CN110702660A - Novel nano gold film anti-counterfeiting method based on surface enhanced Raman spectroscopy - Google Patents
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Abstract
The invention relates to a novel nano-gold film anti-counterfeiting method based on a surface enhanced Raman spectrum technology. The method comprises the steps of firstly preparing Au NRs with a certain length-diameter ratio by adopting a crystal seed growth method, preparing Au @ Au NRs with a nano core-shell structure on the basis, coating different Raman probes in core-shell gaps of the Au @ Au NRs, mixing the Au @ Au NRs coated with the different Raman probes in multiple proportions and multiple components, preparing a compound Au @ Au NRs film by adopting an oil-water interface self-assembly technology, and transferring the film to a flexible PDMS substrate. The Au @ Au NRs loaded with different Raman probes has excellent SERS activity and unique SERS signals, the compound nano-film obtained by mixing multiple components in multiple proportions further improves the density of SERS signals, the unique signals are utilized to manufacture anti-counterfeiting safety marks, and the products can be endowed with safety information with non-replicability and extremely high identification precision, so that the identification between genuine products and counterfeit and shoddy products can be realized, and a new idea is provided for developing a novel anti-counterfeiting technology.
Description
Technical Field
The invention relates to preparation and anti-counterfeiting application of a double-layer gold nanorod film based on a surface enhanced Raman spectroscopy technology, and belongs to the technical anti-counterfeiting field.
Background
Raman Scattering (Raman Scattering) occurs when light irradiates the surface of a substance, fingerprint information of a compound molecular structure is carried in the Raman Scattering light, and a Surface Enhanced Raman Scattering (SERS) technology based on Raman Scattering derivation is a quick, sensitive, strong-specificity and nondestructive technical means, and can provide structural information of the related substance on a molecular level. Raman probe molecules such as MBA, MMTAA, DTNB and the like have excellent Raman signals, and meanwhile, the Raman signals of the Raman probe can be greatly enhanced by the gold nanorod made of the noble metal material. Different Raman probes are selected to be packaged in the nanometer core-shell gap of the Au @ AuNRs, and each obtained Au @ Au NRs corresponds to a specific SERS signal. The Au @ Au NRs loaded with different Raman probes is subjected to multi-component multi-proportion mixing and assembled into a film, the safety mark manufactured by utilizing the SERS signal compounded with the Au @ Au NRs film has extremely high distinguishing precision and non-reproducibility, meanwhile, the Au @ Au NRs film can be integrated on different substrates, and the safety mark has very high stability and SERS signal reproducibility, and provides a theoretical basis for anti-counterfeiting application of the Au @ Au NRs film based on the SERS technology.
Disclosure of Invention
The Au @ AuNRs with the nano core-shell structure is prepared by adopting a seed crystal growth method, different Raman probes are coated in core-shell gaps of the Au @ AuNRs, the Au @ AuNRs coated with the different Raman probes are subjected to multi-proportion multi-component mixing, a multi-proportion multi-component mixed compound Au @ AuNRs film is assembled by adopting an oil-water interface self-assembly technology and is transferred to a flexible PDMS substrate, unique SERS signals of the Au @ AuNRs film loaded with the Raman probes mixed in different proportions can be given, and the signals have extremely high distinguishing precision and irreproducibility and can be used as anti-counterfeiting safety information.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
(1) preparing double-layer gold nanorods: cetyl Trimethyl Ammonium Bromide (CTAB) solution and water (H) are added in sequence2O)、Chloroauric acid (HAuCl)4) Solution and sodium borohydride (NaBH)4) Placing the solution in a dark place to obtain a gold nanorod seed solution; to a cetyltrimethylammonium bromide (CTAB) solution was added successively chloroauric acid (HAuCl)4) Solution, silver nitrate (AgNO)3) Solution, sulfuric acid (H)2SO4) The solution and ascorbic acid (L-AA) solution can obtain a gold nanorod growth solution; adding a certain amount of seed solution into the growth solution, carrying out water bath and dark incubation for a certain time, and then centrifuging and washing the obtained solution for multiple times to complete the preparation of the gold nanorod (Au NRs) solution. Diluting gold nanorod (Au NRs) solution, taking a certain amount of solution, adding different Raman probe (MBA, MMTAA and DTNB) solutions, stirring at room temperature for a certain time, centrifuging and concentrating, and sequentially adding Cetyl Trimethyl Ammonium Bromide (CTAB) solution, polyvinylpyrrolidone (PVP) solution and silver nitrate (AgNO)3) Adding solution, ascorbic acid (L-AA) solution and sodium hydroxide (NaOH) solution, incubating in water bath in dark for a certain time, and adding chloroauric acid (HAuCl)4) Slowly heating the solution, keeping the solution for a certain time, and centrifugally washing the solution for many times to finish the preparation of the double-layer gold nanorods (Au @ AuNRs) containing different Raman probes (MBA, MMTAA and DTNB).
(2) Preparing an anti-counterfeiting film based on double layers of gold nanorods: mixing the double-layer gold nanorod (Au @ Au NRs) solutions encapsulating different Raman probes (MBA, MMTAA and DTNB) according to different components in different proportions, and adding water (H) into the mixed double-layer gold nanorod (Au @ Au NRs) solution2O) and polyvinylpyrrolidone (PVP) solution as water phase, and adding dodecyl mercaptan (DDT) solution as oil phase into n-hexane solution. The water phase and the oil phase are transferred into a small beaker in sequence, so that the oil-water separation phenomenon can occur, and the absolute ethyl alcohol is slowly injected into an oil-water interface by using an injector, so that a layer of double-layer gold nanorod (Au @ Au NRs) film with metal mirror luster is observed to be formed on the oil-water interface.
(3) Transferring the anti-counterfeiting film based on the double-layer gold nanorods: shearing a PDMS substrate prepared in advance into a square of 8mm multiplied by 8mm, standing a small beaker for a certain time, removing an upper oil phase in the beaker by using a liquid-transferring gun, waiting for natural volatilization of the residual oil phase, enabling the PDMS substrate to be parallel to an oil-water interface, and dipping and transferring a double-layer gold nanorod (Au @ Au NRs) film from bottom to top.
The concentration of CTAB solution in the step (1) is 0.1-1mol/L, HAuCl4The concentration of the solution is 1-100mmol/L, NaBH4The concentration of the solution is 1-100mmol/L, AgNO3The concentration of the solution is 1-100mmol/L, H2SO4The concentration of the solution is 0.1-1mol/L, the concentration of the L-AA solution is 0.1-1mol/L, the concentration of the Raman probe solution is 1-10mmol/L, the concentration of the PVP solution is 1-10%, and the concentration of the NaOH solution is 0.1-1 mol/L.
In the preparation of the gold nanorod seed solution in the step (1), the dosage of the CTAB solution is 1-10mL, and HAuCl4The dosage of the solution is 0.1-1mL, NaBH4The dosage of the solution is 0.1-1 mL; in the preparation of the gold nanorod growth solution, the dosage of CTAB solution is 50-150mL, HAuCl4The dosage of the solution is 1-10mL, AgNO3The dosage of the solution is 0.1-5mL, H2SO4The dosage of the solution is 0.1-5mL, and the dosage of the L-AA solution is 0.1-1 mL; in the preparation of the gold nanorod solution, the dosage of the seed solution added into the growth solution is 0.1-1 mL.
The dosage of the gold nanorod solution diluted in the step (1) is 1-10mL, and the dosage of the Raman probe solution is 0.1-5 mL; after centrifugal concentration, the dosage of the added CTAB solution is 0.1-5mL, the dosage of the PVP solution is 1-10mL, and AgNO3The dosage of the solution is 0.1-5mL, the dosage of the L-AA solution is 0.1-1mL, the dosage of the NaOH solution is 0.1-1mL, and the dosage of the HAuCl solution is4The dosage of the solution is 1-10 mL.
In the preparation of the seed solution in the step (1), the seed solution is placed in a dark place for 1 to 5 hours; in the preparation of the gold nanorod solution, the temperature of a water bath is 1-50 ℃, and the time for placing the water bath in a dark place is 10-20 h; the frequency of the gold nanorod solution centrifugal washing is 1-5.
The gold nanorod solution in the step (1) is diluted by 10-100 times; after the Raman probe solution is added, stirring for 1-10h at room temperature; the temperature of the water bath is 1-50 ℃, and the time of the water bath for dark incubation is 1-10 h; adding HAuCl4Heating the solution to80-100 ℃; keeping the temperature for 1-60min after heating; the times of centrifugal washing of the double-layer gold nanorod solution are 1-5 times.
The concentration of the double-layer gold nanorod mixed solution packaged with the Raman probe in the step (2) is 1-100mmol/L, the concentration of the PVP solution is 1-10%, and the concentration of DDT in the n-hexane solution is 0.1-1 mg/L.
The dosage of the double-layer gold nanorod mixed solution packaged with the Raman probe in the step (2) is 1-10mL, and H is2The dosage of O is 1-10mL, the dosage of PVP solution is 1-10mL, the dosage of n-hexane solution is 1-30mL, and the dosage of absolute ethyl alcohol is 1-10 mL.
The injection speed of the absolute ethyl alcohol in the step (2) is 0.1-1 mL/min.
And (4) standing the small beaker in the step (3) for 1-3 h.
The invention has the advantages that:
the double-layer core-shell structure gold nanorod loaded with different Raman probes has excellent SERS activity and unique SERS signals, the nano-film obtained by compounding Au @ Au NRs loaded with different Raman probes further improves the density of SERS signals, and different compounding components and proportions correspond to different SERS information, so that the double-layer core-shell structure gold nanorod has remarkable advantages in the aspect of anti-counterfeiting. The unique signal is processed into a specific safety mark, the Au @ Au NRs film loaded with the anti-counterfeiting code is detected by Raman detection equipment, and the obtained spectrogram is compared with the safety mark to realize the identification between a genuine product and a fake and counterfeit product, so that a new idea is provided for technical anti-counterfeiting.
Drawings
The drawings are only for purposes of illustrating and explaining the present invention and are not to be construed as limiting the scope of the present invention. Wherein:
FIG. 1: is a graph showing the results of example 1 of the present invention. Au @ AuNRs film.
FIG. 2: is a graph showing the results of example 2 of the present invention. The Raman probe is an SERS image of an Au @ Au NRs film of DTNB.
FIG. 3: is a graph showing the results of example 3 of the present invention. And SERS images of the Au @ Au NRs thin film mixed according to the ratio of MBA to DTNB being 1: 2 and corresponding safety marks.
Detailed Description
The invention is described below in connection with specific embodiments with the attached figures. Unless otherwise specified, the technical means used in the present invention are well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various changes or modifications in the components and amounts of the materials used in these embodiments can be made without departing from the spirit and scope of the invention.
Example 1: an oil-water interface self-assembly technology is adopted to prepare a compound Au @ AuNRs film for multi-component and multi-proportion mixing of different Raman probes, and the compound Au @ AuNRs film is transferred to a flexible PDMS substrate. As shown in FIG. 1, the Au @ AuNRs film has a metallic mirror surface gloss, and still maintains a highly reflective mirror surface effect after being transferred to a PDMS substrate.
Example 2: raman testing is carried out on the Au @ Au NRs nano film loaded with the DTNB Raman probe, and an obtained SERS spectrogram is shown in figure 2.
Example 3: scanning SERS spectrogram of the Au @ Au NRs film obtained by mixing the MBA and DTNB Raman probes according to a certain proportion, as shown in figure 3, the spectrogram characteristic peak of the compounded Au @ AuNRs SERS film is mainly concentrated near the peak position of the Raman probe used for mixing, and the specific peak position and the specific intensity are different according to different proportions. And carrying out certain treatment on the generated SERS spectrogram to convert the SERS spectrogram into a specific security identifier. The application of the security mark in the aspect of anti-counterfeiting can be realized by using the security mark and SERS spectrogram of the anti-counterfeiting film for comparison and identification.
Claims (10)
1. A new nano-gold film anti-counterfeiting method based on a surface enhanced Raman spectroscopy technology comprises the following steps:
(1) preparing double-layer gold nanorods: sequentially adding Cetyl Trimethyl Ammonium Bromide (CTAB) solutionLiquid, water (H)2O), chloroauric acid (HAuCl)4) Solution and sodium borohydride (NaBH)4) Placing the solution in a dark place to obtain a gold nanorod seed solution; to a cetyltrimethylammonium bromide (CTAB) solution was added successively chloroauric acid (HAuCl)4) Solution, silver nitrate (AgNO)3) Solution, sulfuric acid (H)2SO4) The solution and ascorbic acid (L-AA) solution can obtain a gold nanorod growth solution; adding a certain amount of seed solution into the growth solution, carrying out water bath and dark incubation for a certain time, and then centrifuging and washing the obtained solution for multiple times to complete the preparation of the gold nanorod (AuNRs) solution. Diluting gold nanorod (Au NRs) solution, taking a certain amount of solution, adding different Raman probe (MBA, MMTAA and DTNB) solutions, stirring at room temperature for a certain time, centrifuging and concentrating, and sequentially adding Cetyl Trimethyl Ammonium Bromide (CTAB) solution, polyvinylpyrrolidone (PVP) solution and silver nitrate (AgNO)3) Adding solution, ascorbic acid (L-AA) solution and sodium hydroxide (NaOH) solution, incubating in water bath in dark for a certain time, and adding chloroauric acid (HAuCl)4) Slowly heating the solution, keeping the temperature for a certain time, and centrifugally washing the solution for multiple times to finish the preparation of double-layer gold nanorods (Au @ Au NRs) containing different Raman probes (MBA, MMTAA and DTNB).
(2) Preparing an anti-counterfeiting film based on double layers of gold nanorods: mixing the double-layer gold nanorod (Au @ Au NRs) solutions encapsulating different Raman probes (MBA, MMTAA and DTNB) according to different components in different proportions, and adding water (H) into the mixed double-layer gold nanorod (Au @ Au NRs) solution2O) and polyvinylpyrrolidone (PVP) solution as water phase, and adding dodecyl mercaptan (DDT) solution as oil phase into n-hexane solution. The water phase and the oil phase are transferred into a small beaker in sequence, so that the oil-water separation phenomenon can occur, and the absolute ethyl alcohol is slowly injected into an oil-water interface by using an injector, so that a layer of double-layer gold nanorod (Au @ Au NRs) film with metal mirror luster is observed to be formed on the oil-water interface.
(3) Transferring the anti-counterfeiting film based on the double-layer gold nanorods: shearing a PDMS substrate prepared in advance into a square of 8mm multiplied by 8mm, standing a small beaker for a certain time, removing an upper oil phase in the beaker by using a liquid-transferring gun, waiting for natural volatilization of the residual oil phase, enabling the PDMS substrate to be parallel to an oil-water interface, and dipping and transferring a double-layer gold nanorod (Au @ Au NRs) film from bottom to top.
2. The new anti-counterfeiting method for the nano-gold film based on the surface-enhanced Raman spectroscopy technology according to claim 1, wherein the concentration of the CTAB solution in the step (1) is 0.1-1mol/L, and HAuCl is added4The concentration of the solution is 1-100mmol/L, NaBH4The concentration of the solution is 1-100mmol/L, AgNO3The concentration of the solution is 1-100mmol/L, H2SO4The concentration of the solution is 0.1-1mol/L, the concentration of the L-AA solution is 0.1-1mol/L, the concentration of the Raman probe solution is 1-10mmol/L, the concentration of the PVP solution is 1-10%, and the concentration of the NaOH solution is 0.1-1 mol/L.
3. The novel method for preventing forgery of gold nano-film based on surface-enhanced Raman spectroscopy according to claim 1, wherein in the preparation of gold nanorod seed solution in the step (1), the amount of CTAB solution is 1-10mL and HAuCl is used4The dosage of the solution is 0.1-1mL, NaBH4The dosage of the solution is 0.1-1 mL; in the preparation of the gold nanorod growth solution, the dosage of CTAB solution is 50-150mL, HAuCl4The dosage of the solution is 1-10mL, AgNO3The dosage of the solution is 0.1-5mL, H2SO4The dosage of the solution is 0.1-5mL, and the dosage of the L-AA solution is 0.1-1 mL; in the preparation of the gold nanorod solution, the dosage of the seed solution added into the growth solution is 0.1-1 mL.
4. The novel nano-gold film anti-counterfeiting method based on the surface-enhanced Raman spectroscopy technology according to claim 1, wherein the amount of the gold nanorod solution diluted in the step (1) is 1-10mL, and the amount of the Raman probe solution is 0.1-5 mL; after centrifugal concentration, the dosage of the added CTAB solution is 0.1-5mL, the dosage of the PVP solution is 1-10mL, and AgNO3The dosage of the solution is 0.1-5mL, the dosage of the L-AA solution is 0.1-1mL, the dosage of the NaOH solution is 0.1-1mL, and the dosage of the HAuCl solution is4The dosage of the solution is 1-10 mL.
5. The novel nano-gold film anti-counterfeiting method based on the surface-enhanced Raman spectroscopy technology according to claim 1, wherein in the preparation of the seed solution in the step (1), the seed solution is kept in the dark for 1-5 hours; in the preparation of the gold nanorod solution, the temperature of a water bath is 1-50 ℃, and the time for placing the water bath in a dark place is 10-20 h; the frequency of the gold nanorod solution centrifugal washing is 1-5.
6. The novel nano-gold film anti-counterfeiting method based on the surface-enhanced Raman spectroscopy technology according to claim 1, wherein the gold nanorod solution in the step (1) is diluted by a factor of 10-100; after the Raman probe solution is added, stirring for 1-10h at room temperature; the temperature of the water bath is 1-50 ℃, and the time of the water bath for dark incubation is 1-10 h; adding HAuCl4Heating the solution to 80-100 ℃; keeping the temperature for 1-60min after heating; the times of centrifugal washing of the double-layer gold nanorod solution are 1-5 times.
7. The novel nano-gold film anti-counterfeiting method based on the surface-enhanced Raman spectroscopy technology according to claim 1, wherein the concentration of the double-layer gold nanorod mixed solution encapsulating the Raman probe in the step (2) is 1-100mmol/L, the concentration of the PVP solution is 1-10%, and the concentration of DDT in the n-hexane solution is 0.1-1 mg/L.
8. The novel nano-gold film anti-counterfeiting method based on the surface-enhanced Raman spectroscopy technology according to claim 1, wherein the amount of the double-layer gold nanorod mixed solution encapsulating the Raman probe in the step (2) is 1-10mL, and H is H2The dosage of O is 1-10mL, the dosage of PVP solution is 1-10mL, the dosage of n-hexane solution is 1-30mL, and the dosage of absolute ethyl alcohol is 1-10 mL.
9. The novel nano-gold film anti-counterfeiting method based on the surface-enhanced Raman spectroscopy technology according to claim 1, wherein the absolute ethanol injection speed in the step (2) is 0.1-1 mL/min.
10. The novel nano-gold film anti-counterfeiting method based on the surface-enhanced Raman spectroscopy technology according to claim 1, wherein the standing time of the small beaker in the step (3) is 1-3 h.
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| CN115141514A (en) * | 2022-07-29 | 2022-10-04 | 天津工业大学 | Preparation method of anti-counterfeiting ink based on surface enhanced Raman spectroscopy |
| CN116223475A (en) * | 2023-01-03 | 2023-06-06 | 上海之江生物科技股份有限公司 | Raman nanoparticle lamellar treatment method and application |
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