CN117467441A - Multi-mode fluorescent anti-counterfeiting material and anti-counterfeiting demonstration device - Google Patents
Multi-mode fluorescent anti-counterfeiting material and anti-counterfeiting demonstration device Download PDFInfo
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Abstract
The invention belongs to the technical field of luminescence and display, and particularly relates to a multi-mode fluorescent anti-counterfeiting material and an anti-counterfeiting demonstration device. The molecular formula of the multi-mode fluorescent anti-counterfeiting material is Re 2 O 2 S:0.08Yb,0.02Er@Re 2 O 2 S0.05 Tb (re=y, gd, la). Re provided by the invention 2 O 2 S:0.08Yb,0.02Er@Re 2 O 2 S0.05 Tb (Re=Y, gd, la) anti-counterfeiting material presents different luminescent colors at 1530nm, 980nm, 254nm (or X rays) and different temperatures, has higher anti-counterfeiting grade, is difficult to replace and forge and greatly improves the anti-counterfeiting compared with the prior single/dual mode material capable of generating one or two luminescent colors under the excitation of one to two specific wavelengthsPseudo security.
Description
Technical Field
The invention relates to a multi-mode fluorescent anti-counterfeiting material and an anti-counterfeiting demonstration device, and belongs to the technical field of light emission and display.
Background
Counterfeit products seriously affect the normal development of socioeconomic performance and the lives of people, and become increasingly serious global problems, causing huge economic losses each year, and being internationally regarded as 'second most public nuisance in the world next to vending toxicity'. In order to maintain legal rights of consumers and enterprises, research on anti-counterfeiting technology has become an international front-end hotspot in recent years, and a great deal of related reports have appeared. Among them, the fluorescent anti-counterfeiting technology is widely focused on having the advantages of high concealment, easy observation, difficult replication, mass production and the like.
The luminescent materials adopted by the fluorescent anti-counterfeiting technology mainly comprise rare earth luminescent materials (1) WU Youfusheng, WU Wei.Combinations of superior inorganic phosphors for level-tunable information hiding and encoding.advanced Optical Materials,2021,9 (17): 2100281; (2) TSANG Mingku, BAI Gongxun, HAO Jianhua. Stimuli-responsive upconversion luminescence nanomaterials and films for various applications chemical Society Reviews,2015,44 (6): 1585-1607; (3) LIU Xiaowang, JIQiang, HU Qian, et al Dual-mode Long-lived luminescence of Mn 2+ -doped nanoparticles for multilevel anti-counterfeiting.ACS Applied Materials&Interface,2019,11 (33): 30146-30153 ], semiconductor quantum dots [ 4 ] XU Leimeng, CHEN Jiawei, SONG Jizhong, et al double protected all-inorganic perovskite nanocrystals by crystalline matrix and silica for triple-moddal anti-counter-characteristics codes.ACS Applied Materials&Interface,2017,9 (31): 26556-26564; (5) CHEN Xi, WANG Qi, WANG Xiaojun, et al Synthesis and performance of ZnO quantum dots water-based fluorescent ink for anti-countering applications, scientific Reports,2021,11:5841 ], luminescent carbon materials [ 6 ] JIANG Kai, WANG Yuhui, LI Zhongjun, et al Aftergrow of carbon dots: mechanics, strategy and applications. Materials Chemistry Frontiers,2019,4 (2): 386-399; (7) BAKER S N, BAKER G A.luminescence carbon nanodots: email nanodots Chemie International Edition,2010,49:6726-6744 ], organic luminescent materials etc. (8) AHANGER F A, NAZIR N, LONE M S, et al.emission color tuning and white light generation from a trimolecular cocktail in cationic micellar system with promising applicability in the anticounterfeiting technology, langmuir,2021,37:7730-7740; (9) HAN Jiangli, FENG Wenhui, MULETA Yadeta, et al Small-molecular-doped organic crystals with long-advanced Functional Materials,2019,29 (30): 1902503). The rare earth luminescent material has stable physical and chemical properties, wide emission wavelength coverage range and narrow emission band, and is the optimal fluorescent anti-counterfeiting material. The rare earth luminescent materials currently applied to fluorescent anti-counterfeiting technology are mostly single/double colors or single/double modes capable of generating one or two luminescent colors under the excitation of one to two specific wavelengths, the technical barriers of the luminescent materials are not high, and the luminescent materials are possibly replaced by substances with the same emission, so that the luminescent materials still have the risks of imitation and counterfeiting.
Disclosure of Invention
The invention aims to provide a multi-mode fluorescent anti-counterfeiting material and an anti-counterfeiting demonstration device, compared with the single/dual modes, the multi-mode anti-counterfeiting material can greatly increase the imitation difficulty, thereby greatly improving the anti-counterfeiting grade.
In order to achieve the above object, the technical scheme of the present invention is as follows:
in one aspect, the invention provides a multi-mode fluorescent anti-counterfeiting material, wherein the molecular formula of the material is Re 2 O 2 S:0.08Yb,0.02Er@Re 2 O 2 S0.05 Tb, where re=y, gd, la.
Further, the material emits red light upon excitation at a wavelength of 1530 nm. Tb of shell layer under excitation of 1530nm wavelength 3+ Ion does not emit light, er in nuclear layer 3+ The ions present two groups of emission bands, namely red light and green light, and the red light band is far stronger than the green light, so that the whole material emits red light.
Further, the material emits green light upon excitation at 254nm wavelength or X-rays. Tb of the shell layer under 254nm wavelength or X-ray excitation 3+ The ions show stronger green luminescence, er in the nuclear layer 3+ The ion luminescence is very weak and is completely controlled by Tb 3+ The green luminescence of the ions is masked, and thus the overall luminescence color is green.
Further, the material emits yellow light at 303K under excitation at 980nm wavelength. Tb of shell layer under 980nm wavelength excitation 3+ Ion does not emit light, er in nuclear layer 3+ The ions exhibit both red and green emission bands, but green emission is significantly enhanced compared to excitation at 1530nm, with a reduced ratio of red to green emission intensities, resulting in an overall emission color of yellow.
Further, the material emits orange-red light at 513K under excitation at 980nm wavelength. As the temperature increases from 303K to 513K, the green intensity drops sharply, while the red intensity changes only slightly, causing the overall emission color to change from yellow to orange-red.
The invention also provides application of the multi-mode fluorescent anti-counterfeiting material in preparation of anti-counterfeiting materials.
By Re 2 O 2 S:0.08Yb,0.02Er@Re 2 O 2 S0.05 Tb (Re=Y, gd, la) material Er in core-shell structure 3+ And Tb 3+ The ions have different luminescent colors under the excitation of different wavelengths, and meanwhile, the luminescent colors can also change along with the change of temperature, so that the fluorescent anti-counterfeiting is realized through the different luminescent colors.
The invention also provides application of the multi-mode fluorescent anti-counterfeiting material in an anti-counterfeiting demonstration device.
The display device comprises a luminescent layer and a matrix, wherein the luminescent layer is prepared by dispersing the multi-mode fluorescent anti-counterfeiting material in a transparent medium containing an additive; the transparent medium is one or more of epoxy resin, acrylic resin, polyester resin, polyethylene resin, polyamide resin, perchloroethylene resin, polyvinyl chloride resin, ethylene-vinyl acetate copolymer resin, alkyd resin and polymethyl methacrylate;
the additive is one or more of a curing agent, a stabilizing agent, a leveling agent, a defoaming agent, a plasticizer, a surfactant, a flame retardant, a pigment and a surface modifier; the substrate is glass, ceramic, aluminum foil plate, tin plate, aluminum plate, stainless steel plate, polyester plate, polypropylene plate, polyvinyl chloride plate or polyethylene plate.
The beneficial effects of the invention are as follows:
re provided by the invention 2 O 2 S:0.08Yb,0.02Er@Re 2 O 2 The 0.05Tb (Re=Y, gd, la) anti-counterfeiting material presents different luminescent colors at 1530nm, 980nm and 254nm (or X rays) and different temperatures, and compared with the single/double mode material capable of generating one or two luminescent colors under the excitation of one to two specific wavelengths in the past, the anti-counterfeiting material has higher anti-counterfeiting grade, is difficult to replace and forge, and greatly improves the anti-counterfeiting safety. Meanwhile, the rare earth oxysulfide with excellent luminescence property is used as a matrix, and the rare earth oxysulfide has the characteristics of stable physical and chemical properties, no toxicity, excellent optical performance and the like, and is suitable for anti-counterfeiting application of daily necessities.
The anti-counterfeiting demonstration device provided by the invention can display two-dimensional luminous images with different colors under the excitation of 1530nm, 980nm and 254nm (or X rays), and can be applied to experimental teaching of universities.
Drawings
FIG. 1 is Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S is 0.05Tb is an emission spectrum under 980nm excitation;
FIG. 2 is Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S is an emission spectrum of 0.05Tb under 1530nm excitation;
FIG. 3 is Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S is 0.05Tb of emission spectrum under 254nm excitation;
FIG. 4 is Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S is 0.05Tb of emission spectrum under X-ray excitation;
FIG. 5 is Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S0.05 Tb is excited at different wavelengthsThe luminous color coordinates are sent down;
FIG. 6 is Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S, 0.05Tb is an emission spectrum (excitation wavelength is 980 nm) changing along with the temperature;
FIG. 7 is Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S, luminescence color coordinates of 0.05Tb with temperature change (excitation wavelength is 980 nm).
Detailed Description
The following examples of the present invention are given as illustration, but the present invention is not limited to these examples.
Example 1
Multi-mode fluorescent anti-counterfeiting material with molecular formula of Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S is 0.05Tb, and the preparation method is as follows:
(1) 90ml of Y (NO) are measured separately 3 ) 3 (0.1mol/L)、8ml Yb(NO 3 ) 3 (0.1 mol/L) and 2ml Er (NO) 3 ) 3 Mixing (0.1 mol/L) solution with deionized water to obtain 200ml of rare earth nitrate mixed solution, dissolving 1mol of urea in deionized water to obtain 800ml of urea solution, respectively heating the two solutions to 60 ℃, mixing to obtain 1000ml of mixed solution, continuously heating to 85 ℃, continuously curing for 1.5h after turbidity of the mixed solution is observed to obtain a first precursor precipitate, centrifuging the precipitate, respectively washing with deionized water and absolute ethyl alcohol, drying at 40 ℃ for 12h, and roasting the dried precursor powder in a resistance furnace at 600 ℃ for 1h to obtain Y 2 O 3 0.08Yb,0.02Er powder;
(2) 95ml of Y (NO) was measured separately 3 ) 3 (0.1 mol/L) and 5ml of Tb (NO) 3 ) 3 Mixing (0.1 mol/L) solution with deionized water to obtain 200ml of rare earth nitrate mixed solution, dissolving 1mol of urea in deionized water to obtain 800ml of urea solution, respectively heating the two solutions to 60 ℃, mixing to obtain 1000ml of mixed solution, and mixing the Y obtained in the step (1) 2 O 3 0.08Yb,0.02Er powder was ultrasonically dispersed in the mixed solution, followed byHeating the mixed solution to 85 ℃, curing for 30min to obtain a precursor precipitate II, centrifuging, washing, drying and annealing at 600 ℃ for 1h to obtain a core-shell structure Y 2 O 3 :0.08Yb,0.02Er@Y 2 O 3 0.05Tb powder;
(3) Spreading the core-shell structure powder obtained in the step (2) in a quartz boat, putting the quartz boat at the bottom of a quartz tube, putting a proper amount of sulfur powder in another quartz boat, putting the quartz boat at a proper position in the quartz tube, introducing argon gas into the quartz tube for 40min, exhausting air, then placing the quartz tube in a resistance furnace at 800 ℃, controlling sulfur vapor by controlling the flow of the argon gas, taking out the quartz tube after vulcanizing for 1h, cooling to room temperature, and finally obtaining Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S0.05 Tb powder.
The application of the multi-mode fluorescent anti-counterfeiting material in an anti-counterfeiting demonstration device comprises a luminous layer and a matrix, and the preparation method is as follows:
by mixing the above Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 And S, adding 0.05Tb powder, epoxy resin, a leveling agent and a defoaming agent into a high-speed stirrer together for mechanical mixing, uniformly mixing all materials, coating the materials on an aluminum plate, forming a luminescent layer through heat treatment, and assembling the luminescent layer on a substrate to obtain the anti-counterfeiting demonstration device. Since the substrate is made of a material having excellent heat conduction properties, the light-emitting layer can be subjected to irradiation with high excitation power.
FIGS. 1, 2, 3 and 4 are prepared Y 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S0.05 Tb sample respectively emits spectra under 980nm, 1530nm, 254nm and X-ray excitation, and the corresponding luminous color coordinates are shown in FIG. 5.
Under excitation at 980nm and 1530nm wavelengths, the sample showed only Er in the core 3+ Red and green light emissions of ions, but the relative intensities of red and green light are different, resulting in overall luminescent colors of the sample being yellow and red, respectively; er in the nucleus under 254nm wavelength or X-ray excitation 3+ The ion luminescence is very weak and is completely covered by the outer layer Tb 3+ The green luminescence of the ions is masked, so the overall luminescence colorGreen.
FIG. 6 is a graph of Y under 980nm excitation 2 O 2 S:0.08Yb,0.02Er@Y 2 O 2 S0.05 Tb sample with temperature change emission spectrum, and the luminous color coordinates at different temperatures are shown in FIG. 7.
It can be seen that as the temperature increases from 303K to 513K, the green emission intensity of the sample drops sharply, while the red intensity changes only slightly, so that the overall emission color changes from yellow to orange-red.
In this embodiment, the rare earth element in the matrix may be one or a combination of Y, gd, la, with no effect on the final product.
The above examples are only preferred embodiments of the present invention and are not limiting of the implementation. The protection scope of the present invention shall be subject to the scope defined by the claims. Other variations or modifications may be made in the various forms based on the above description. Obvious variations or modifications of the embodiments are within the scope of the invention.
Claims (7)
1. A multi-mode fluorescent anti-counterfeiting material is characterized in that the molecular formula of the material is Re 2 O 2 S:0.08Yb,0.02Er@Re 2 O 2 S0.05 Tb, where re=y, gd, la.
2. The multi-mode fluorescent anti-counterfeiting material according to claim 1, wherein the material emits red light under excitation at a wavelength of 1530 nm.
3. The multi-mode fluorescent anti-counterfeiting material according to claim 1, wherein the material emits green light under excitation at 254nm wavelength or X-ray.
4. The multi-mode fluorescent anti-counterfeiting material according to claim 1, wherein the material emits yellow light under excitation at 980nm wavelength at 303K.
5. The multi-mode fluorescent anti-counterfeiting material according to claim 1, wherein the material emits orange-red light under excitation at 980nm wavelength at 513K.
6. Use of a multi-mode fluorescent anti-counterfeiting material according to any one of claims 1 to 5 for preparing an anti-counterfeiting material.
7. Use of a multi-mode fluorescent anti-counterfeiting material according to any one of claims 1 to 5 in an anti-counterfeiting presentation device.
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