CN114672858A - Nano gold film for enhancing Raman scattering activity and preparation method thereof - Google Patents
Nano gold film for enhancing Raman scattering activity and preparation method thereof Download PDFInfo
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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- 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
Abstract
The invention discloses a nano gold film for enhancing Raman scattering activity and a preparation method thereof, wherein the nano gold film for enhancing Raman scattering activity comprises a conductive substrate and a three-dimensional multilayer gold nanoparticle film stacked on the conductive substrate; the thickness of the three-dimensional multilayer gold nanoparticle film is 0.1-2 mu m, the gold nanoparticles are of a sphere-like polyhedral structure, and the particle size is 150-400 nm. According to the nano gold film with enhanced Raman scattering activity and the preparation method thereof, after gold seed crystals are attached to the conductive substrate, the gold seed crystals are used as nucleation points, and the conductive substrate is cultivated by an electrodeposition method to form the three-dimensional multilayer gold nanoparticle film.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a nano gold film for enhancing Raman scattering activity and a preparation method thereof.
Background
The Surface Enhanced Raman Scattering (SERS) spectrum detection technology has wide application prospects in the fields of analytical chemistry, environmental pollutant monitoring, drug monitoring, food safety detection and the like. Due to the advantages of the resonance property of the surface plasmon, stable chemical property and the like, the gold nano unit assembled structure has wide application in the aspect of SERS spectrum.
Recently, some beneficial attempts and efforts have been made to obtain gold nano-unit assembled structures with surface plasmon resonance properties, such as articles entitled "Instant interfacial self-assembly for nanoparticles enabled consistent 'lift-on' thin film technology", sci. adv.2021, 7, eabk2852 ("conformal tirele film technology for preparing uniform nanoparticle monolayers based on transient interfacial self-assembly", Science Advances, volume 7, eabk2852, 2021). The single-layer gold nanoparticle film mentioned in the article is a film formed by assembling single-layer gold nanoparticles and covered on a substrate, and the preparation method comprises the steps of obtaining the single-layer film formed by assembling the gold nanoparticles by using a liquid level self-assembly method, and directly transferring the single-layer film to the surface of the substrate to obtain a product. Although the film has better uniformity, the film and the preparation method thereof have the following defects: firstly, the gold nanoparticles in the film are only a single layer, which not only restricts the activity of SERS, but also has very easy damage to the uniformity of the SERS by water waiting for detection solution, thereby seriously affecting the uniformity of SERS signals; secondly, the preparation method cannot obtain a thin film product with high SERS activity and without being damaged by water waiting for a detection solution.
In a patent with the invention name of 'gold nanoparticle assembled thin film and preparation method and application thereof' (with the publication number of CN106967978B) published in 2017, 7, 21 and 7, a gold nanoparticle assembled thin film and a preparation method thereof are disclosed. The film is a film which is formed by mutually adhering a plurality of layers of gold nano particles to form a thickness of 200nm-2 mu m and is covered on a conductive substrate, wherein the particle size of the gold nano particles is 30-120nm, and gaps or gaps which are less than or equal to 10nm are formed among the gold nano particles; the preparation method comprises the steps of sputtering a gold film on the surface of a conductive substrate to obtain the conductive substrate with the surface covered with the gold film, placing the conductive substrate with the surface covered with the gold film in a gold electrolyte by taking a graphite sheet as an anode and taking the conductive substrate with the surface covered with the gold film as a cathode, and performing electrodeposition under constant current to obtain a target product. However, in practical production, it has been found that when a gold film having the same thickness range is sputtered on the surface of a conductive substrate by a sputtering apparatus, it is difficult to prepare a target product by electrodeposition; the preparation method is highly dependent on sputtering instruments and experimental conditions, and the repeatability of the preparation method is poor, so that the application and popularization of the preparation method are severely restricted. In addition, the size of the gold nanoparticles has a remarkable influence on a surface plasmon resonance (LSPR) absorption peak, and the LSPR absorption peak can be adjusted from a purple light range to a near infrared range or even a middle infrared range by adjusting and controlling the size. Therefore, a new method is developed to prepare a film assembled by gold nanoparticles with larger size, and the method has important significance for controlling LSPR absorption peaks of the gold film and further applying to SERS detection with different excitation wavelengths.
Disclosure of Invention
Based on the technical problem, the invention provides a nano gold film for enhancing Raman scattering activity and a preparation method thereof.
The invention provides a nano gold film for enhancing Raman scattering activity, which comprises a conductive substrate and a three-dimensional multilayer gold nanoparticle film stacked on the conductive substrate;
the thickness of the three-dimensional multilayer gold nanoparticle film is 0.1-2 mu m, the gold nanoparticles are in a nearly spherical polyhedral structure, and the particle size is 150-400 nm.
Preferably, the three-dimensional multilayer gold nanoparticle film has a plurality of nano-voids among the gold nanoparticles, and the number of the nano-voids with the size less than or equal to 10nm accounts for not less than 80% based on the total number of all the nano-voids.
Preferably, the number of layers of the three-dimensional multilayer gold nanoparticle film is 2-6.
Preferably, the conductive substrate is a silicon wafer substrate, an indium tin oxide substrate or a fluorine-doped tin dioxide conductive glass substrate.
The invention provides a preparation method of the nano gold film for enhancing the Raman scattering activity, which comprises the following steps: after the gold seed crystals are attached to the conductive substrate, the conductive substrate with the gold seed crystals attached is used as a negative electrode, electrodeposition is carried out in a gold electrolyte containing a dispersing agent, and the gold seed crystals are used as nucleation points to culture and form the three-dimensional multilayer gold nanoparticle film on the conductive substrate.
Preferably, the "attaching gold seeds to a conductive substrate" has a structure including: uniformly coating the gold seed crystal solution on a conductive substrate, and drying to attach the gold seed crystal on the conductive substrate to obtain the conductive substrate attached with the gold seed crystal;
preferably, the gold seed crystal solution is obtained by dissolving a gold ion salt and a dispersant in water and then reducing the solution by a reducing agent under an acidic condition, wherein the gold ion salt is preferably gold chloride, the dispersant is preferably polyvinylpyrrolidone, the reducing agent is preferably sodium borohydride, and the particle size of the gold seed crystal is preferably 3-50 nm;
preferably, the coating method is a spin coating method, and the spin coating rotation speed is preferably 100-;
preferably, the conductive substrate is a silicon wafer substrate, an indium tin oxide substrate or a fluorine-doped tin dioxide conductive glass substrate.
Preferably, the gold electrolyte comprises a gold ion salt, a dispersant and an acid reagent;
preferably, the gold ion salt is gold chloride, the dispersant is polyvinylpyrrolidone, and the acid reagent is hydrochloric acid;
preferably, the mass ratio of the gold ion salt, the dispersing agent and the acid reagent is 2-10:100-300: 3-9.
Preferably, the electrodeposition parameters include: the current density is 10-30 muA/cm2The electrodeposition time is 0.5-6 h.
In the invention, the electrolyte comprising the gold ion salt, the dispersing agent and the acid reagent is selected, so that the deposition efficiency of gold particles can be enhanced, and the nano gold film which is relatively uniform in particle size, smooth in surface and stacked into a multilayer structure can be obtained; compared with an electrolyte only comprising gold ion salt and an acid reagent, the SERS electrolyte has more nanovoids with the size less than or equal to 10nm, so that higher SERS activity is obtained.
The invention also provides an application of the nano gold film for enhancing the Raman scattering activity, which comprises the following steps: and taking the nano gold film as a Raman detection substrate to carry out Raman detection on the object to be detected.
Preferably, the application of the nano gold film for enhancing raman scattering activity comprises the following steps: and taking the nano gold film as a Raman detection substrate, and carrying out Raman detection on rhodamine 6G under the condition that the excitation wavelength is 532 nm.
Compared with the prior art, the invention has the beneficial effects that:
(1) the nano gold film comprises a conductive substrate and a three-dimensional multilayer gold nanoparticle film stacked on the conductive substrate, the gold nanoparticles are of a large-size polyhedral structure similar to a sphere, and the nano gold film has a high specific surface area after being stacked and assembled together to obtain the nano gold film, so that the SERS activity is greatly improved; the gold nanoparticles are distributed in a staggered manner, nano gaps are formed between adjacent gold nanoparticles, and the gaps are connected with each other to form a network of gaps, so that the gaps are beneficial to becoming hot spots for inducing SERS; when the gold nanoparticles with the nearly spherical polyhedral structure are stacked, compared with the spherical gold nanoparticles, the gold nanoparticles have surface contact and only point contact, so that the former is higher than the latter in terms of stacking density, and the number of the nano-voids with the size less than or equal to 10nm is far higher than the latter on the basis of the total number of all nano-voids, so that the gold nanoparticles have higher SERS activity; the whole structure of the nano gold film is uniform, so that the nano gold film has high SERS activity, stability and uniformity; a plurality of gold nanoparticles are stacked to form a multilayer structure, so that the SERS activity of the gold nanoparticles can be improved by multiple times, and the phenomenon that the uniformity of SERS signals of the gold nanoparticles is damaged by the dissolution of solutions to be detected, such as water and the like, can be avoided.
(2) The gold nano-film is used as an SERS active substrate, and multiple times of multiple batches of tests are carried out on rhodamine 6G under different concentrations, so that the concentration of the rhodamine 6G as a tested object is as low as 10-11At mol/L, the method can still effectively detect the protein, and the consistency and repeatability of detection are very good for multiple points and any point on the product.
(3) The preparation method of the nano gold film is characterized in that a layer of gold seed crystal is uniformly covered on the surface of the conductive substrate, and the gold seed crystal is used as a nucleation point to grow on the conductive substrate through electrodeposition to form the gold nano particle film.
Drawings
FIG. 1 is a scanning electron microscope image of a nanogold thin film according to example 1 of the invention;
FIG. 2 is a cross-sectional scanning electron microscope of the nano-gold thin film according to example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the nano-gold thin film described in examples 2-6;
FIG. 4 is a scanning electron microscope photograph of a nanogold thin film according to comparative example 1;
FIG. 5 is a scanning electron microscope photograph of a nanogold thin film according to comparative example 2;
FIG. 6 is a Raman detection result spectrum of the nanogold film on rhodamine 6G described in example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples, but these examples should be explicitly mentioned for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a nano gold film for enhancing raman scattering activity, which is prepared by the following method:
(1) sequentially adding 3mg of gold chloride tetrahydrate and 0.3g of polyvinylpyrrolidone (K29-32) into 20mL of deionized water to form a mixed solution, then dropwise adding 200 mu L of hydrochloric acid with the concentration of 30g/L into the mixed solution, dropwise adding a sodium borohydride solution with the concentration of 1g/L into the mixed solution until the mixed solution becomes dark reddish brown to prepare a gold seed crystal solution, wherein the size range of gold seed crystal particles is 3-50nm, and sealing and standing for 24h for use;
(2) using ITO conductive glass with the thickness of 1.5mm, the area of 1cm multiplied by 3cm, the resistance of less than 6 omega and the transmittance of more than or equal to 84 percent as a conductive substrate, cleaning the ITO conductive glass by using ethanol and deionized water in sequence, spin-coating 100 mu L of the gold seed crystal solution on the ITO conductive glass uniformly at the rotating speed of 200r/min by using a spin-coating method, and drying the ITO conductive glass in an oven at the temperature of 80 ℃ to prepare the ITO conductive glass with a layer of gold seed crystal attached to the surface;
(3) sequentially adding 3mg of gold chloride tetrahydrate, 0.15g of polyvinylpyrrolidone (K29-32) and 200 mu L of hydrochloric acid with the concentration of 30g/L into 15mL of deionized water, and uniformly stirring to form a mixed solution, thereby preparing a gold electrolyte;
(4) using ITO conductive glass with a layer of gold seed crystal attached to the surface as a cathode, using a rectangular graphite sheet as an anode, placing the cathode in the gold electrolyte, and controlling the current density to be 25 muA/cm2Electrodepositing for 6h under the condition of constant current, and coating on ITO conductive glassGrowing gold nanoparticles by taking gold seed crystals as nucleation points to obtain the nano gold film;
(5) and (2) cleaning the nano-gold film for three times by using deionized water, soaking the nano-gold film in the deionized water for 30min to remove polyvinylpyrrolidone on the surface of the product, drying the obtained product at 60 ℃, and then carrying out scanning electron microscope detection, wherein the results are shown in fig. 1 and 2, fig. 1 is a scanning electron microscope image of the nano-gold film in example 1, and fig. 2 is a scanning electron microscope image of the cross section of the nano-gold film in example 1.
Referring to fig. 1 and 2, the gold nanoparticle film is a three-dimensional multilayer gold nanoparticle film, the thickness of the gold nanoparticle film is 0.8 μm, the gold nanoparticles are in a nearly spherical polyhedral structure, the particle size range is 150-400nm, the gold nanoparticle film has a plurality of nano-voids among the gold nanoparticles, and the number of layers of the gold nanoparticle film is 5.
The nano gold film is used as a Raman detection substrate, and a confocal laser Raman spectrometer is used for measuring the content of 2 multiplied by 10- 9mol/L and 1X 10-11Respectively characterizing the to-be-detected objects of the rhodamine 6G in mol/L, wherein the wavelength of exciting light of a laser Raman spectrometer is 532nm, the power is 0.1-2mW, the integration time is 1-120s, the detection result is shown in FIG. 6, and FIG. 6 is a Raman detection result spectrum of the nano gold film on the rhodamine 6G in the embodiment 1.
Referring to fig. 6, the nano gold thin film described in example 1 has very high SERS activity as a SERS substrate, and the detection concentration is as low as 1 × 10-11The SERS spectrum can still be obtained by mol/L rhodamine 6G, and the characteristic peak is more obvious.
Example 2
This example proposes a nano gold thin film with enhanced Raman scattering activity, which was prepared in the same manner as in example 1, except that in step (4), the current density was 25. mu.A/cm2And electrodepositing for 5s under the condition of constant current.
Example 3
This example proposes a nano gold thin film with enhanced Raman scattering activity, which was prepared in the same manner as in example 1, except that in step (4), the current density was 25. mu.A/cm2Constant current condition underLower electrodeposition 120 s.
Example 4
This example proposes a nano gold thin film with enhanced Raman scattering activity, which was prepared in the same manner as in example 1, except that in step (4), the current density was 25. mu.A/cm2Under constant current conditions, 180s of electrodeposition was carried out.
Example 5
This example proposes a nano gold thin film with enhanced Raman scattering activity, which was prepared in the same manner as in example 1, except that in step (4), the current density was 25. mu.A/cm2Under constant current conditions, the electrodeposition is carried out for 900 s.
The nanogold film in example 5 is used as a SERS substrate, and a SERS spectrum can be obtained only by detecting rhodamine 6G with high concentration.
Example 6
This example proposes a nano gold thin film with enhanced Raman scattering activity, which was prepared in the same manner as in example 1, except that in step (4), the current density was 25. mu.A/cm2Under constant current conditions, 1800s (0.5h) are electrodeposited.
The scanning electron microscope detection of the products obtained in examples 2-6 shows the results in FIG. 3, and FIGS. 3(a-e) are the scanning electron microscope images of the nano-gold films described in examples 2-6, respectively.
Referring to fig. 3, as the time for electrodeposition increases, the gold nanoparticles in the gold nanoparticle thin film become larger until stacked to form a three-dimensional multilayer gold nanoparticle film and have high SERS activity.
Comparative example 1
The comparative example provides a nano gold film for enhancing Raman scattering activity, which is prepared by the following method:
(1) using ITO conductive glass with the thickness of 1.5mm, the resistance of less than 6 omega and the transmittance of more than or equal to 84 percent as a conductive substrate, sequentially using ethanol and deionized water to clean the ITO conductive glass, and sputtering the ITO conductive glass by a sputtering instrument to form a gold film with the thickness of 10nm to prepare the ITO conductive glass with a layer of gold film attached to the surface;
(2) sequentially adding 3mg of gold chloride tetrahydrate, 0.15g of polyvinylpyrrolidone (K29-32) and 200 mu L of hydrochloric acid with the concentration of 30g/L into 15mL of deionized water, and uniformly stirring to form a mixed solution, thereby preparing a gold electrolyte;
(3) using ITO conductive glass with a layer of gold film attached to the surface as a cathode, using a rectangular graphite sheet as an anode, placing the cathode in the gold electrolyte, and controlling the current density to be 25 muA/cm2Carrying out electrodeposition for 6 hours under the condition of constant current to obtain the nano gold film;
(4) and (3) cleaning the nano-gold film for three times by using deionized water, soaking the nano-gold film in water for 30min, drying the obtained product at 60 ℃, and then carrying out scanning electron microscope detection, wherein the result is shown in figure 4, and figure 4 is a scanning electron microscope image of the nano-gold film in comparative example 1.
Referring to fig. 4, the nano gold thin film obtained in this comparative example produces a dense gold film, which has no significant gap, lacks hot spots, and has low SERS activity.
It can be known that the comparative example method is highly dependent on sputtering instruments and experimental conditions, and the preparation method has poor repeatability, thereby severely restricting the application and popularization of the preparation method.
Comparative example 2
The comparative example provides a nano gold film for enhancing Raman scattering activity, which is prepared by the following method:
(1) using ITO conductive glass with the thickness of 1.5mm, the resistance of less than 6 omega and the transmittance of more than or equal to 84 percent as a conductive substrate, and sequentially cleaning the ITO conductive glass by using ethanol and deionized water;
(2) sequentially adding 3mg of gold chloride tetrahydrate, 0.15g of polyvinylpyrrolidone (K29-32) and 200 mu L of hydrochloric acid with the concentration of 30g/L into 15mL of deionized water, and uniformly stirring to form a mixed solution, thereby preparing a gold electrolyte;
(3) the cleaned ITO conductive glass is used as a cathode, a rectangular graphite sheet is used as an anode, the cathode is placed in the gold electrolyte, and the current density is 25 muA/cm2Carrying out electrodeposition for 6 hours under the condition of constant current to obtain the nano gold film;
(4) and (3) cleaning the nano-gold film for three times by using deionized water, soaking the nano-gold film in water for 30min, drying the obtained product at 60 ℃, and then carrying out scanning electron microscope detection, wherein the result is shown in figure 5, and figure 5 is a scanning electron microscope image of the nano-gold film in the comparative example 2.
Referring to fig. 5, it can be seen that the au nanopyrases in the au nanopyrase film obtained in this comparative example have a large curvature area, but are dispersed in the film as a whole and in a small amount, and cannot form uniform hot spots in a large area.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The nano gold film for enhancing Raman scattering activity is characterized by comprising a conductive substrate and a three-dimensional multilayer gold nanoparticle film stacked on the conductive substrate;
the thickness of the three-dimensional multilayer gold nanoparticle film is 0.1-2 mu m, the gold nanoparticles are of a nearly spherical polyhedral structure, and the particle size is 150-400 nm.
2. The nanogold thin film for enhanced raman scattering activity according to claim 1, wherein said three-dimensional multilayer gold nanoparticle film has a plurality of nanovoids between gold nanoparticles; the number of the nano-voids with the size less than or equal to 10nm accounts for no less than 80 percent based on the total number of all the nano-voids.
3. The nanogold thin film with enhanced raman scattering activity according to claim 1 or 2, wherein the number of layers of the three-dimensional multilayer gold nanoparticle film is 2 to 6.
4. The nanogold thin film with enhanced raman scattering activity according to any one of claims 1 to 3, wherein the conductive substrate is a silicon wafer substrate, an indium tin oxide substrate or a fluorine-doped tin dioxide conductive glass substrate.
5. A method for preparing the nano gold film with the enhanced Raman scattering activity according to any one of claims 1 to 4, comprising: after the gold seed crystals are attached to the conductive substrate, the conductive substrate with the gold seed crystals attached is used as a negative electrode, electrodeposition is carried out in a gold electrolyte containing a dispersing agent, and the gold seed crystals are used as nucleation points to culture and form the three-dimensional multilayer gold nanoparticle film on the conductive substrate.
6. The method for preparing a nano gold film with enhanced raman scattering activity according to claim 5, wherein the step of attaching a gold seed crystal to a conductive substrate comprises: uniformly coating the gold seed crystal solution on a conductive substrate, and drying to attach the gold seed crystal on the conductive substrate to obtain the conductive substrate attached with the gold seed crystal;
preferably, the gold seed crystal solution is obtained by dissolving a gold ion salt and a dispersant in water and then reducing the solution by a reducing agent under an acidic condition, wherein the gold ion salt is preferably gold chloride, the dispersant is preferably polyvinylpyrrolidone, the reducing agent is preferably sodium borohydride, and the particle size of the gold seed crystal is preferably 3-50 nm;
preferably, the coating method is a spin coating method, and the spin coating rotation speed is preferably 100-;
preferably, the conductive substrate is a silicon wafer substrate, an indium tin oxide substrate or a fluorine-doped tin dioxide conductive glass substrate.
7. The method for preparing a nano gold film with enhanced raman scattering activity according to claim 5 or 6, wherein the gold electrolyte comprises a gold ion salt, a dispersant and an acid reagent;
preferably, the gold ion salt is gold chloride, the dispersant is polyvinylpyrrolidone, and the acid reagent is hydrochloric acid;
preferably, the mass ratio of the gold ion salt, the dispersant and the acid reagent is 2-10:100-300: 3-9.
8. According to the claimsThe method for preparing the nano gold film with the enhanced Raman scattering activity according to any one of claims 5 to 7, wherein the electrodeposition parameters comprise: the current density is 10-30 muA/cm2The electrodeposition time is 0.5-6 h.
9. Use of the nanogold thin film with enhanced raman scattering activity according to any one of claims 1 to 4, comprising: and taking the nano gold film as an enhanced Raman detection substrate to carry out Raman detection on the object to be detected.
10. Use of the nano-gold film for enhancing raman scattering activity according to claim 9, comprising: and taking the nano gold film as a Raman detection substrate, and carrying out Raman detection on rhodamine 6G under the condition that the excitation wavelength is 532 nm.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170115226A1 (en) * | 2015-10-23 | 2017-04-27 | King Fahd University Of Petroleum And Minerals | Anisotropic monolayer gold nanoassembly: a highly sers-active substrate for molecular detection |
| CN106967978A (en) * | 2017-05-03 | 2017-07-21 | 中国科学院合肥物质科学研究院 | Film of gold nano grain assembling and its production and use |
| CN108254355A (en) * | 2018-01-17 | 2018-07-06 | 安徽农业大学 | A kind of preparation method of salt bridge auxiliary primary battery induced growth gold nano grain surface enhanced Raman scattering substrate |
| CN109722683A (en) * | 2019-01-04 | 2019-05-07 | 中国科学院合肥物质科学研究院 | Gold nano structure and its preparation method and application with cone spiked surface |
| CN112893865A (en) * | 2021-03-26 | 2021-06-04 | 江苏师范大学 | Double-layer gold nanoparticle modified flexible SERS substrate and preparation method thereof |
| CN113092441A (en) * | 2021-04-08 | 2021-07-09 | 吉林大学 | Ultrasensitive biochip based on surface enhanced Raman scattering and preparation method thereof |
| CN113668029A (en) * | 2021-08-27 | 2021-11-19 | 安徽大学 | Film formed by rough gold nanoparticles and preparation method and application thereof |
-
2022
- 2022-04-27 CN CN202210448354.7A patent/CN114672858B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170115226A1 (en) * | 2015-10-23 | 2017-04-27 | King Fahd University Of Petroleum And Minerals | Anisotropic monolayer gold nanoassembly: a highly sers-active substrate for molecular detection |
| CN106967978A (en) * | 2017-05-03 | 2017-07-21 | 中国科学院合肥物质科学研究院 | Film of gold nano grain assembling and its production and use |
| CN108254355A (en) * | 2018-01-17 | 2018-07-06 | 安徽农业大学 | A kind of preparation method of salt bridge auxiliary primary battery induced growth gold nano grain surface enhanced Raman scattering substrate |
| CN109722683A (en) * | 2019-01-04 | 2019-05-07 | 中国科学院合肥物质科学研究院 | Gold nano structure and its preparation method and application with cone spiked surface |
| CN112893865A (en) * | 2021-03-26 | 2021-06-04 | 江苏师范大学 | Double-layer gold nanoparticle modified flexible SERS substrate and preparation method thereof |
| CN113092441A (en) * | 2021-04-08 | 2021-07-09 | 吉林大学 | Ultrasensitive biochip based on surface enhanced Raman scattering and preparation method thereof |
| CN113668029A (en) * | 2021-08-27 | 2021-11-19 | 安徽大学 | Film formed by rough gold nanoparticles and preparation method and application thereof |
Non-Patent Citations (5)
| Title |
|---|
| LIU, D: "Seed-assisted electrodeposition of multilayer Au nanoparticles-assembled films for sensitive surface-enhanced Raman scattering detection", MICROCHEMICAL JOURNAL, vol. 191, pages 1 - 8 * |
| WU, QIAO ; LUO, CHUNXIANG ; YU, HUIMIN ; KONG, GEZHI ; HU, JIAWEN: "Surface sol–gel growth of ultrathin SiO2 films on roughened Au electrodes: Extending borrowed SERS to a SERS inactive material", CHEMICAL PHYSICS LETTERS, vol. 608, pages 35 - 39 * |
| 张璐涛;周光明;张彩红;罗丹;: "新型膜状金纳米活性基底的制备及拉曼光谱增强研究", 光谱学与光谱分析, no. 06, pages 1741 - 1746 * |
| 朱储红;孟国文;王秀娟;: "金微/纳颗粒阵列的SERS效应研究", 光散射学报, no. 02, pages 116 - 119 * |
| 李玉;黄小平;王影;侯宇蒙;陈涛;张培锋;黄秋莹;赵青: "金纳米颗粒阵列基底的化学置换制备及其表面增强拉曼散射特性研究", 光谱学与光谱分析, vol. 37, no. 012, pages 3725 - 3729 * |
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