CN113956869B - Manufacturing method of dielectric microsphere patterned array up-conversion luminescence flexible film applied to anti-counterfeiting mark - Google Patents
Manufacturing method of dielectric microsphere patterned array up-conversion luminescence flexible film applied to anti-counterfeiting mark Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 62
- 239000004005 microsphere Substances 0.000 title claims abstract description 55
- 238000004020 luminiscence type Methods 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 68
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 68
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 42
- 239000000203 mixture Substances 0.000 claims description 31
- 239000002105 nanoparticle Substances 0.000 claims description 25
- 238000000059 patterning Methods 0.000 claims description 21
- 238000004528 spin coating Methods 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 18
- 239000000654 additive Substances 0.000 claims description 15
- 230000000996 additive effect Effects 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000002390 adhesive tape Substances 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- 230000005284 excitation Effects 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- 239000011258 core-shell material Substances 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 7
- 238000005411 Van der Waals force Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002356 single layer Substances 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 3
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 2
- 230000001419 dependent effect Effects 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 9
- 230000003287 optical effect Effects 0.000 abstract description 8
- 230000007547 defect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 4
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- G—PHYSICS
- 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
- G09F3/02—Forms or constructions
- G09F3/0291—Labels or tickets undergoing a change under particular conditions, e.g. heat, radiation, passage of time
-
- G—PHYSICS
- 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
- G09F3/02—Forms or constructions
- G09F3/0291—Labels or tickets undergoing a change under particular conditions, e.g. heat, radiation, passage of time
- G09F3/0294—Labels or tickets undergoing a change under particular conditions, e.g. heat, radiation, passage of time where the change is not permanent, e.g. labels only readable under a special light, temperature indicating labels and the like
Abstract
The invention discloses a manufacturing method of a dielectric microsphere patterned array up-conversion luminescence flexible film applied to an anti-counterfeiting mark. The existing preparation method of the anti-counterfeiting mark has the defects of complex preparation flow, high cost, insufficient protection of the authenticity of the commodity and the like. The dielectric microsphere patterned array up-conversion luminescence flexible film in the manufacturing method has outstanding flexibility and optical performance, and provides an alternative scheme for the application of the wearable near-infrared anti-counterfeiting mark.
Description
Technical Field
The invention relates to the technical field of optical anti-counterfeiting, and provides a preparation method of a dielectric microsphere patterning array up-conversion luminescence flexible film applied to anti-counterfeiting marks.
Background
With the development of commodity economy, the appearance of counterfeit and inferior products has serious adverse effects on various aspects of the market. Development of advanced anti-counterfeiting strategies and anti-counterfeiting security technologies to resist counterfeit goods is important to avoid a series of problems caused by counterfeit products. The anti-counterfeiting mark is used as a unique identification mode, is convenient to identify and is difficult to copy, and the anti-counterfeiting mark is widely focused by society. However, the existing preparation method of the anti-counterfeiting mark has the defects of complex preparation flow, high cost, insufficient protection of the authenticity of the commodity and the like. Here, development of low-cost and high-yield anti-counterfeit marks has become an urgent practical requirement for various commodities.
In order to solve the existing problems, optical anti-counterfeiting marks based on optical materials such as semiconductor quantum dots, organic dyes and the like commonly used in traditional anti-counterfeiting ink are generated. Although these optical materials have good fluorescence properties, further applications in the field of security against counterfeiting are limited by their strong photobleaching, high toxicity, and ease of replication. The up-conversion nano-particle (UCNP) material is used as an emerging luminescent material, has the characteristics of high optical stability, long fluorescence life, low toxicity and the like, and a near infrared source for exciting up-conversion luminescence is difficult to obtain, so that the up-conversion anti-counterfeiting mark is difficult to copy, and becomes a research hot spot in the current safety anti-counterfeiting technical field. Currently, QR codes based on RGB up-conversion ink and multicolor anti-counterfeiting patterns encrypted by core-shell structure up-conversion fluorescent materials are prepared by using printing or photoetching modes, however, the existing up-conversion anti-counterfeiting technology has a plurality of limitations, the complex thermal decomposition preparation process of core-shell up-conversion nano particles requires higher reaction temperature and longer reaction period, and the photoetching technology and the ink-jet printing technology have the defect of high cost, thereby further impeding the wide application of the technology. Although the up-conversion luminescent material has wide application potential, the luminous efficiency is generally low, and the efficient luminescence is generally realized by increasing the excitation power, so that it is important to find a structure for effectively improving the up-conversion luminous efficiency under low power.
The dielectric microsphere array structure has the advantages of convenient preparation, simple structure, good stability, low price and the like, plays an important role in regulating and controlling a sightseeing field, becomes an effective way for realizing up-conversion luminescence regulation and control, realizes the application of anti-counterfeiting marks under low power by combining with high-concentration up-conversion ink, has extremely important scientific research significance and potential application value, and has not been reported in the preparation method of the up-conversion luminescence flexible film for patterning dielectric microspheres.
Disclosure of Invention
The invention aims to provide a preparation method of a dielectric microsphere patterned array up-conversion luminescence flexible film applied to an anti-counterfeiting mark by utilizing the effect of light field regulation of dielectric microspheres.
Another object of the present invention is to provide an upconversion luminescent security device that relies on excitation power.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a manufacturing method of a dielectric microsphere patterned array up-conversion luminescence flexible film applied to anti-counterfeiting marks comprises the following steps:
step 1: naYF is prepared 4 :Yb 3+ /Tm 3+ @NaYF 4 :Yb 3+ /Nd 3+ Core-shell typeUpconverting nanoparticles (UCNPs) are suspended in the dispersion;
step 2: polymethyl methacrylate (PMMA) powder is dissolved in toluene to obtain PMMA solution;
step 3: mixing the UCNP suspension and the PMMA solution, and then placing the mixture solution in a vacuum chamber to remove bubbles;
step 4: spin-coating the UCNP/PMMA mixture solution on a glass substrate, and standing and solidifying in air to obtain a UCNP/PMMA mixture film;
step 5: drawing a required anti-counterfeiting pattern on the UCNP/PMMA film by using the UCNP solution as ink;
step 6: and (3) attaching a patterning mold to the surface of the UCNP/PMMA film, spraying the dried transparent dielectric microspheres on the patterning position of the mold, mechanically pressurizing by using a 3M low-viscosity adhesive tape, adhering the microspheres on the surface of the film by electrostatic contact and Van der Waals force, repeatedly pressing for a plurality of times, and removing the microspheres which are not adhered on the surface of the film after stripping the 3M adhesive tape. Pressing and stripping for multiple times to obtain a single-layer patterned dielectric microsphere array;
step 7: the application of the dielectric microsphere patterning array up-conversion luminescence flexible film which depends on the excitation power is realized by irradiating the patterned UCNP/PMMA film with laser.
In the above technical scheme, in step 1, the average size of the up-conversion nanoparticles is 30-40nm, the dispersion solvent is cyclohexane, and the concentration of the up-conversion nanoparticles is 5mg/mL.
In the technical scheme, in the step 2, the PMMA solution consists of powder, solvent and additive, wherein the grain size of the PMMA powder is 70-100 mu m, and the PMMA powder is dissolved in toluene in a mass ratio of 0.3-1 wt%; the additive in the PMMA solution is acetone, and the mass of the additive is 0.05-0.6% of the mass of the solvent.
In the above technical scheme, in step 3, the UCNP suspension and the PMMA solution are mixed by repeated pumping, so that they are fully mixed to obtain a uniform mixture solution.
In the technical scheme, in the step 4, the UCNP concentration in the mixture solution is 0.02-0.1mg/mL, the spin coating speed is set to 1500-3000r/min, and the spin time is set to 15-30s.
In the above technical scheme, in step 5, the UCNP solution concentration for drawing the anti-counterfeiting pattern is 5mg/mL as the ink.
In the above technical scheme, in step 7, the excitation light source is a 980nm laser with adjustable power, and the infrared dual-mode anti-counterfeiting function is realized by adjusting the power.
Compared with the prior art, the invention has the following advantages:
(1) The manufacturing method of the dielectric microsphere patterned array up-conversion luminescence flexible film applied to the anti-counterfeiting mark is simple, low in cost, free of limitation of substrate materials, high in stability and convenient to recycle;
(2) According to the manufacturing method of the dielectric microsphere patterned array up-conversion luminescence flexible film applied to the anti-counterfeiting mark, the drawn pattern can be adjusted or the pattern of the dielectric microsphere array can be changed according to different requirements of practical application so as to realize anti-counterfeiting requirements of different scenes;
(3) The dielectric microsphere patterned array up-conversion luminescence flexible film applied to the anti-counterfeiting mark combines the regulation and control effect of the dielectric microsphere on the optical field, has stable physicochemical property in air, realizes anti-counterfeiting application under low-power near infrared light excitation, and has good application prospect in the technical field of optical anti-counterfeiting.
Drawings
FIG. 1 is a schematic diagram of a process for manufacturing a flexible film for converting luminescence on a patterned array of dielectric microspheres applied to security markings;
FIG. 2 shows the power density at 43mW/cm 2 A 980nm near infrared light excited dielectric microsphere patterning array up-conversion luminescence flexible film anti-counterfeiting pattern photo;
FIG. 3 shows the power density at 56mW/cm 2 A 980nm near infrared light excited dielectric microsphere patterning array up-conversion luminescence flexible film anti-counterfeiting pattern photo;
FIG. 4 shows the up-conversion luminescence spectrum of the up-conversion luminescent flexible film after being enhanced by the patterned array of dielectric microspheres;
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A manufacturing method of a dielectric microsphere patterned array up-conversion luminescence flexible film applied to anti-counterfeiting marks comprises the following steps:
step 1: naYF with average size of 40nm 4 :Yb 3+ /Tm 3+ @NaYF 4 :Yb 3+ /Nd 3+ Core-shell type up-conversion nanoparticles (UCNPs) are suspended in cyclohexane dispersion liquid, and the concentration of the up-conversion nanoparticles is 5mg/mL;
step 2: dissolving polymethyl methacrylate (PMMA) powder in toluene to obtain a PMMA solution, wherein the PMMA powder has a grain size of 100 mu m and is dissolved in the toluene in a mass ratio of 0.5wt%, and the additive in the PMMA solution is acetone, and the mass of the additive is 0.2% of the mass of the solvent;
step 3: uniformly mixing UCNP suspension and PMMA solution by repeated suction, and then placing the mixture in a vacuum chamber to remove bubbles to obtain a mixture solution with the concentration of up-conversion nano particles of 0.02 mg/mL;
step 4: the mixture solution with the concentration of the up-conversion nano particles being 0.02mg/mL is spin-coated on the glass substrate, wherein the spin-coating speed is 1000rpm/min at a low speed, the spin-coating time is 15s, and the spin-coating time is 20s at a high speed of 2000 rpm/min. Standing and solidifying in the air after spin coating is finished to obtain a UCNP/PMMA mixture film;
step 5: drawing a required anti-counterfeiting pattern on the UCNP/PMMA mixture film by using a UCNP solution with the concentration of 5mg/mL as ink;
step 6: and (3) attaching a patterning mold to the surface of the UCNP/PMMA film, spraying the dried transparent dielectric microspheres on the patterning position of the mold, mechanically pressurizing by using a 3M low-viscosity adhesive tape, adhering the microspheres on the surface of the film by electrostatic contact and Van der Waals force, repeatedly pressing for a plurality of times, and removing the microspheres which are not adhered on the surface of the film after stripping the 3M adhesive tape. Pressing and stripping for multiple times to obtain a single-layer patterned dielectric microsphere array;
step 7: the patterned UCNP/PMMA film is irradiated by the laser with adjustable power of 980nm, thereby realizing the application of the dielectric microsphere patterning array up-conversion luminescence flexible film which depends on the excitation power.
Example 2
A manufacturing method of a dielectric microsphere patterned array up-conversion luminescence flexible film applied to anti-counterfeiting marks comprises the following steps:
step 1: naYF with average size of 40nm 4 :Yb 3+ /Tm 3+ @NaYF 4 :Yb 3+ /Nd 3+ Core-shell type up-conversion nanoparticles (UCNPs) are suspended in cyclohexane dispersion liquid, and the concentration of the up-conversion nanoparticles is 5mg/mL;
step 2: dissolving polymethyl methacrylate (PMMA) powder in toluene to obtain a PMMA solution, wherein the PMMA powder has a grain size of 100 mu m and is dissolved in the toluene in a mass ratio of 0.7wt%, and the additive in the PMMA solution is acetone, and the mass of the additive is 0.3% of the mass of the solvent;
step 3: uniformly mixing UCNP suspension and PMMA solution by repeated suction, and then placing the mixture in a vacuum chamber to remove bubbles to obtain a mixture solution with the concentration of up-conversion nano particles of 0.04 mg/mL;
step 4: the mixture solution with the concentration of the up-conversion nano particles being 0.04mg/mL is spin-coated on the glass substrate, wherein the spin-coating speed is 1000rpm/min at a low speed, the spin-coating time is 15s, and the spin-coating time is 20s at a high speed of 2000 rpm/min. Standing and solidifying in the air after spin coating is finished to obtain a UCNP/PMMA mixture film;
step 5: drawing a required anti-counterfeiting pattern on the UCNP/PMMA mixture film by using a UCNP solution with the concentration of 5mg/mL as ink;
step 6: and (3) attaching a patterning mold to the surface of the UCNP/PMMA film, spraying the dried transparent dielectric microspheres on the patterning position of the mold, mechanically pressurizing by using a 3M low-viscosity adhesive tape, adhering the microspheres on the surface of the film by electrostatic contact and Van der Waals force, repeatedly pressing for a plurality of times, and removing the microspheres which are not adhered on the surface of the film after stripping the 3M adhesive tape. Pressing and stripping for multiple times to obtain a single-layer patterned dielectric microsphere array;
step 7: the patterned UCNP/PMMA film is irradiated by the laser with adjustable power of 980nm, thereby realizing the application of the dielectric microsphere patterning array up-conversion luminescence flexible film which depends on the excitation power.
Example 3
A manufacturing method of a dielectric microsphere patterned array up-conversion luminescence flexible film applied to anti-counterfeiting marks comprises the following steps:
step 1: naYF with average size of 40nm 4 :Yb 3+ /Tm 3+ @NaYF 4 :Yb 3+ /Nd 3+ Core-shell type up-conversion nanoparticles (UCNPs) are suspended in cyclohexane dispersion liquid, and the concentration of the up-conversion nanoparticles is 5mg/mL;
step 2: dissolving polymethyl methacrylate (PMMA) powder in toluene to obtain a PMMA solution, wherein the PMMA powder has a grain size of 100 mu m and is dissolved in the toluene in a mass ratio of 0.9wt%, and the additive in the PMMA solution is acetone, and the mass of the additive is 0.4% of the mass of the solvent;
step 3: uniformly mixing UCNP suspension and PMMA solution by repeated suction, and then placing the mixture in a vacuum chamber to remove bubbles to obtain a mixture solution with the concentration of up-conversion nano particles of 0.06 mg/mL;
step 4: the mixture solution with the concentration of the up-conversion nano particles being 0.06mg/mL is spin-coated on the glass substrate, wherein the spin-coating speed is 1000rpm/min at a low speed, the spin-coating time is 15s, and the spin-coating time is 20s at a high speed of 2000 rpm/min. Standing and solidifying in the air after spin coating is finished to obtain a UCNP/PMMA mixture film;
step 5: drawing a required anti-counterfeiting pattern on the UCNP/PMMA mixture film by using a UCNP solution with the concentration of 5mg/mL as ink;
step 6: and (3) attaching a patterning mold to the surface of the UCNP/PMMA film, spraying the dried transparent dielectric microspheres on the patterning position of the mold, mechanically pressurizing by using a 3M low-viscosity adhesive tape, adhering the microspheres on the surface of the film by electrostatic contact and Van der Waals force, repeatedly pressing for a plurality of times, and removing the microspheres which are not adhered on the surface of the film after stripping the 3M adhesive tape. Pressing and stripping for multiple times to obtain a single-layer patterned dielectric microsphere array;
step 7: the patterned UCNP/PMMA film is irradiated by the laser with adjustable power of 980nm, thereby realizing the application of the dielectric microsphere patterning array up-conversion luminescence flexible film which depends on the excitation power.
Example 4
A manufacturing method of a dielectric microsphere patterned array up-conversion luminescence flexible film applied to anti-counterfeiting marks comprises the following steps:
step 1: naYF with average size of 40nm 4 :Yb 3+ /Tm 3+ @NaYF 4 :Yb 3+ /Nd 3+ Core-shell type up-conversion nanoparticles (UCNPs) are suspended in cyclohexane dispersion liquid, and the concentration of the up-conversion nanoparticles is 5mg/mL;
step 2: polymethyl methacrylate (PMMA) powder is dissolved in toluene, and the obtained PMMA solution consists of powder, a solvent and additives, wherein the grain size of the PMMA powder is 100 mu m, the PMMA powder is dissolved in toluene in a mass ratio of 1wt%, and the additive in the PMMA solution is acetone, and the mass of the additive is 0.6% of the mass of the solvent;
step 3: uniformly mixing UCNP suspension and PMMA solution by repeated suction, and then placing the mixture in a vacuum chamber to remove bubbles to obtain a mixture solution with the concentration of up-conversion nano particles of 0.07 mg/mL;
step 4: the mixture solution with the concentration of the up-conversion nano particles of 0.07mg/mL is spin-coated on the glass substrate, wherein the spin-coating speed is 1000rpm/min at a low speed, the spin-coating time is 15s, and the spin-coating time is 20s at a high speed of 2500 rpm/min. Standing and solidifying in the air after spin coating is finished to obtain a UCNP/PMMA mixture film;
step 5: drawing a required anti-counterfeiting pattern on the UCNP/PMMA mixture film by using a UCNP solution with the concentration of 5mg/mL as ink;
step 6: and (3) attaching a patterning mold to the surface of the UCNP/PMMA film, spraying the dried transparent dielectric microspheres on the patterning position of the mold, mechanically pressurizing by using a 3M low-viscosity adhesive tape, adhering the microspheres on the surface of the film by electrostatic contact and Van der Waals force, repeatedly pressing for a plurality of times, and removing the microspheres which are not adhered on the surface of the film after stripping the 3M adhesive tape. Pressing and stripping for multiple times to obtain a single-layer patterned dielectric microsphere array;
step 7: the patterned UCNP/PMMA film is irradiated by the laser with adjustable power of 980nm, thereby realizing the application of the dielectric microsphere patterning array up-conversion luminescence flexible film which depends on the excitation power.
The anti-fake luminous effect of embodiment 1, namely the anti-fake luminous effects of fig. 2 and 3 in the description of the drawings are similar to those of embodiment 2-4, and only the excitation power dependence is different in anti-fake application.
Finally, the above examples of the present invention are provided for clarity of illustration only and are not intended to limit the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. Not all embodiments are exhaustive. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A manufacturing method of a dielectric microsphere patterned array up-conversion luminescence flexible film applied to anti-counterfeiting marks is characterized by comprising the following steps:
step 1: naYF is prepared 4 : Yb 3+ / Tm 3+ @ NaYF 4 : Yb 3+ /Nd 3+ Suspending core-shell up-conversion nanoparticles (UCNPs) in the dispersion liquid to obtain UCNP suspension liquid; the concentration of the up-conversion nano particles is 5mg/mL;
step 2: polymethyl methacrylate (PMMA) powder is dissolved in toluene to obtain PMMA solution; the PMMA solution consists of powder, solvent toluene and additives, wherein the PMMA powder is dissolved in toluene in a mass ratio of 0.3-1 wt%; the additive in the PMMA solution is acetone, and the weight of the additive is 0.05-0.6wt% of the weight of the solvent toluene; step 3: mixing the UCNP suspension and PMMA solution, and then placing the mixture in a vacuum chamber to remove bubbles; the UCNP concentration in the mixture is 0.02-0.1 mg/mL;
step 4: spin-coating the UCNP/PMMA mixture solution on a glass substrate, and standing and solidifying in air to obtain a UCNP/PMMA mixture film;
step 5: drawing a required anti-counterfeiting pattern on the UCNP/PMMA mixture film by using the UCNP solution as ink; the UCNP solution with the concentration of 5mg/mL is used as the ink, and the concentration of the up-conversion nano particles in the mixture film is 0.02-0.1 mg/mL;
step 6: pasting a patterning mould on the surface of a UCNP/PMMA film, spraying dry transparent dielectric microspheres on the patterning position of the mould, mechanically pressurizing by using a 3M adhesive tape, adhering the microspheres on the surface of the film by electrostatic contact and Van der Waals force, repeatedly pressing for a plurality of times, and removing the microspheres which are not adhered on the surface of the film after stripping the 3M adhesive tape; and (3) carrying out repeated pressing and stripping to obtain a single-layer patterned dielectric microsphere array.
2. The method for manufacturing the dielectric microsphere patterned array up-conversion luminescence flexible film applied to the anti-counterfeiting mark according to claim 1, wherein the method comprises the following steps: in the step 1, the average size of the up-conversion nano particles is 30-40nm, and the dispersion solvent is cyclohexane.
3. The manufacturing method according to claim 1, characterized in that: the PMMA powder has a grain size of 70-100 mu m.
4. The manufacturing method according to claim 1, characterized in that: in the step 4, the spin coating speed is set to 1500-3000r/min, and the spin time is set to 15-30s.
5. The use of the film prepared by the manufacturing method according to claim 1, wherein the patterned UCNP/PMMA film is irradiated with laser light to realize the use of the excitation power dependent dielectric microsphere patterned array up-conversion luminescent flexible film.
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| CN110735160A (en) * | 2019-05-10 | 2020-01-31 | 湖北大学 | Preparation method of up-conversion fluorescent anti-counterfeiting labels |
| CN111040225A (en) * | 2019-12-05 | 2020-04-21 | 中山大学 | Repeatedly erasable anti-counterfeiting film based on photonic crystal structural color and preparation method and application thereof |
| CN113105886A (en) * | 2021-04-26 | 2021-07-13 | 东南大学 | Up-conversion luminescent composite nano powder with variable luminescent color and preparation method and application thereof |
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