CN114350350B - Pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect as well as preparation method and application thereof - Google Patents
Pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effects and a preparation method and application thereof. The pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effects comprises the following components in percentage by mass: europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder: 10% -90%; colorant having effect of changing color with light: 10 to 90 percent. The preparation method of the pigment with photoluminescence, mechanoluminescence and light-dependent heterochromous effects comprises the following steps: and (3) physically mixing the europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder and a pigment with a light-dependent heterochromatic effect to obtain the europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder. The pigment has the effects of photoluminescence, mechanoluminescence and light-dependent color change, has obvious color change effect under different light source conditions, is simple in preparation process, low in cost, easy for industrial production and wide in application prospect in the technical field of anti-counterfeiting.
Description
Technical Field
The invention relates to the technical field of anti-counterfeiting, in particular to a pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effects as well as a preparation method and application thereof.
Background
The anti-counterfeiting technology is a measure which is adopted for achieving the anti-counterfeiting purpose and is convenient for a user to distinguish true from false, and has practical application value for social stability and economic development. The traditional anti-counterfeiting technologies such as scratch-off, bar code and watermark have the problems of single mode, easy counterfeiting and the like, and the security is not high, and the advanced anti-counterfeiting technologies such as radio frequency identification and laser holography have the problem of high cost and are greatly limited in application. In recent years, fluorescent anti-counterfeiting technology becomes the leading edge and hot spot of research, and optical materials are the key of the fluorescent anti-counterfeiting technology. The existing fluorescent anti-counterfeiting technology generally adopts optical materials such as organic dyes, semiconductor quantum dots, rare earth doped luminescent powder and the like, the optical materials do not have anti-counterfeiting capability in normal environment, but can show the luminescent characteristic under the excitation of specific wavelength light, the anti-counterfeiting mode is single, the moldability is higher, and the practical application requirements are difficult to be completely met.
Therefore, it is very important to develop a non-toxic, chemically stable, multifunctional powder that can exhibit different colors and luminescent properties under different environmental conditions, which helps to broaden the application modes of fluorescent anti-counterfeiting technologies and significantly improve the anti-counterfeiting security.
Disclosure of Invention
The invention aims to provide a pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effects, and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
a pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effects comprises the following components in percentage by mass:
europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder: 10% -90%;
colorant having effect of changing color with light: 10 to 90 percent.
Preferably, the europium-dysprosium-zirconium co-doped strontium aluminate fluorescent powder has a chemical general formula as follows: srAl 2 O 4 :Eu 2+ 0.02 ,Dy 3 + 0.03 ,Zr 4+ x In the formula, 0<x≤0.2。
Preferably, the europium-dysprosium-zirconium co-doped strontium aluminate fluorescent powder is prepared by the following method: with reference to the general chemical formula SrAl 2 O 4 :Eu 2+ 0.02 ,Dy 3+ 0.03 ,Zr 4+ x The stoichiometric ratio of each element in the mixture is SrCO 3 、Al 2 O 3 、Eu 2 O 3 、Dy 2 O 3 、ZrO 2 Mixing with a fluxing agent, calcining in a reducing atmosphere, cooling, grinding and sieving to obtain the europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder.
Preferably, the fluxing agent is at least one selected from boric acid, chloride salts, fluoride salts and ammonium salts.
Preferably, the amount of the flux added is SrCO 3 、Al 2 O 3 、Eu 2 O 3 、Dy 2 O 3 And ZrO 2 0 to 12 percent of the total mass.
Preferably, the reducing atmosphere is N 2 -H 2 Mixing the atmosphere.
Preferably, the calcination is carried out at 1100-1400 ℃, and the heat preservation time is 1-6 h.
Preferably, the number of the selected screens is 100-325.
Preferably, the particle size of the europium-dysprosium-zirconium co-doped strontium aluminate fluorescent powder is less than or equal to 150 mu m.
Preferably, the pigment with the effect of changing color along with light is selected from at least one of holmium molybdate, neodymium disilicate and neodymium aluminate.
Preferably, the colorant having a light-dependent color effect is prepared by the following method: refer to the general chemical formula Ho 2 MoO 6 、Nd 2 MoO 6 、NdAlO 3 And Nd 2 Si 2 O 7 Weighing Ho according to stoichiometric ratio of elements 2 O 3 、Nd 2 O 3 、MoO 3 、 Al 2 O 3 、SiO 2 Mixing with fluxing agent, calcining in air atmosphere, cooling, grinding and sieving to obtain the pigment with light-dependent color effect.
Preferably, the flux is at least one selected from boric acid, chloride salt, fluoride salt and ammonium salt.
Preferably, the amount of the flux added is 0 to 6% of the total mass of the other raw materials.
Preferably, the calcination is carried out at 1000-1300 ℃, and the heat preservation time is 1-6 h.
Preferably, the number of the selected screens is 100-325.
Preferably, the pigment having the effect of changing color with light has a particle size of 150 μm or less.
The preparation method of the pigment with photoluminescence, mechanoluminescence and light-dependent heterochromous effects comprises the following steps: and (3) physically mixing the europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder with a pigment with a light-dependent heterochromatic effect to obtain the pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect.
The invention has the beneficial effects that: the pigment has the effects of photoluminescence, mechanoluminescence and light-dependent color change, has obvious color change effect under different light source conditions, is simple in preparation process, low in cost, easy for industrial production and wide in application prospect in the technical field of anti-counterfeiting.
Specifically, the method comprises the following steps:
1) The colorants of the present invention are stable under different light source conditions (e.g.: d65, A, F2, F11 and an ultraviolet lamp), and can be effectively excited by ultraviolet light, sunlight and fluorescence to emit yellow-green light;
2) The pigment of the invention can also emit light under the excitation of mechanical force;
3) The pigment of the invention has simple preparation process and low cost, is easy to carry out industrial production, and can be applied to the technical field of anti-counterfeiting safety.
Drawings
FIG. 1 is an XRD pattern of a coloring material having photoluminescence, mechanoluminescence and a photoheterochromic effect in example 1.
FIG. 2 is a PL diagram of a coloring material having photoluminescence, and photochromic effects in example 1.
FIG. 3 is an ML chart of a coloring material having photoluminescence, and photochromic effects in example 1.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a colorant with photoluminescence, mechanoluminescence and photoheterochromous effects, its preparation method includes the following steps:
1) With reference to the general chemical formula SrAl 2 O 4 :0.02Eu 2+ ,0.03Dy 3+ ,0.05Zr 4+ Weighing 2.9526g of SrCO according to stoichiometric ratio 3 2.0392g of Al 2 O 3 0.0704g Eu 2 O 3 0.01119g Dy 2 O 3 0.1232g of ZrO 2 And 0.1059g of H 3 BO 3 Mechanically mixing, adding the obtained mixed powder into an alumina crucible, placing in a tube furnace, and charging with N 2 And H 2 Keeping the temperature of 1300 ℃ for 3h in a reducing atmosphere consisting of 19:1 by volume, cooling, grinding and sieving with a 150-mesh sieve to obtain europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder;
2) See general chemical formula Ho 2 MoO 6 Weighing 7.5572g Ho according to stoichiometric ratio 2 O 3 And 2.8788g of MoO 3 Mechanically mixing, adding the obtained mixed powder into an alumina crucible, placing the alumina crucible in a tubular furnace, filling air, preserving the temperature for 3 hours at 1000 ℃, cooling, grinding and sieving by a 150-mesh sieve to obtain a holmium molybdate pigment;
3) Mixing europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder and holmium molybdate pigment according to a mass ratio of 1:1, and grinding to obtain the pigment with photoluminescence, mechanoluminescence and light-dependent heterochromous effects.
And (3) performance testing:
1) The crystal structure of the coloring material having photoluminescence, mechanoluminescence and photoheterochromatic effects of this example was measured with an X-ray diffractometer of model X' Pert Pro from PANALYtic, netherlands, and the X-ray diffraction (XRD) pattern obtained is shown in FIG. 1.
As can be seen from fig. 1: the diffraction peak of the coloring material of this example having photoluminescence, mechanoluminescence and photochromic effectsSharp and good crystallinity, and its crystal phase contains SrAl 2 O 4 Crystalline phase and Ho 2 MoO 6 The crystal phases are monoclinic phase crystals.
2) The fluorescence emission performance of the pigment with photoluminescence, mechanoluminescence and heterochromous effect of the present example was tested using a fluorescence spectrometer type TRIA-320 from Edinburgh, UK, and the obtained Photoluminescence (PL) spectrum is shown in FIG. 2.
As can be seen from fig. 2: the coloring material having photoluminescence, mechanoluminescence and photochromic effects of the present example emits a broad spectrum of 450 to 600nm (yellow-green light) under the excitation of 365nm light.
3) The mechanoluminescence performance of the colorant having photoluminescence, mechanoluminescence and heterochromous effect of the present example was tested by using a mechanoluminescence meter, and the obtained Mechanoluminescence (ML) spectrum is shown in fig. 3.
As can be seen from fig. 3: the pigment with photoluminescence, mechanoluminescence and heterochromous effect has obvious mechanoluminescence performance, a test sample can have an obvious mechanoluminescence peak under the excitation of impact force, and the luminous intensity is increased rapidly and then gradually decreased.
Comprehensive tests prove that the pigment with photoluminescence, photoluminescence and light-dependent heterochromatic effects in the embodiment can be effectively excited by ultraviolet light, sunlight and fluorescence to emit yellowish green light visible to naked eyes, can emit yellowish green light under the action of mechanical forces such as impact force, extrusion force and the like, and can also have heterochromatic effects under different light sources (such as sunlight D65, an incandescent lamp A, a cold white fluorescent lamp F2 and a three-frequency fluorescent lamp F11), and the test results of L a b values show that: the color difference between the standard illuminant D65 (pale yellow-green) and the illuminant F11 (red hue) was 12.48.
Example 2:
a colorant with photoluminescence, mechanoluminescence and photoheterochromous effects, its preparation method includes the following steps:
1) With reference to the general chemical formula SrAl 2 O 4 :0.02Eu 2+ ,0.03Dy 3+ ,0.05Zr 4+ 2.9526g of SrCO is weighed according to stoichiometric ratio 3 2.0392g of Al 2 O 3 0.0704g Eu 2 O 3 0.01119g Dy 2 O 3 0.1232g of ZrO 2 And 0.1059g of H 3 BO 3 Mechanically mixing, adding the obtained mixed powder into an alumina crucible, placing the alumina crucible in a tube furnace, and charging N 2 And H 2 Keeping the temperature at 1300 ℃ for 3h according to a reducing atmosphere consisting of the components with the volume ratio of 19 to 1, cooling, grinding and sieving by a 150-mesh sieve to obtain europium-dysprosium-zirconium co-doped strontium aluminate fluorescent powder;
2) Reference chemical formula Nd 2 MoO 6 Weighing 6.7296g Nd according to stoichiometric ratio 2 O 3 And 2.8788g of MoO 3 Mechanically mixing, adding the obtained mixed powder into an alumina crucible, placing the alumina crucible in a tubular furnace, filling air, preserving the heat at 1200 ℃ for 3 hours, cooling, grinding and sieving by a 150-mesh sieve to obtain a holmium molybdate pigment;
3) Mixing the europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder and the holmium molybdate pigment according to the mass ratio of 1:1, and grinding to obtain the pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effects.
Comprehensive tests prove that the pigment with photoluminescence, photoluminescence and light-dependent heterochromatic effects in the embodiment can be effectively excited by ultraviolet light, sunlight and fluorescence to emit yellowish green light visible to naked eyes, can emit yellowish green light under the action of mechanical forces such as impact force, extrusion force and the like, and can also have heterochromatic effects under different light sources (such as sunlight D65, an incandescent lamp A, a cold white fluorescent lamp F2 and a three-frequency fluorescent lamp F11), and the test results of L a b values show that: the color difference between standard illuminant a (violet) and F11 (cyan) was 8.09.
Example 3:
a colorant with photoluminescence, mechanoluminescence and photoheterochromous effects, its preparation method includes the following steps:
1) With reference to the general chemical formula SrAl 2 O 4 :0.02Eu 2+ ,0.03Dy 3+ ,0.05Zr 4+ Weighing 2.9526g of SrCO according to stoichiometric ratio 3 2.0392g of Al 2 O 3 0.0704g Eu 2 O 3 0.01119g Dy 2 O 3 0.1232g of ZrO 2 And 0.1059g of H 3 BO 3 Mechanically mixing, adding the obtained mixed powder into an alumina crucible, placing the alumina crucible in a tube furnace, and charging N 2 And H 2 Keeping the temperature of 1300 ℃ for 3h in a reducing atmosphere consisting of 19:1 by volume, cooling, grinding and sieving with a 150-mesh sieve to obtain europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder;
2) Reference chemical formula Nd 2 Si 2 O 7 Weighing 6.7296g Nd according to stoichiometric ratio 2 O 3 2.4032g of SiO 2 And 0.1827g of H 3 BO 3 Mechanically mixing, adding the obtained mixed powder into an alumina crucible, placing the alumina crucible in a tubular furnace, filling air, keeping the temperature at 1200 ℃ for 3 hours, cooling, grinding, and sieving by a 150-mesh sieve to obtain a holmium molybdate pigment;
3) Mixing europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder and holmium molybdate pigment according to a mass ratio of 1:1, and grinding to obtain the pigment with photoluminescence, mechanoluminescence and light-dependent heterochromous effects.
Comprehensive tests prove that the pigment with photoluminescence, photoluminescence and light-dependent heterochromatic effects in the embodiment can be effectively excited by ultraviolet light, sunlight and fluorescence to emit yellowish green light visible to naked eyes, can emit yellowish green light under the action of mechanical forces such as impact force, extrusion force and the like, and can also have heterochromatic effects under different light sources (such as sunlight D65, an incandescent lamp A, a cold white fluorescent lamp F2 and a three-frequency fluorescent lamp F11), and the test results of L a b values show that: the color difference between standard illuminant A (light pink) and F11 (light yellow) was 6.61.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. The pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effects is characterized by comprising the following components in percentage by mass:
europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder: 10% -90%;
colorant having effect of changing color with light: 10% -90%;
the europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder has the chemical general formula: srAl 2 O 4 :Eu 2+ 0.02 ,Dy 3+ 0.03 ,Zr 4+ x In the formula, 0<x≤0.2；
The coloring material with the effect of changing color along with light is at least one selected from holmium molybdate, neodymium pyrosilicate and neodymium aluminate;
the particle size of the europium-dysprosium-zirconium co-doped strontium aluminate fluorescent powder is less than or equal to 150 mu m;
the grain diameter of the pigment with the effect of changing color along with light is less than or equal to 150 mu m.
2. A colorant having both photoluminescent, mechanoluminescent and photochromic effects according to claim 1, wherein: the europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder is prepared by the following method: with reference to the general chemical formula SrAl 2 O 4 :Eu 2 + 0.02 ,Dy 3+ 0.03 ,Zr 4+ x The stoichiometric ratio of each element in the mixture is SrCO 3 、Al 2 O 3 、Eu 2 O 3 、Dy 2 O 3 、ZrO 2 Mixing with a fluxing agent, calcining in a reducing atmosphere, cooling, grinding and sieving to obtain the europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder.
3. A colorant having both photoluminescent, mechanoluminescent and photochromic effects according to claim 2, wherein: the fluxing agent is selected from at least one of boric acid, chloride salt, fluoride salt and ammonium salt.
4. A colorant having both photoluminescent, mechanoluminescent and photochromic effects according to claim 2, wherein: the addition amount of the fluxing agent is SrCO 3 、Al 2 O 3 、Eu 2 O 3 、Dy 2 O 3 And ZrO 2 0 to 12 percent of the total mass.
5. A colorant having both photoluminescent, mechanoluminescent and photochromic effects according to claim 2, wherein: the calcination is carried out at 1100-1400 ℃, and the heat preservation time is 1-6 h.
6. A method for preparing a colorant having photoluminescence, mechanoluminescence and metachromatism effects as defined in any one of claims 1 to 5, comprising the steps of: and (3) physically mixing the europium-dysprosium-zirconium codoped strontium aluminate fluorescent powder with a pigment with a light-dependent heterochromatic effect to obtain the pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect.
7. Use of a colorant having photoluminescent, mechanoluminescent and photochromic effects according to any one of claims 1 to 5 in the field of anti-counterfeiting.
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