CN110625134B - Preparation method of anti-counterfeiting film based on double-layer gold nanorods - Google Patents

Preparation method of anti-counterfeiting film based on double-layer gold nanorods Download PDF

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CN110625134B
CN110625134B CN201910878389.2A CN201910878389A CN110625134B CN 110625134 B CN110625134 B CN 110625134B CN 201910878389 A CN201910878389 A CN 201910878389A CN 110625134 B CN110625134 B CN 110625134B
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李秋瑾
陈霖娜
张健飞
赵芷芪
赵玉
巩继贤
李政
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Tianjin Polytechnic University
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    • 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
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Abstract

The invention relates to a preparation method of an anti-counterfeiting film based on double-layer gold nanorods, belonging to the field of composite materials. The method comprises the steps of firstly preparing Au NRs by adopting a seed crystal growth method, preparing Au @ Au NRs on the basis, packaging different Raman probes in core-shell gaps of the Au @ Au NRs, preparing Au @ Au NRs films packaged with the different Raman probes by adopting an oil-water interface self-assembly technology, and transferring the Au @ Au NRs films to a PDMS substrate. Because different Raman probes correspond to unique SERS signals, the anti-counterfeiting safety mark is manufactured by using the Raman probes, and the product can be endowed with safety information with non-replicability and extremely high identification degree, so that counterfeit and shoddy products can be identified.

Description

Preparation method of anti-counterfeiting film based on double-layer gold nanorods
Technical Field
The invention relates to a preparation method of an anti-counterfeiting film based on double-layer gold nanorods, belonging to the field of composite materials.
Background
The Surface Enhanced Raman (SERS) technique is a fast, sensitive, non-destructive technique, and each chemical corresponds to a specific raman spectrum. Noble metal material gold nanorod has excellent SERS activity, select different Raman probe encapsulation at Au @ Au NRs nanogap, make Au @ Au NRs film have specific SERS signal, the safety marking who utilizes its SERS signal to prepare has high discernment precision and can not reproducibility, au @ Au NRs film can integrate to different bases simultaneously, have very high stability and SERS signal reproducibility, these provide the theoretical basis for the anti-fake application based on the Au @ Au NRs film of SERS technique.
Disclosure of Invention
The method adopts a seed crystal growth method to prepare Au NRs, prepares Au @ Au NRs on the basis, encapsulates different Raman probes in the core-shell gaps of the Au @ Au NRs, adopts an oil-water interface self-assembly technology to prepare Au @ Au NRs films coated with different Raman probes, and transfers the Au @ Au NRs films to the PDMS substrate. Different Raman probes correspond to different SERS signals, so that the film loaded with Au @ Au NRs can be endowed with unique SERS signals, and the signals are used as anti-counterfeiting safety information.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of an anti-counterfeiting film based on double-layer gold nanorods comprises the following steps:
(1) Preparing gold nanorods: mixing Cetyl Trimethyl Ammonium Bromide (CTAB) solution and water (H) 2 O) and chloroauric acid (HAuCl) 4 ) After the solution, freshly prepared sodium borohydride (NaBH) was added 4 ) Placing the solution in dark to complete the preparation of the seed solution; to a cetyltrimethylammonium bromide (CTAB) solution was added successively chloroauric acid (HAuCl) 4 ) Solution, silver nitrate (AgNO) 3 ) Solution, sulfuric acid (H) 2 SO 4 ) Shaking the solution evenly, and finally adding a freshly prepared ascorbic acid (L-AA) solution to complete the preparation of a growth solution; adding a certain amount of seed solution into the growth solution, placing the seed solution in a water bath in a dark place at a certain temperature, centrifuging and washing the obtained solution for multiple times to obtain a gold nanorod (Au NRs) solution, and refrigerating and storing the gold nanorod solution in a dark place.
(2) Preparing double-layer gold nanorods: diluting gold nanorod (Au NRs) solution, taking a certain amount of diluted gold nanorod (Au NRs) solution, adding different Raman probe (MBA, MMTAA, DTNB) solutions under the stirring condition, stirring at room temperature for a certain time, centrifuging and concentrating, adding Cetyl Trimethyl Ammonium Bromide (CTAB) solution, shaking uniformly, adding polyvinylpyrrolidone (PVP) solution under ultrasonic treatment, and sequentially adding silver nitrate (AgNO) 3 ) Incubating in water bath at certain temperature in dark place with ascorbic acid (L-AA) solution and sodium hydroxide (NaOH) solution, and adding chloroauric acid (HAuCl) 4 ) And heating the solution for a period of time, and performing centrifugal water washing for multiple times to complete the preparation of the double-layer gold nanorods (Au @ Au NRs) containing different Raman probes.
(3) Prevention based on double-layer gold nanorodsPreparation of a pseudo film: mixing and packaging double-layer gold nanorod (Au @ Au NRs) solution and water (H) with Raman probe 2 O) and polyvinylpyrrolidone (PVP) solution as the aqueous phase and a solution of dodecyl mercaptan (DDT) in n-hexane as the oil phase. Respectively transferring the water phase and the oil phase into a small beaker to cause the phenomenon of oil-water separation, slowly injecting absolute ethyl alcohol into an oil-water interface by using an injector, standing for a period of time to form a layer of compact double-layer gold nanorod (Au @ Au NRs) film on the oil-water interface, removing the upper oil phase and waiting for the natural evaporation of the residual oil phase, and transferring the double-layer gold nanorod (Au @ Au NRs) film by using a PDMS substrate and adopting a bottom-up dipping method.
The concentration of CTAB solution in the step (1) is 0.1-1mol/L, HAuCl 4 The concentration of the solution is 1-100mmol/L, naBH 4 The concentration of the solution is 1-100mmol/L, agNO 3 The concentration of the solution is 1-100mmol/L, H 2 SO 4 The concentration of the solution is 0.1-1mol/L, and the concentration of the L-AA solution is 0.1-1mol/L.
In the preparation of the seed solution in the above step (1), the CTAB solution is used in an amount of 1-10mL 4 The dosage of the solution is 0.1-1mL 4 The dosage of the solution is 0.1-1mL; in the preparation of the growth solution, the CTAB solution is used in an amount of 50-150mL 4 The dosage of the solution is 1-5mL 3 The dosage of the solution is 0.1-5mL 2 SO 4 The dosage of the solution is 0.1-5mL, and the dosage of the L-AA solution is 0.1-1mL; in the preparation of the gold nanorod solution, the dosage of the seed solution added into the growth solution is 0.1-1mL.
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 10-20h; the times of the gold nanorod solution centrifugal washing are 1-5.
The concentration of the Raman probe solution in the step (2) is 1-10mmol/L, the concentration of the CTAB solution is 0.1-1mol/L, the concentration of the PVP solution is 1-10%, and AgNO is 3 The concentration of the solution is 1-10mmol/L, the concentration of the L-AA solution is 0.1-1mol/L, the concentration of the NaOH solution is 0.1-1mol/L, and HAuCl 4 The concentration of the solution is 1-10mmol/L.
The dosage of the diluted gold nanorod solution in the step (2) is 1-10mL, the dosage of the Raman probe solution is 0.1-5mL, the dosage of the CTAB solution is 0.1-5mL, the dosage of the PVP solution is 1-10mL, and the dosage of the AgNO solution is 1-10mL 3 The 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, the dosage of the HAuCl solution is less than or equal to the total dosage of the sodium hydroxide and the sodium hydroxide, and the dosage of the sodium hydroxide and the sodium hydroxide is less than or equal to the total dosage of the sodium hydroxide and the sodium hydroxide 4 The dosage of the solution is 1-10mL.
The gold nanorod solution in the step (2) 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 dark incubation of the water bath is 1-10h; adding HAuCl 4 Heating 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.
The concentration of the double-layer gold nanorod mixed solution packaged with the Raman probe in the step (3) is 1-100mmol/L, the concentration of the PVP solution is 1-10%, and the concentration of DDT in the n-hexane solution is 0.1-1mg/L.
The method for preparing an anti-counterfeiting film based on the double-layer gold nanorods according to claim 1, wherein the amount of the double-layer gold nanorod mixed solution encapsulating the Raman probe in the step (3) is 1-10mL 2 The 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 1-10mL.
The absolute ethyl alcohol injection speed in the step (3) is 0.1-1mL/min; standing for 1-3h.
The invention has the advantages that:
the Au @ Au NRs containing different Raman probes has excellent SERS activity and unique SERS signals, and has great advantages in the aspect of anti-counterfeiting. The anti-counterfeiting safety mark manufactured by the anti-counterfeiting label can endow the product with extremely high identification degree and uncopyable safety information, thereby realizing the identification between genuine products and counterfeit products.
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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.
FIG. 2: is a graph showing the results of example 2 of the present invention.
FIG. 3: is a graph of the results of example 3 of the present invention.
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: the Au @ Au NRs film packaged with different Raman probes is prepared by adopting an oil-water interface self-assembly technology and is transferred to a PDMS substrate. As shown in FIG. 1, the Au @ Au NRs film exhibits a metallic specular gloss, and exhibits different colors and gloss levels depending on the angle.
Example 2: the Au @ Au NRs film was dried, adhered to a sample stage with a conductive adhesive, and observed using a Phenom bench-type scanning electron microscope. As shown in FIG. 2, the Au @ Au NRs film is attached to the surface of the PDMS substrate, and the Au @ Au NRs is uniformly distributed on the PDMS substrate.
Example 3: the Au @ Au NRs nano-film packaged with the DTNB Raman probe is subjected to Raman test, the obtained SERS spectrogram is shown in figure 3, and the nano-film has a unique SERS spectrum based on the type of the used Raman probe. The unique SERS spectrogram can be used as security information for subsequent anti-counterfeiting application.

Claims (1)

1. A preparation method of an anti-counterfeiting film based on double-layer gold nanorods comprises the following steps:
(1) Preparing gold nanorods: mixing 1-10mL of cetyltrimethylammonium bromide (CTAB) solution with water (H) 2 O) and 0.1-1mL of chloroauric acid (HAuCl) 4 ) After the solution, 0.1-1mL of freshly prepared sodium borohydride (NaBH) was added 4 ) Placing the solution in dark for 1-5h to complete the preparation of the seed solution; to 50-150mL of cetyltrimethylammonium bromide (CTAB) solution was added 1-5mL of chloroauric acid (HAuCl) 4 ) Solution, 0.1-5mL silver nitrate (AgNO) 3 ) Solution, 0.1-5mL sulfuric acid (H) 2 SO 4 ) Shaking the solution, and finally adding 0.1-1mL of freshly prepared ascorbic acid (L-AA) solution to complete the preparation of the growth solution; adding 0.1-1mL of seed solution into the growth solution, placing in a water bath at 1-50 ℃ in a dark place for 10-20h, centrifuging and washing the obtained solution for 1-5 times to obtain a gold nanorod (Au NRs) solution, and refrigerating in a dark place for storage;
(2) Preparing double-layer gold nanorods: diluting gold nanorod (Au NRs) solution by 10-100 times, taking 1-10mL of diluted gold nanorod (Au NRs) solution, adding 0.1-5mL of different Raman probe 5,5' -dithiobis (2-nitrobenzoic acid), 2-mercaptobenzoic acid and 2-mercapto-4-methyl-5-thiazoleacetic acid solution under the condition of stirring, stirring at room temperature for 1-10h, centrifugally concentrating, adding 0.1-5mL of hexadecyltrimethylammonium bromide (CTAB) solution, shaking uniformly, adding 1-10mL of polyvinylpyrrolidone (PVP) solution under ultrasonic treatment, and sequentially adding 0.1-5mL of silver nitrate (AgNO) 3 ) The solution, 0.1-1mL ascorbic acid (L-AA) solution and 0.1-1mL sodium hydroxide (NaOH) solution are incubated in water bath at 1-50 deg.C for 1-10h in the dark, and 1-10mL chloroauric acid (HAuCl) is added 4 ) Heating the solution to 80-100 deg.C, maintaining for 1-60min, centrifuging for 1-5 times, and washing to obtain double-layer gold nanorods (Au @ Au NRs) containing different Raman probes;
(3) Preparing an anti-counterfeiting film based on double layers of gold nanorods: mixing 1-10mL of double-layer gold nanorod (Au @ Au NRs) solution packaged with Raman probe and 1-10mL of water (H) 2 O) and 1-10mL of polyvinylpyrrolidone (PVP) solution are used as water phases, and 1-30mL of n-hexane solution containing dodecyl mercaptan (DDT) is used as an oil phase; transferring water phase and oil phase into small beaker respectively to separate oil and water, injecting 1-10mL absolute ethanol into oil-water interface at 0.1-1mL/min with injector, standing for 1-3 hr to form a layer of compact double-layer gold nanorod (Au @ Au NRs) film on the oil-water interface, transferringWalking an upper oil phase, waiting for the natural evaporation of the residual oil phase, and transferring a double-layer gold nanorod (Au @ Au NRs) film by using a PDMS substrate and adopting a bottom-up dipping method;
in the step (1), the concentration of the hexadecyl trimethyl ammonium bromide solution is 0.1-1mol/L, the concentration of the chloroauric acid solution is 1-100mmol/L, the concentration of the sodium borohydride solution is 1-100mmol/L, the concentration of the silver nitrate solution is 1-100mmol/L, the concentration of the sulfuric acid solution is 0.1-1mol/L, and the concentration of the ascorbic acid solution is 0.1-1mol/L;
in the step (2), the concentration of the Raman probe 5,5' -dithiobis (2-nitrobenzoic acid), 2-mercaptobenzoic acid and 2-mercapto-4-methyl-5-thiazoleacetic acid solution is 1-10mmol/L, the concentration of hexadecyl trimethyl ammonium bromide solution is 0.1-1mol/L, the concentration of polyvinylpyrrolidone solution is 1-10%, the concentration of silver nitrate solution is 1-10mmol/L, the concentration of ascorbic acid solution is 0.1-1mol/L, the concentration of sodium hydroxide solution is 0.1-1mol/L, and the concentration of chloroauric acid solution is 1-10mmol/L;
the concentration of the double-layer gold nanorod mixed solution packaged with the Raman probe in the step (3) is 1-100mmol/L, the concentration of the polyvinylpyrrolidone solution is 1-10%, and the concentration of dodecyl mercaptan in the n-hexane solution is 0.1-1mg/L.
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