanoplatelets, nanowires, or nanoparticles; and/or
The metal nano structure is made of gold, silver or copper.
In some embodiments, the metal matrix is a copper mesh with mesh openings of 200-400 meshes, the mesh openings are regular hexagons, the mesh openings are distributed in an array, and the metal nano-structures are silver nano-particles with diameters of 100-300 nm.
The metal substrate of the surface enhanced Raman substrate is of a mesh structure, and a metal nano structure is modified on the surface of the metal substrate. The mesh structure of the metal matrix enables the surface-enhanced Raman substrate to be positioned through the positions of the meshes, and the detection positions on the surface-enhanced Raman substrate are marked through the distribution positions of the meshes. Compared with the traditional surface enhanced Raman substrate, the surface enhanced Raman substrate can realize accurate positioning and marking through the mesh structure of the metal matrix, so that the position with high Raman enhancement effect uniformity can be screened out for Raman detection, and the repeatability for Raman detection is high. The metal nano structure is modified on the surface of the metal matrix, so that the surface enhanced Raman substrate has a rough surface, the specific surface area is increased, and the Raman signal enhancement effect is good.
The invention also provides a preparation method of the surface enhanced Raman substrate, which comprises the following steps:
carrying out surface modification on the metal matrix to enable the surface of the metal matrix to be modified with a metal nano structure;
wherein, the metal matrix is in a mesh structure.
According to the preparation method of the surface enhanced Raman substrate, the metal matrix with the mesh structure is selected, the metal nano structure is modified on the surface of the metal matrix, so that the prepared surface enhanced Raman substrate has the mesh structure which is the same as that of the metal matrix, the mesh structure enables the surface enhanced Raman substrate to be positioned through the positions of meshes, the detection positions on the surface enhanced Raman substrate are marked through the distribution positions of the meshes, and the surface enhanced Raman substrate with a good Raman enhancement effect and high consistency can be obtained.
Meanwhile, the surface enhanced Raman substrate prepared by the preparation method of the surface enhanced Raman substrate has good modification morphology uniformity at the same position and high Raman signal enhancement effect consistency.
The invention also provides application of the surface-enhanced Raman substrate in Raman spectrum detection.
The invention also provides a Raman spectrum detection method, which comprises the following steps:
screening and marking the surface enhanced Raman substrate to obtain a detection site;
placing the surface enhanced Raman substrate in a liquid sample to be tested;
acting a liquid sample to be detected on the surface enhanced Raman substrate, and taking the detection site for Raman detection;
the surface enhancement substrate comprises a metal matrix and a metal nano structure modified on the surface of the metal matrix, wherein the metal matrix is in a mesh structure.
According to the Raman spectrum detection method, the surface-modified metal nano structure is adopted, the metal matrix is the surface-enhanced Raman substrate with the mesh structure, the surface-enhanced Raman substrate can be accurately positioned through the meshes on the metal matrix, and detection sites with compact surface modification and good Raman enhancement effect can be conveniently screened and marked for Raman spectrum detection. By performing Raman detection on the detection sites obtained by screening and marking, the obtained detection result has good enhancement effect and high consistency, the repeatability of the Raman detection is ensured, and the detection result is reliable.
Drawings
FIG. 1 is a microscope (a) of a surface-enhanced Raman substrate before surface modification and a microscope (b) of a surface-enhanced Raman substrate after surface modification according to the present invention;
FIG. 2 shows a 10 μm high power microscope image (a) and a 500nm high power microscope image (b) of the surface enhanced Raman substrate of the present invention;
FIG. 3 is a Raman spectrum (a) of the surface enhanced Raman substrate for furfural detection and a Raman spectrum (b) of the surface enhanced Raman substrate for furfural detection without the substrate;
FIG. 4 is a Raman spectrum of 20 sets of surface enhanced substrates prepared under the same conditions for detecting a furfural oil sample under the same positioning coordinates;
FIG. 5 shows 1702cm in Raman spectrogram of 20 sets of surface enhanced substrates prepared under the same conditions for detecting furfural oil samples under the same positioning coordinates-1Statistical plots of the intensity of the raman characteristic peaks.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
An embodiment of the present invention provides a surface-enhanced raman scattering substrate, which includes a metal matrix and a metal nanostructure modified on a surface of the metal matrix, wherein the metal matrix is a mesh structure.
In some of these embodiments, the metal matrix has a mesh opening size of 200 mesh to 400 mesh.
Preferably, the aperture of the metal matrix is 400 meshes, and the Raman enhancement effect of the surface-enhanced Raman substrate is good at the aperture.
In some of these embodiments, the mesh of the metal matrix is circular, pentagonal, or hexagonal. Preferably, the meshes of the metal matrix are regular hexagons.
In some of these embodiments, the metal matrix has a mesh pattern. The mesh structure of the array distribution facilitates the marking on the surface enhanced Raman substrate through the mesh. It will be appreciated that location coordinates may be established on the mesh structure distributed in the array, and the location of each mesh may be determined from the location coordinates to locate and mark each mesh.
In some embodiments, the metal substrate is made of gold, silver or copper.
In some embodiments, the metal nanostructure is a nanosheet, nanowire or nanoparticle, and/or the metal nanostructure is gold, silver or copper.
On the surface of a good metal conductor with a rough surface, such as gold, silver, copper and the like, a Raman scattering signal is greatly enhanced compared with a common Raman scattering signal.
In some embodiments, the metal matrix is a copper mesh with mesh openings of 200-400 meshes, the mesh openings are regular hexagons, the mesh openings are distributed in an array, and the metal nano-structure is silver nano-particles with the diameter of 100-300 nm.
The metal substrate of the surface enhanced Raman substrate is of a mesh structure, and a metal nano structure is modified on the surface of the metal substrate. The mesh structure of the metal matrix enables the surface-enhanced Raman substrate to be positioned through the positions of the meshes, and the detection positions on the surface-enhanced Raman substrate are marked through the distribution positions of the meshes. Compared with the traditional surface enhanced Raman substrate, the surface enhanced Raman substrate can realize accurate positioning and marking through the mesh structure of the metal matrix, so that the position with high Raman enhancement effect uniformity can be screened out for Raman detection, and the repeatability for Raman detection is high. The metal nano structure is modified on the surface of the metal matrix, so that the surface enhanced Raman substrate has a rough surface, the specific surface area is increased, and the Raman signal enhancement effect is good.
The embodiment of the invention also provides a preparation method of the surface-enhanced Raman substrate, which comprises the following steps:
carrying out surface modification on the metal matrix to enable the surface of the metal matrix to be modified with a metal nano structure;
wherein, the metal matrix is in a mesh structure.
In some embodiments, the metal substrate is made of gold, silver or copper. Furthermore, the material of the metal nano structure is gold, silver or copper.
In some embodiments, the material of the metal substrate is selected to have a greater reactivity than the metal nanostructures. Therefore, the metal nano structure can be formed by utilizing the high activity of the metal matrix and taking the metal matrix as an in-situ reaction point by adopting a chemical replacement method.
In a specific example, the material of the metal substrate is copper, that is, the metal substrate is a copper mesh; the metal nanostructures are silver nanoparticles. Specifically, the step of performing surface modification on the metal substrate to modify the metal nanostructure on the surface of the metal substrate comprises:
preparing a silver nitrate solution;
adding a silver nitrate solution to the copper mesh, and reacting to obtain the copper mesh with the surface modified with the silver nanoparticles;
and washing the copper net with the surface modified with the silver nanoparticles.
In some embodiments, the step of modifying the surface of the metal substrate with the metal nanostructures further includes a step of pretreating the copper mesh, and the step of pretreating the copper mesh includes:
soaking the copper mesh in ethanol and deionized water, and removing dirt on the surface of the copper mesh by ultrasonic;
soaking the copper mesh in dilute hydrochloric acid to remove oxides on the surface of the copper mesh;
washing the copper mesh with ethanol and deionized water, and drying;
the dried copper mesh was fixed on a quartz glass plate.
In the embodiment of the invention, the ethanol used is absolute ethanol.
Specifically, the copper mesh is soaked in dilute hydrochloric acid for 3min to remove the oxide on the surface of the copper mesh.
Further, in the preparation method of the surface-enhanced Raman substrate, the drying temperature is 40-60 ℃, and the drying time is 5-20 min. Preferably, the drying temperature is 40 ℃ and the drying time is 5 min.
Dirt and oxides on the surface of the copper mesh are removed through pretreatment, and then the metal nano structure is modified on the surface, so that the prepared surface enhanced Raman substrate nano structure is uniform in size, and good in uniformity and compactness. The copper net is fixed on the quartz glass through pretreatment, so that the positioning and the marking of the surface enhanced Raman substrate are facilitated.
According to the preparation method of the surface enhanced Raman substrate, the metal matrix with the mesh structure is selected, the metal nano structure is modified on the surface of the metal matrix, so that the prepared surface enhanced Raman substrate has the mesh structure which is the same as that of the metal matrix, the mesh structure enables the surface enhanced Raman substrate to be positioned through the positions of meshes, the detection positions on the surface enhanced Raman substrate are marked through the distribution positions of the meshes, and the surface enhanced Raman substrate with a good Raman enhancement effect and high consistency can be obtained.
Meanwhile, the surface enhanced Raman substrate prepared by the preparation method of the surface enhanced Raman substrate has good modification morphology uniformity at the same position and high Raman signal enhancement effect consistency.
The invention also provides application of the surface enhanced Raman substrate in Raman spectrum detection.
The invention also provides a Raman spectrum detection method, which comprises the following steps:
step S1: screening and marking the surface enhanced Raman substrate to obtain a detection site;
step S2: placing the surface-enhanced Raman substrate in a liquid sample to be tested;
step S3: acting a liquid sample to be detected on the surface enhanced Raman substrate, and taking a detection site for Raman detection;
the surface enhanced substrate comprises a metal matrix and a metal nano structure modified on the surface of the metal matrix, and the metal matrix is of a mesh structure.
In some embodiments, the step of screening and labeling the surface enhanced raman substrate to obtain detection sites comprises:
and (3) acquiring photos through electron microscope scanning and a CMOS camera, screening and marking detection positions with good surface modification uniformity and compactness as detection sites.
Specifically, screening and marking the surface enhanced Raman substrate are realized through mesh positioning of a metal matrix, coordinates are established for a mesh structure, and screened positions for detection are marked through the coordinates to obtain detection sites.
Further, in some embodiments, the step of screening and labeling the surface-enhanced raman substrate to obtain the detection sites further comprises:
and performing Raman detection on the plurality of detection sites, and screening the detection sites with good Raman enhancement effect for subsequent detection steps.
In some of these embodiments, the liquid test sample is a furfural oil sample.
According to the Raman spectrum detection method, the surface-modified metal nano structure is adopted, the metal matrix is the surface-enhanced Raman substrate with the mesh structure, the surface-enhanced Raman substrate can be accurately positioned through the meshes on the metal matrix, and detection sites with compact surface modification and good Raman enhancement effect can be conveniently screened and marked for Raman spectrum detection. By performing Raman detection on the detection sites obtained by screening and marking, the obtained detection result has good enhancement effect and high consistency, the repeatability of the Raman detection is ensured, and the detection result is reliable.
The Raman spectrum detection method is used for furfural detection, has good Raman enhancement effect, and has enhancement factor of 10 compared with common Raman detection Raman signal enhancement3～104And the Raman detection result of the same detection site has small relative error, high consistency and good repeatability. The Raman spectrum detection method is used for furfural detection, and can realize accurate, quick and efficient in-situ detection of furfural in transformer oil.
The invention will now be described in more detail with reference to specific examples, which are intended to illustrate the invention further, but not to limit it. The instruments and reagents used in the examples are all commercially available. To help better understand the technical scheme of the present application, the following analysis is performed with pure furfural as a material.
The Raman detection platform of the following specific embodiment adopts a 532nm laser, a Leica DM2700 type positive microscope, an Andor SR-500i dispersion type Raman spectrometer and an Andor iDus-416 type CCD. The microscope beam path uses a 50 × long-focus objective. The reading and refrigerating temperature of the CCD detector can reach-75 ℃, the monitoring wavelength range is 200-1100 nm, the pixel is 2000 multiplied by 256, the dark current is less than 0.0006e/s/pixel, and the Raman scattering wavelength monitoring of trace furfural dissolved in the transformer oil can be met.
Example 1
(1) A400-mesh copper net carrying net is prepared, holes on the copper net are regular hexagonal holes, the center distance is 75 mu m, the rib width is 10 mu m, and the hole diameter is 65 mu m. Soaking the copper mesh in absolute ethyl alcohol and deionized water, and performing ultrasonic treatment for 2 min. Then the copper mesh is soaked for 3min by dilute hydrochloric acid. The markable copper screen was then rinsed again with absolute ethanol and deionized water and placed in a vacuum oven to dry for 5min at 40 ℃. And finally, fixing the copper net on the quartz glass sheet.
(2) A0.4 mM silver nitrate solution was prepared by dissolving 0.0136g of silver nitrate in 200mL of absolute ethanol. Then, the prepared silver nitrate solution with the concentration of 0.4mM is dripped on the pretreated copper mesh for waiting for reaction for 10min, and the copper mesh is observed to change from purple red to grey white. And washing the surface enhanced Raman substrate with absolute ethyl alcohol and deionized water, and drying in a vacuum drying oven at 40 ℃ for 5min for later use.
(3) And observing the surface enhanced Raman substrate by a CMOS camera, screening out the positions with good surface modification uniformity and compactness, and marking the screened positions by the coordinates of meshes to obtain detection sites.
(4) A transformer oil sample with a furfural concentration of 88mg/L was prepared. Carrying out Raman detection on the oil sample under the detection site of the prepared surface enhanced Raman substrate; in addition, the Raman detection is directly carried out without adding an SERS substrate. And obtaining a Raman spectrogram, determining a Raman characteristic peak of the furfural, and judging the substrate enhancement effect.
When 0.4mM silver nitrate solution was added to the pretreated copper mesh and reacted for 10 minutes, the surface of the copper mesh was observed to change from copper red to off-white. Referring to fig. 1, the copper mesh after being treated with 0.4mM silver nitrate solution changes from copper red (fig. 1(a)) to grey white (fig. 1(b)), and the copper mesh after surface modification is slightly rougher than that before surface modification. Referring to fig. 2, the silver nanoparticles modified on the surface of the surface enhanced raman substrate prepared in example 1 have uniform size, good uniformity and good compactness. The silver nanoparticles covered on the surface of the metal substrate are in a uniform nano-block structure by controlling the concentration of the silver nitrate solution to be 0.4 mM. Referring to fig. 3, compared with the raman detection directly, the surface enhanced raman substrate prepared in example 1 has good enhancement performance for performing raman detection on furfural oil sample, and furfural content is 1702cm-1The Raman characteristic peak signal is obviously enhanced, and the enhancement factor is 103～104。
Example 2
Preparing 20 groups of surface enhanced Raman substrates according to the steps (1) and (2) in the example 1, wherein the sample number of the surface enhanced Raman substrate is 1-20, and carrying out Raman detection on the furfural oil sample in the step (4) in the example 1 under the same positioning coordinate marked in the step (3). And calculating the strong relative standard error of the Raman characteristic peak, and comparing the repeatability of the Raman characteristic peak.
Fig. 4 is a raman spectrum of 20 sets of surface enhanced raman substrates prepared under the same conditions in example 2 for furfural oil-like detection. Referring to FIG. 5, the Raman spectrum of FIG. 4 is at 1702cm-1Statistical analysis of Raman characteristic peak intensity at 1702cm-1The relative standard error of the Raman characteristic peak intensity is 4.58%, and the repeatability is good within the acceptable error range.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The surface-enhanced Raman substrate is characterized by comprising a metal matrix and a metal nano structure modified on the surface of the metal matrix, wherein the metal matrix is in a mesh structure.
2. The surface-enhanced raman substrate according to claim 1, wherein a mesh aperture of the metal matrix is 200 to 400 mesh.
3. The surface-enhanced raman substrate according to claim 1, wherein the mesh of said metal matrix is circular, pentagonal or hexagonal.
4. The surface-enhanced raman substrate according to claim 1, wherein the meshes of said metal matrix are distributed in an array.
5. The surface-enhanced raman substrate according to claim 1, wherein the metal matrix is made of gold, silver or copper.
6. The surface-enhanced Raman substrate of any one of claims 1 to 5 wherein the metallic nanostructures are nanoplates, nanowires, or nanoparticles; and/or
The metal nano structure is made of gold, silver or copper.
7. The surface-enhanced Raman substrate of claim 1, wherein the metal matrix is a copper mesh with mesh openings of 200-400 meshes, the mesh openings are regular hexagons, the mesh openings are distributed in an array, and the metal nanostructures are silver nanoparticles with diameters of 100-300 nm.
8. A preparation method of a surface enhanced Raman substrate is characterized by comprising the following steps:
carrying out surface modification on the metal matrix to enable the surface of the metal matrix to be modified with a metal nano structure;
wherein, the metal matrix is in a mesh structure.
9. Use of a surface enhanced raman substrate according to any one of claims 1 to 7 in raman spectroscopy detection.
10. A Raman spectrum detection method is characterized by comprising the following steps:
screening and marking the surface enhanced Raman substrate to obtain a detection site;
placing the surface enhanced Raman substrate in a liquid sample to be tested;
acting a liquid sample to be detected on the surface enhanced Raman substrate, and taking the detection site for Raman detection;
the surface enhancement substrate comprises a metal matrix and a metal nano structure modified on the surface of the metal matrix, wherein the metal matrix is in a mesh structure.
CN202011058622.1A 2020-09-30 2020-09-30 Surface-enhanced Raman substrate and preparation method and application thereof Pending CN112229829A (en)

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