CN113278327A - Double-encryption anti-counterfeiting perovskite ink and preparation method thereof - Google Patents
Double-encryption anti-counterfeiting perovskite ink and preparation method thereof Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C09D11/30—Inkjet printing inks
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- C09D11/30—Inkjet printing inks
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Abstract
The invention provides double-encryption anti-counterfeiting water-based perovskite quantum dot ink and a preparation method thereof, and belongs to the technical field of anti-counterfeiting. The aqueous perovskite quantum dot ink provided by the invention uses a green solvent, is simple to prepare, consists of the encryption liquid and the decryption liquid, the encryption liquid can form any anti-counterfeiting mark by printing or writing with a pen, and the mark is invisible under ambient light or ultraviolet light. After the perovskite quantum dots are subjected to synthesis reaction by spraying of the decryption liquid, the anti-counterfeiting mark is displayed under ambient light, and the anti-counterfeiting mark emits bright fluorescence under the irradiation of ultraviolet light. The encryption and decryption process not only improves the anti-counterfeiting effect, but also implements the protection function on the anti-counterfeiting information, and realizes the safe storage and double anti-counterfeiting of the information.
Description
Technical Field
The invention relates to the technical field of anti-counterfeiting ink, in particular to perovskite anti-counterfeiting ink and a preparation method thereof.
Background
Lead-calcium-titanium halide nano-gradeCrystal CsPbX3(X = Cl, Br, I) has unique physicochemical properties: adjustable emission wavelength (400-700 nm), narrow full width at half maximum, high color purity and high fluorescence quantum yield (-90%). These excellent properties make them potentially useful for lighting, displays, security, sensors and other optoelectronic devices. Therefore, in recent years, there are more reports on such inorganic lead-halogen perovskite materials, and the perovskite nanocrystals applied in the anti-counterfeiting field in the current reports have many problems in green production and anti-counterfeiting performance, and are complex to synthesize.
For example, the Chinese patent publication No. CN112126280A discloses a perovskite quantum dot invisible ink-jet printing ink, and when the invisible ink-jet printing ink prepared by polymethyl methacrylate/perovskite resin powder is used as an anti-counterfeiting mark, the invisible ink-jet printing ink has better dispersibility, adhesiveness and stability compared with the traditional anti-counterfeiting ink, so that the fluorescent stability is good, the color development range is wide, and the perovskite quantum dot invisible ink-jet printing ink is not easy to decay. However, the anti-counterfeiting ink needs to be pre-synthesized into luminescent perovskite quantum dots, the synthesis method is complex, and a large amount of toxic and flammable organic solvents are used. The Chinese patent publication No. CN108624150A discloses a fluorescent anti-counterfeiting code-spraying ink, which is orange yellow in appearance under the synergistic effect of components with specific contents, and is orange yellow fluorescent under the irradiation of an ultraviolet lamp. However, the ink can expose the anti-counterfeiting mark under ultraviolet light, and the anti-counterfeiting performance is poor. The document [ ACS Applied Materials And Interfaces, 2021, 13(17): 20622-. However, the formed anti-counterfeiting label is exposed under ultraviolet light, is easy to copy and has poor anti-counterfeiting effect.
Disclosure of Invention
The invention aims to solve the problems that the existing luminescent anti-counterfeiting technology is complex in synthesis, contains expensive, toxic and flammable organic solvents and is easy to imitate, so that a good anti-counterfeiting effect cannot be achieved, and provides the perovskite ink which is simple in synthesis method and uses the green environment-friendly solvent, the ink can enable the anti-counterfeiting mark not to be visible under ambient light or ultraviolet light before decryption, so that the invisible effect is achieved, and the perovskite nanocrystalline synthesis is carried out by spraying decryption liquid, so that the invisible anti-counterfeiting mark has strong fluorescence performance, and the invisible anti-counterfeiting mark can be displayed.
In order to achieve the purpose, the invention provides a double-encryption anti-counterfeiting perovskite ink which is composed of an encryption liquid composed of alkali metal halide, lead halide, water, a polar organic solvent and a film-forming agent and a decryption liquid composed of cesium halide, the polar organic solvent and water, and the preparation method of the perovskite ink comprises the following steps:
the method comprises the following steps: adding alkali metal halide and lead halide into water for dissolving, and then adding a polar organic solvent and a film-forming agent to obtain an encrypted liquid;
step two: and adding cesium halide into a solvent consisting of water and an organic solvent to obtain a decryption liquid.
The mass percentages of the alkali metal halide, the lead halide, the polar organic solvent, the film forming agent and the water in the encryption liquid in the step one are respectively 10-50%, 2-30%, 0-40%, 0-30% and 40-90%.
Step one, the alkali metal halide comprises one or more of NaCl, NaBr, NaI, KCl, KBr and KI; the lead halide comprises PbCl2、PbBr2And PbI2One or more of them. Too high a content of alkali halide to dissolve will form a solid-liquid two phase, and too low a content will form a white suspension with lead halide. Alkali metal halide and lead halide are easily dissolved in an aqueous solvent to form a clear and transparent solution after a certain proportion, and the formed anti-counterfeiting mark can realize the invisible function under ambient light and ultraviolet light. After the anti-counterfeiting mark formed by the encryption liquid ink is dried, the alkali metal halide and the lead halide in the anti-counterfeiting mark are crystallized and precipitated together and are coated with each other. The lead halide provides a source of lead and a source of halogen required to form the perovskite; the alkali metal halide provides a halogen source, acts as a lead halide crystallization site and protects the perovskite nanocrystals synthesized during the spraying of the decrypting liquid from the destruction of oxygen and moisture in the environment, thereby providing excellent fluorescent properties.
The polar organic solvent is one or more of monohydric alcohol, diol, triol with less than 18 carbon atoms, and monomethyl ether and monoethyl ether of the diol and triol, and the polar organic solvent can improve the stability of the whole ink of the encrypted liquid and the wetting capacity of a substrate in the encrypted solution, and ensure that the ink does not block a nozzle in the ink-jet printing process and has the capacity of multiple applications. However, their percentage content must be within the above range, and exceeding 40% causes difficulty in rapid drying of the ink.
The film forming agent comprises one or more of polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, waterborne polyurethane, waterborne polyacrylate and polyvinyl butyral. The film forming agent can adjust the viscosity of the encryption liquid ink, so that the encryption liquid ink has good film forming property in the drying and crystallization process, the ink diffusion is prevented, the anti-counterfeiting mark with higher calibration rate is formed, but the content is in a proper range, the low content is beneficial to printing, the high content ink has high viscosity and cannot adapt to ink-jet printing but can be used for printing, but the viscosity is too high when the content exceeds 30 percent, and the perovskite precursor is excessively coated, so that the perovskite nanocrystal cannot be synthesized in the decryption process.
And the mass percentages of the cesium halide, the water and the polar organic solvent in the decryption liquid in the step two are respectively 2-20%, 50-80% and 0-40%.
The cesium halide includes one or more of CsCl, CsBr, and CsI. Cesium halide provides a cesium source and a halogen source required for forming perovskite, when the cesium halide is sprayed with a decryption liquid, the cesium halide reacts immediately to generate perovskite nanocrystalline once contacting a lead source in the anti-counterfeiting label, the anti-counterfeiting label is changed from a hidden state to a visible state, a yellow visible anti-counterfeiting label is formed under ambient light, the anti-counterfeiting label has excellent fluorescence performance under ultraviolet light, the fluorescence intensity is high, the peak value of an emission peak is 518nm, and the corresponding half-peak width is 23 nm.
The polar organic solvent in the decryption liquid is one or more of monohydric alcohol with less than 18 carbon atoms, diol, triol and monomethyl ether and monoethyl ether of diol and triol. The decryption liquid solvent consists of water and a polar organic solvent and is used for completely dissolving cesium halide to form a clear solution, the surface tension can be reduced by adding the polar organic solvent, the generated crystals in the anti-counterfeiting mark are difficult to dissolve, the morphological characteristics of the decryption liquid ink can be guaranteed not to be damaged while the decryption liquid ink can be in contact reaction with the invisible anti-counterfeiting mark fully in the process of spraying decryption, and safe storage and double anti-counterfeiting of information are realized.
The encryption and decryption method comprises the following steps: printing the encrypted liquid synthesized in the first step, and drying at room temperature to form an invisible anti-counterfeiting mark which is invisible under ambient light or ultraviolet light; when decryption is needed, the anti-counterfeiting mark is sprayed with decryption liquid, and due to the rapid synthesis of the perovskite nanocrystalline, the anti-counterfeiting mark gradually appears under ambient light in the decryption process, so that a yellow anti-counterfeiting mark is presented, the anti-counterfeiting mark does not have fluorescence under the ambient light, bright green fluorescence can be emitted under ultraviolet light, the multiple encryption anti-counterfeiting function is realized, and the anti-counterfeiting performance is excellent.
The invention has the following advantages: (1) the green solvent is used to simply synthesize the ink solution. The ink solvent is an aqueous green environment-friendly solvent, so that the required perovskite precursor can be completely dissolved, and the synthesis process only needs stirring and ultrasonic dispersion. The environment-friendly and simple synthesis method makes the method very suitable for mass production; (2) the perovskite nanocrystalline is rapidly synthesized by utilizing solid-liquid two-phase contact. The perovskite nanocrystalline can be immediately generated only by contacting the invisible anti-counterfeiting mark formed by the decryption liquid and the encryption liquid, the invisible anti-counterfeiting mark is converted into a yellow anti-counterfeiting mark with excellent fluorescence property, the fluorescence signal is strong, the identification is convenient, and no fluorescence exists under the condition of no specific exciting light; (3) the anti-counterfeiting encryption liquid is divided into encryption liquid and decryption liquid, so that the double anti-counterfeiting encryption function is realized. The invisible anti-counterfeiting mark formed by the encryption liquid has no fluorescence and is invisible under ambient light or ultraviolet light. After the decryption liquid is sprayed and the synthesis reaction of the perovskite nanocrystalline is completed, the anti-counterfeiting mark is changed, the mark is yellow under ambient light, and has no fluorescence and excellent fluorescence performance under ultraviolet light.
Drawings
FIG. 1: the ultraviolet absorption and fluorescence spectra of the security mark formed in example 1;
FIG. 2 is a drawing: a TEM image of the security mark formed in example 1;
FIG. 3: XRD pattern of the security mark formed in example 1.
Detailed Description
Example 1
Adding 7.5g of potassium bromide and 0.55g of lead bromide into a mixed encryption liquid ink solvent consisting of 12ml of water, 2ml of ethylene glycol and 1ml of ethanol, fully dissolving, then adding 0.1g of polyvinylpyrrolidone, and forming a clear and transparent encryption liquid after complete dissolution; 0.32g of cesium bromide was added to a mixed decryption liquid ink solvent consisting of 13ml of ethanol and 2ml of water, and the mixture was sufficiently dissolved by stirring to form a clear and transparent decryption liquid.
The encryption and decryption method comprises the following steps: printing the encrypted liquid synthesized in the first step, and drying at room temperature to form an invisible anti-counterfeiting mark which is invisible under ambient light or ultraviolet light; when decryption is needed, the anti-counterfeiting mark is sprayed with decryption liquid, and due to the rapid synthesis of the perovskite nanocrystalline, the anti-counterfeiting mark gradually appears under ambient light to present a yellow anti-counterfeiting mark which does not have fluorescence under the ambient light and can emit bright green fluorescence under ultraviolet light.
Example 2
Adding 5.5g of potassium bromide and 0.275g of lead bromide into a mixed encryption liquid ink solvent consisting of 12ml of water, 2ml of ethylene glycol and 1ml of ethanol, fully dissolving, then adding 0.1g of polyvinylpyrrolidone, and forming a clear and transparent encryption liquid after complete dissolution; 0.32g of cesium bromide was added to a mixed decryption liquid ink solvent consisting of 13ml of ethanol and 2ml of water, and the mixture was sufficiently dissolved by stirring to form a clear and transparent decryption liquid.
The encryption and decryption method comprises the following steps: printing the encrypted liquid synthesized in the first step, and drying at room temperature to form an invisible anti-counterfeiting mark which is invisible under ambient light or ultraviolet light; when decryption is needed, the anti-counterfeiting mark is sprayed with decryption liquid, and due to the rapid synthesis of the perovskite nanocrystalline, the anti-counterfeiting mark gradually appears under ambient light to present a yellow anti-counterfeiting mark which does not have fluorescence under the ambient light and can emit bright green fluorescence under ultraviolet light.
Example 3
Adding 6.5g of sodium bromide and 0.55g of lead bromide into a mixed encryption liquid ink solvent consisting of 12ml of water, 2ml of 1, 2-propylene glycol and 1ml of ethanol, fully dissolving, then adding 0.1g of polyvinyl alcohol, stirring at a constant temperature of 95 ℃, and forming a clear and transparent encryption liquid after complete dissolution; 0.32g of cesium bromide was added to a mixed decryption liquid ink solvent consisting of 13ml of ethanol and 2ml of water, and the mixture was sufficiently dissolved by stirring to form a clear and transparent decryption liquid.
The encryption and decryption method comprises the following steps: printing the encrypted liquid synthesized in the first step, and drying at room temperature to form an invisible anti-counterfeiting mark which is invisible under ambient light or ultraviolet light; when decryption is needed, the anti-counterfeiting mark is sprayed with decryption liquid, and due to the rapid synthesis of the perovskite nanocrystalline, the anti-counterfeiting mark gradually appears under ambient light to present a yellow anti-counterfeiting mark which does not have fluorescence under the ambient light and can emit bright green fluorescence under ultraviolet light.
Example 4
Adding 4g of potassium bromide and 0.416g of lead chloride into a mixed encryption liquid ink solvent consisting of 12ml of water and 1ml of glycerol, fully dissolving, then adding 1ml of waterborne polyurethane, and forming a clear and transparent encryption liquid after complete dissolution; 0.252g of cesium chloride was added to a mixed decryption liquid ink solvent consisting of 13ml of ethanol and 2ml of water, and sufficiently dissolved by stirring to form a clear and transparent decryption liquid.
The encryption and decryption method comprises the following steps: printing the encrypted liquid synthesized in the first step, and drying at room temperature to form an invisible anti-counterfeiting mark which is invisible under ambient light or ultraviolet light; when decryption is needed, the anti-counterfeiting mark is sprayed with decryption liquid, and due to the rapid synthesis of the perovskite nanocrystalline, the anti-counterfeiting mark gradually appears under ambient light to present a white anti-counterfeiting mark which does not have fluorescence under the ambient light and can emit blue fluorescence under ultraviolet light.
Example 5
Adding 5.5g of potassium bromide and 0.345g of lead iodide into a mixed encryption liquid ink solvent consisting of 12ml of water and 3ml of isopropanol, fully dissolving, then adding 0.1g of polyvinyl butyral, and forming a clear and transparent encryption liquid after complete dissolution; 0.39g of cesium bromide was added to a mixed decryption liquid ink solvent consisting of 13ml of ethanol and 2ml of water, and the mixture was sufficiently dissolved by stirring to form a clear and transparent decryption liquid.
The encryption and decryption method comprises the following steps: printing the encrypted liquid synthesized in the first step, and drying at room temperature to form an invisible anti-counterfeiting mark which is invisible under ambient light or ultraviolet light; when decryption is needed, the anti-counterfeiting mark is sprayed with decryption liquid, and due to the rapid synthesis of the perovskite nanocrystalline, the anti-counterfeiting mark gradually appears under ambient light, presents an orange anti-counterfeiting mark, does not have fluorescence under the ambient light, and can emit red fluorescence under ultraviolet light.
Claims (8)
1. The double-encryption anti-counterfeiting perovskite ink is characterized in that the perovskite ink consists of an encryption liquid composed of alkali metal halide, lead halide, water, a polar organic solvent and a film-forming agent and a decryption liquid composed of cesium halide, the polar organic solvent and water, and the preparation method comprises the following steps:
the method comprises the following steps: adding alkali metal halide and lead halide into water for dissolving, and then adding a polar organic solvent and a film-forming agent to obtain an encrypted liquid;
step two: adding cesium halide into a solvent consisting of water and a polar organic solvent to obtain a decryption liquid.
2. The perovskite ink and the preparation method thereof as claimed in claim 1, wherein the weight percentage of the alkali metal halide, the lead halide, the polar organic solvent, the film forming agent and the water in the encryption liquid is respectively 10% -50%, 2% -30%, 0.1% -40%, 0.1% -30% and 40% -90%.
3. The perovskite ink and the preparation method thereof as claimed in claim 1, wherein the mass percentages of the cesium halide, the water and the polar organic solvent in the decryption liquid are respectively 2% -20%, 50% -80% and 0% -40%.
4. The perovskite ink and the preparation method thereof as claimed in claims 1 and 2, wherein the alkali metal halide is one or more of NaCl, NaBr, NaI, KCl, KBr and KI.
5. The perovskite ink and the production method thereof as claimed in claims 1 and 2, whereinIn that the lead halide is PbCl2、PbBr2And PbI2One or more of them.
6. The perovskite ink and the preparation method thereof as claimed in claims 1,2 and 3, wherein the polar organic solvent is one or more of monohydric alcohol with less than 18 carbon atoms, diol, triol and monomethyl ether and monoethyl ether of diol and triol.
7. The perovskite ink and the preparation method thereof as claimed in claims 1 and 2, wherein the film forming agent is one or more of polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, aqueous polyurethane, aqueous polyacrylate and polyvinyl butyral.
8. The perovskite ink and the preparation method thereof as claimed in claims 1 and 3, wherein the cesium halide is one or more of CsCl, CsBr and CsI.
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| CN114907723A (en) * | 2022-04-18 | 2022-08-16 | 太原科技大学 | Fluorescent encryption anti-counterfeiting ink based on halide perovskite quantum dots and preparation method thereof |
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