CN110767075B - Flexible anti-counterfeiting layer based on metal micro-nano network, and preparation method and application thereof - Google Patents
Flexible anti-counterfeiting layer based on metal micro-nano network, and preparation method and application thereof Download PDFInfo
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- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
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- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
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Abstract
The invention relates to a flexible anti-counterfeiting layer based on a metal micro-nano network, and a preparation method and application thereof. The metal elements in the metal micro-nano network comprise transition metal elements. The anti-counterfeiting layer is a flexible transparent metal micro-nano network, is not easy to see by naked eyes under visible light, and has larger reflectivity in an infrared light area, so that the anti-counterfeiting layer is easy to be identified by an infrared camera; the metal nano network has good flexibility and rough surface smoothness, can maintain good identification effect under the deformation conditions of high-temperature treatment, stretching, bending, folding and the like, and can be used for technical anti-counterfeiting of products such as painting and calligraphy artworks, paper money, commodity labels and the like.
Description
Technical Field
The invention belongs to the technical field of anti-counterfeiting, and particularly relates to a flexible anti-counterfeiting layer based on a metal micro-nano network, and a preparation method and application thereof.
Background
Counterfeit and shoddy products are rolled in the global market, bring huge risks to human health and national security, and become a global economic public nuisance. Various anti-counterfeiting modes and products are produced in order to protect the own rights and interests of consumers and merchants. The anti-counterfeiting ink has the advantages of low cost, good concealment, convenient inspection, strong reproducibility and the like, and is the preferred anti-counterfeiting technology for paper money and trademarks of various countries.
However, the anti-counterfeiting functional material in the ink has poor fluorescence stability and is easy to oxidize and decompose, is difficult to disperse in an oily medium and has high synthesis difficulty, the anti-counterfeiting ink cannot meet the requirement of stretchability and high flexibility, and the development of a new anti-counterfeiting technology complementary to the prior art is urgently needed.
Therefore, there is a need in the art to develop a new anti-counterfeiting layer, which has high flexibility, can be stretched, has no need of excitation light source, and has simple preparation process and can be industrially produced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a flexible anti-counterfeiting layer based on a metal micro-nano network, and a preparation method and application thereof. The flexible anti-counterfeiting layer based on the metal micro-nano network has the advantages of smooth attachment of a rough surface, high-temperature stability, stretching, bending and folding deformation, no excitation light source requirement and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a flexible anti-counterfeiting layer based on a metal micro-nano network, wherein metal elements in the metal micro-nano network are transition metal elements.
The metal micro-nano network has the requirement of high reflectivity in an infrared region and is used for the identification of an infrared camera, and the metal micro-nano network has the requirement of high transparency (> 90%) in a visible light region and cannot be easily observed by human eyes, so that the anti-counterfeiting function is realized. The transition metal element adopted by the invention has higher reflectivity and transparency to the infrared region.
The anti-counterfeiting layer is a flexible, transparent and stretchable metal micro-nano network, is not easy to see by naked eyes under visible light, and has larger reflectivity in an infrared light area, so that the anti-counterfeiting layer is easy to be identified by an infrared camera; the metal nano network has good flexibility and rough surface smoothness, further realizes good laminating and anti-counterfeiting effects, and is wide in application; meanwhile, the anti-counterfeiting label can maintain good identification effect under deformation conditions of high-temperature treatment, stretching, bending or folding and the like, has excellent mechanical stability, and can be used for technical anti-counterfeiting of products such as painting and calligraphy artworks, paper money, commodity labels and the like.
Preferably, the metal duty cycle of the metal micro-nano network is 2% to 50%, for example, 5%, 8%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, or 45%.
The metal duty ratio is the ratio of the area of the metal strip in the metal network to the total area.
Preferably, the thickness of the metal micro-nano network is 5nm to 10 μm, preferably 5nm to 1 μm, such as 10nm, 20nm, 50nm, 80nm, 100nm, 200nm, 300nm, 500nm, 600nm, 800nm, 1 μm, 2 μm, 5 μm, 6 μm, 8 μm or 9 μm, etc.
The thickness of the metal micro-nano network selected by the invention can be completely attached to different rough surfaces in a shape following manner. The thickness is too large, the bending rigidity of the metal nano network is large, the smooth attachment with the microstructure with the rough surface cannot be realized, and the good attachment effect cannot be realized.
Preferably, the width of the metal wire in the metal micro-nano network is 10-200 nm, such as 20nm, 30nm, 50nm, 60nm, 80nm, 100nm, 120nm, 150nm, 160nm or 180 nm.
The width of the metal wire in the metal micro-nano network is as follows: the wire of the present invention is not necessarily cylindrical, so the cross-section is not necessarily circular, and the width is the distance of the farthest point of the wire cross-section.
Preferably, the size of the mesh in the metal micro-nano network is 50nm to 100 μm, preferably 50nm to 20 μm, such as 80nm, 100nm, 200nm, 300nm, 500nm, 600nm, 800nm, 1 μm, 2 μm, 5 μm, 6 μm, 8 μm, 10 μm, 12 μm, 15 μm, 16 μm, 18 μm, 19 μm, 20 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 80 μm or 90 μm, etc.
The mesh size of the selected metal micro-nano network is related to the transmittance of a visible light area and the reflectance of an infrared light area. The mesh is too small, so that the transmittance of visible light is reduced; the mesh is too large, reducing the reflectivity of infrared light. By regulating and controlling the metal duty ratio, the line width and the mesh size of the metal micro-nano network, the ultrahigh transmittance of a visible light area and the high reflectance of an infrared light area are met.
Preferably, the metal in the metal micro-nano network is a metal simple substance and/or an alloy.
Preferably, the metal simple substance is any one of gold, silver or copper.
Preferably, the alloy is any one of gold-silver alloy, gold-copper alloy, copper-silver alloy or gold-silver-copper alloy.
The metal in the selected metal micro-nano network is made into the metal micro-nano network, so that the advantages of high-temperature stability, chemical stability, mechanical stability and the like can be simultaneously met, and other metal elements cannot be simultaneously met.
Preferably, the structure of the metal micro-nano network comprises any one of a square network structure, a rectangular network structure, a diamond network structure, a hexagonal network structure, a round hole network structure, a cracking network structure, a serpentine network structure, a nanowire network structure, a polymer phase-separated random network structure or an irregular network structure.
Preferably, the transmittance of the metal micro-nano network in a visible light band of 400-760 nm is higher than 90%, for example 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99% or 99.9%. Which is not readily visible to the naked eye.
Preferably, the reflectivity of the metal micro-nano network in an infrared band of 2-5 μm and 8-14 μm is higher than 10%, for example, 12%, 15%, 18%, 20%, 25%, 28%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, or the like. The patterns formed by the metal micro-nano network are easy to be identified by an infrared camera.
Preferably, the infrared light reflected by the metal micro-nano network is from an infrared heat source in the environment, and is preferably electrical heating equipment or a human body.
The second purpose of the present invention is to provide a method for preparing a flexible anti-counterfeiting layer based on a metal micro-nano network according to the first purpose, wherein the method comprises the following steps:
(1) preparing a metal material, and patterning the metal material to obtain a metal network with a specific pattern, namely a patterned metal network;
(2) and (3) transferring the patterned metal network obtained in the step (1) to a product needing anti-counterfeiting to obtain a flexible anti-counterfeiting layer of the metal micro-nano network.
Preferably, the metal material in step (1) is prepared by a nanotechnology processing method, a chemical synthesis method, electron beam evaporation, thermal evaporation or magnetron sputtering.
Preferably, the nanotechnology processing method includes a grain boundary transfer method, a spinning template method, a nanowire spraying method, an inkjet printing method, or a laser cutting metal thin film method.
Preferably, the spinning template method comprises electrospinning or biological spinning.
Preferably, the metal material in step (1) includes any one of or a combination of at least two of a metal elementary substance nanowire with a nanometer thickness, an alloy nanowire with a nanometer thickness, a metal elementary substance network and an alloy network.
Preferably, the elemental metal network and the alloy network are respectively and independently selected from any one of an integrated network film or a composite network film formed by coating nanowires.
Preferably, the patterning method of step (1) includes any one of an adhesive tape stencil transfer method, a mask spray pattern method, an ink jet printing method, or a photolithography patterning method.
Preferably, the patterned metal network in the step (2) is an anti-counterfeiting pattern which can be identified under an infrared camera.
The invention also aims to provide an application of the flexible anti-counterfeiting layer based on the metal micro-nano network, which is used in the field of product anti-counterfeiting, preferably any one or a combination of at least two of paper money anti-counterfeiting, painting and calligraphy anti-counterfeiting, artwork anti-counterfeiting and commodity label anti-counterfeiting.
Compared with the prior art, the invention has the following beneficial effects:
(1) the selected metal micro-nano network can be highly and smoothly combined with a rough substrate (anti-counterfeiting product), can meet the anti-counterfeiting requirements of most smooth or rough substrate materials, and has wide material application range;
(2) the metal micro-nano network has good flexibility, can still keep good infrared camera identification effect under the deformation operations of stretching, bending or folding and the like, and is suitable for anti-counterfeiting of a bent substrate or a large-deformation substrate;
(3) the metal micro-nano network anti-counterfeiting layer has high temperature stability and chemical stability, and can still maintain a good infrared camera identification effect in an air environment or a high temperature environment;
(4) according to the invention, no additional excitation light source is needed for pattern recognition of the metal micro-nano network, and infrared light sources can be provided for pattern recognition by electrical equipment or heating objects such as human bodies in the environment.
Drawings
Fig. 1 is a flow chart of a preparation process of a silver nanowire network anti-counterfeiting layer provided in embodiment 1 of the present invention;
fig. 2A, fig. 2B, fig. 2C, fig. 3A, fig. 3B and fig. 3C are scanned images of the silver nanowire network anti-counterfeiting layer provided in embodiment 1 of the present invention at different spraying densities (the scale in the figures is 5 μm);
fig. 4A to 4F are diagrams of the recognition effect of the infrared camera of the silver nanowire network anti-counterfeiting layer provided in embodiment 1 of the present invention under different spraying densities;
fig. 5 is a graph comparing transmittance of the silver nanowire network anti-counterfeiting layer provided in embodiment 1 in visible light regions at different spraying densities;
fig. 6 is a graph showing the transmittance of the silver nanowire network in the visible light region and the reflectance of the silver nanowire network in the infrared light region according to example 1 of the present invention;
fig. 7A is an optical diagram of the silver nanowire network anti-counterfeiting layer provided in embodiment 1 of the present invention under bending, fig. 7B is an infrared camera identification effect diagram after bending, and fig. 7C is an infrared camera identification effect diagram (scale in the diagram is 5mm) of the silver nanowire network anti-counterfeiting layer provided in embodiment 1 of the present invention under tensile deformation;
fig. 8A to 8B are temperature test charts of the silver nanowire network anti-counterfeiting layer provided in embodiment 1 of the present invention, where fig. 8A is a normal temperature infrared camera identification chart of the anti-counterfeiting layer, and fig. 8B is an infrared camera identification chart of the anti-counterfeiting layer after heating at 200 ℃ for 2 hours (the scale in the chart is 5 mm);
fig. 9A to 9D are graphs (with a scale of 10mm) of an anti-counterfeiting effect of a silver nanowire network anti-counterfeiting layer provided in embodiment 1, where fig. 9A is a scanning electron microscope graph, fig. 9B is an optical graph and an infrared anti-counterfeiting effect graph of a silver nanowire network on a banknote, fig. 9C is an optical graph of a silver nanowire network on a smooth and transparent silica gel, and fig. 9D is a grayscale graph of the silver nanowire network realizing different infrared reflection effects by controlling a spraying density;
fig. 10A to fig. 10C, fig. 11A to fig. 11C, fig. 12A to fig. 12C, and fig. 13A to fig. 13C are anti-counterfeiting effect diagrams (10 mm in scale) of pattern coding of a rough surface by the silver nanowire network anti-counterfeiting layer provided in embodiment 1 of the present invention, where fig. 10A to fig. 10C are scanning diagrams, optical diagrams, and infrared effect diagrams of the silver nanowire network anti-counterfeiting layer on the surface of the matte paper, respectively; 11A-11C are respectively a scanned image, an optical image and an infrared effect image of the silver nanowire network anti-counterfeiting layer on the surface of 10000-mesh sandpaper; fig. 12A-12C are a scan, an optical, and an infrared effect of the silver nanowire network anti-counterfeiting layer on the surface of a 1000-mesh sandpaper replica (silica gel), respectively; FIGS. 13A-13C are a scanned, optical, and infrared effect plot, respectively, of a silver nanowire network anti-counterfeiting layer on the surface of a replica (silica gel) of a leaf of Neuma velveteen;
fig. 14A, 14B, 15A, and 15B are test charts of the gold nano-network anti-counterfeiting layer according to embodiment 2 of the present invention, in which fig. 14A is a transmittance chart, fig. 14B is an optical chart, fig. 15A is a scanned chart, and fig. 15B is an infrared identification chart.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment uses a sprayed silver nanowire network as an infrared anti-counterfeiting layer, patterns of the anti-counterfeiting layer are encrypted by adopting a mask plate during spraying, the anti-counterfeiting layer which is difficult to observe by naked eyes is obtained, decoding of the anti-counterfeiting layer is realized under shooting of an infrared camera, and a flow schematic diagram for preparing the infrared anti-counterfeiting layer is shown in figure 1 and comprises the following steps:
(1) heating the smooth or rough substrate surface to 80 ℃;
(2) placing a negative mask plate with an encrypted pattern on a spraying surface;
(3) spraying superfine silver nanowire (diameter of 20nm and length of 30 μm) water solution with an automatic spray gun;
(4) removing the negative mask plate to obtain an encryption pattern composed of the silver nanowire network, namely a silver nanowire anti-counterfeiting layer, so that the surface densities of the obtained silver nanowire networks are 0.3 mu g/cm respectively2、0.8μg/cm2、1.6μg/cm2、3.1μg/cm2、6.3μg/cm2And 9.4. mu.g/cm2；
(5) And (4) decrypting and identifying the silver nanowire anti-counterfeiting layer by using an infrared camera.
Fig. 2A, 2B, 2C, 3A, 3B, and 3C are scanning images of the anti-counterfeit layer prepared by the silver nanowire network in the embodiment at different spraying densities, and fig. 4A to 4F are recognition effect images of the infrared camera at different spraying densities, which shows that as the spraying density increases, the brightness of the recognition pattern of the infrared camera is greater;
fig. 5 is a graph comparing the transmittance of the silver nanowire network anti-counterfeiting layer in the visible light region under different spraying densities in the present embodiment, and it can be seen from the graph that, for the silver nanowire network, as the spraying density increases, the transmittance in the visible light region slightly decreases;
FIG. 6 shows that the spraying density of the silver nanowires in this example is 3.1 μ g/cm2The transmittance of the obtained anti-counterfeiting layer in a visible light region is higher than 97%, and the reflectivity in an infrared light region reaches 30%, so that the intensity of the environmental infrared rays reflected by the anti-counterfeiting layer based on the silver nanowires is enough to be received and identified by an infrared camera;
fig. 7A is an optical diagram of the silver nanowire network anti-counterfeiting layer in the embodiment under bending, fig. 7B is an infrared camera recognition effect diagram after bending, and fig. 7C is an infrared camera recognition effect diagram of the anti-counterfeiting layer under stretching deformation (the scale in the diagram is 5mm), and it can be seen from the diagrams that the anti-counterfeiting layer obtained by the invention has better mechanical stability and can still better recognize patterns under bending or stretching deformation;
fig. 8A-8B are temperature test charts of the silver nanowire network anti-counterfeiting layer in the embodiment, where fig. 8A is a normal-temperature infrared camera identification chart of the anti-counterfeiting layer, and fig. 8B is an infrared camera identification chart of the anti-counterfeiting layer after being heated at 200 ℃ for 2 hours (the scale in the chart is 5mm), and it can be seen from the charts that the obtained silver nanowire network anti-counterfeiting layer has good high-temperature stability, and can be completely identified by the infrared camera after being heated at 200 ℃ for 2 hours;
fig. 9A to 9D are graphs (with a scale of 10mm) of an anti-counterfeiting effect of a silver nanowire network anti-counterfeiting layer provided in embodiment 1, where fig. 9A is a scanning electron microscope graph, fig. 9B is an optical graph and an infrared anti-counterfeiting effect graph of a silver nanowire network on a banknote, fig. 9C is an optical graph of a silver nanowire network on a smooth and transparent silica gel, and fig. 9D is a grayscale graph of the silver nanowire network realizing different infrared reflection effects by controlling a spraying density;
fig. 10A to fig. 10C, fig. 11A to fig. 11C, fig. 12A to fig. 12C, and fig. 13A to fig. 13C are anti-counterfeiting effect diagrams (with a scale of 10mm) obtained by pattern-coding the rough surface of the silver nanowire network anti-counterfeiting layer provided in this embodiment, where fig. 10A to fig. 10C are respectively a scanned diagram, an optical diagram, and an infrared effect diagram of the silver nanowire network anti-counterfeiting layer on the surface of the matte paper; 11A-11C are respectively a scanned image, an optical image and an infrared effect image of the silver nanowire network anti-counterfeiting layer on the surface of 10000-mesh sandpaper; fig. 12A-12C are a scan, an optical, and an infrared effect of the silver nanowire network anti-counterfeiting layer on the surface of a 1000-mesh sandpaper replica (silica gel), respectively; FIGS. 13A-13C are a scanned, optical, and infrared effect plot, respectively, of a silver nanowire network anti-counterfeiting layer on the surface of a replica (silica gel) of a leaf of Neuma velveteen; as can be seen from the figure, the silver nanowire network anti-counterfeiting layer has wide application, and can perform pattern password anti-counterfeiting on smooth or rough planes or curved surfaces.
Example 2
In this embodiment, a gold nano-network obtained by a grain boundary transfer method is used as an anti-counterfeiting layer, the gold nano-network is patterned by a sugar transfer method to obtain an anti-counterfeiting layer that is difficult to observe by naked eyes, and the anti-counterfeiting layer is decoded under the shooting of an infrared camera, wherein the preparation method comprises the following steps:
(1) transferring the gold nano network obtained by the grain boundary transfer method to flexible polydimethylsiloxane;
(2) preparing a bendable plastic mask plate by using a laser cutting machine for patterning the gold nano-network;
(3) patterning and transferring the gold nano network by adopting a sucrose transfer method, placing a plastic mask plate with a required pattern (five-pointed star) on the gold nano network, and casting a molten sucrose film;
(4) when the sucrose is cooled to 25 ℃ and solidified, the sucrose becomes sufficiently viscous to peel off the gold nanoweb and transfer to the skin; finally, washing off sucrose by using deionized water to obtain an infrared anti-counterfeiting layer of the gold nano network with the required pattern;
(5) and (4) decrypting and identifying the silver nanowire anti-counterfeiting layer by using an infrared camera.
Fig. 14A, 14B, 15A, and 15B are test charts of the gold nano-network anti-counterfeiting layer according to embodiment 2 of the present invention, in which fig. 14A is a transmittance chart, fig. 14B is an optical chart, fig. 15A is a scanned chart, and fig. 15B is an infrared identification chart.
Therefore, the metal-based nano network obtained by the invention has wide application, mechanical stability and high-temperature stability, and can be used for anti-counterfeiting of different materials.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (12)
1. A flexible anti-counterfeiting layer based on a metal micro-nano network is characterized in that metal elements in the metal micro-nano network comprise transition metal elements;
the metal in the metal micro-nano network is a metal simple substance and/or an alloy;
the metal simple substance is any one of gold, silver or copper;
the alloy is any one of gold-silver alloy, gold-copper alloy, copper-silver alloy or gold-silver-copper alloy;
the metal duty ratio of the metal micro-nano network is 2% -50%;
the thickness of the metal micro-nano network is 5 nm-2 μm;
the width of a metal wire in the metal micro-nano network is 10-200 nm;
the mesh size in the metal micro-nano network is 50 nm-20 mu m;
the transmittance of the metal micro-nano network in a visible light waveband of 400-760 nm is higher than 90%, and the reflectivity in an infrared light waveband of 2-5 microns and 8-14 microns is higher than 30%;
the infrared light reflected by the metal micro-nano network is from an infrared heat source in the environment.
2. The flexible anti-counterfeiting layer based on the metal micro-nano network according to claim 1, wherein the structure of the metal micro-nano network comprises any one of a square network structure, a rectangular network structure, a diamond network structure, a hexagonal network structure, a round hole network structure, a cracking type network structure, a serpentine network structure, a nanowire network structure, a polymer phase-separated random network structure or an irregular network structure.
3. A preparation method of the flexible anti-counterfeiting layer based on the metal micro-nano network as claimed in claim 1 or 2, wherein the method comprises the following steps:
(1) preparing a metal material, and patterning the metal material to obtain a metal network with a specific pattern, namely a patterned metal network;
(2) and (3) transferring the patterned metal network obtained in the step (1) to a product needing anti-counterfeiting to obtain a flexible anti-counterfeiting layer of the metal micro-nano network.
4. The method according to claim 3, wherein the metal material of step (1) is prepared by a nanotechnology processing method, a chemical synthesis method, electron beam evaporation, thermal evaporation, or magnetron sputtering.
5. The method of claim 4, wherein the nanotechnology process comprises a grain boundary transfer method, a spinning template method, a nanowire spraying method, an ink jet printing method, or a laser cutting metal thin film method.
6. The method of claim 5, wherein the spinning template process comprises electrospinning or biological spinning.
7. The method according to claim 3, wherein the metal material in step (1) includes any one of or a combination of at least two of nano-thickness elemental metal nanowires, nano-thickness alloy nanowires, elemental metal networks, and alloy networks.
8. The method according to claim 7, wherein the elemental metal network and the alloy network are independently selected from any one of an integrated network film and a composite network film formed by coating nanowires.
9. The method of claim 3, wherein the patterning process of step (1) comprises any one of an adhesive tape stencil transfer process, a mask spray pattern process, an ink jet printing process, or a photolithographic patterning process.
10. The method of claim 3, wherein the patterned metal network of step (2) is a security pattern that can be identified with an infrared camera.
11. Use of the flexible anti-counterfeiting layer based on the metal micro-nano network according to claim 1 or 2, wherein the flexible anti-counterfeiting layer based on the metal micro-nano network is used in the field of product anti-counterfeiting.
12. The use according to claim 11, wherein the flexible anti-counterfeiting layer based on the metal micro-nano network is used for any one or a combination of at least two of paper money anti-counterfeiting, painting and calligraphy anti-counterfeiting, artwork anti-counterfeiting and commodity label anti-counterfeiting.
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