CN109054062B - Photoluminescent film, and preparation method and application thereof - Google Patents

Photoluminescent film, and preparation method and application thereof Download PDF

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CN109054062B
CN109054062B CN201811179235.6A CN201811179235A CN109054062B CN 109054062 B CN109054062 B CN 109054062B CN 201811179235 A CN201811179235 A CN 201811179235A CN 109054062 B CN109054062 B CN 109054062B
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film
quantum dots
photoluminescence
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quantitative
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CN109054062A (en
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张孟
周群刚
汪红
王明元
郑然�
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Suzhou City Central Blood Station
Jiaxing Nading Optoelectronics Technology Co ltd
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Suzhou City Central Blood Station
Jiaxing Nading Optoelectronics Technology Co ltd
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Abstract

The invention discloses a photoluminescent film and a preparation method and application thereof, wherein the preparation method of the photoluminescent film comprises the following steps: at least more than one quantum dot, photoinitiator, light scattering particles and resin are mixed and cured under the condition of keeping out of the sun to prepare the photoluminescence film. The invention prepares the photoluminescence film by introducing the free radical initiator into the quantum dot film. The free radical initiator is utilized to destroy the mixed quantum dots through the free radicals formed by light irradiation decomposition, so that the light color conversion is realized through the destruction of single quantum dots, the stability difference of the quantum dots is realized by controlling the synthesis process of the quantum dots, the color of the photoluminescence film is quantitatively controlled, and the indirect quantitative light energy is realized. The light source irradiates the photoluminescence film under different intensities and different distances to realize slow color change of the photoluminescence film, thereby realizing quantitative control of illumination energy.

Description

Photoluminescent film, and preparation method and application thereof
Technical Field
The invention relates to the technical field of quantum dot luminescence, in particular to a photoluminescent film and a preparation method and application thereof.
Background
Quantum dots are semiconductor crystals composed of several atoms, which have excellent luminescence properties due to their quantum-local effect. In modern society, there are many occasions in which quantitative detection of light energy is required, such as sterilization and disinfection, especially in the places susceptible to infection, dense in people and high in requirements for working environment, such as hospitals and blood stations. Ultraviolet lamps are generally used in modern markets for disinfection and sterilization, however, human bodies or cells cannot be exposed to ultraviolet or strong light environments for a long time, how to quantify sterilization energy and reduce light energy received by the human bodies is important for people to pay attention to whether quantified visible light can be used for replacing the ultraviolet or strong light.
Disclosure of Invention
The invention mainly aims to provide a photoluminescent film, a preparation method and application thereof, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of a photoluminescence film, which comprises the following steps: at least more than one quantum dot, photoinitiator, light scattering particles and resin are mixed and cured under the condition of keeping out of the sun to prepare the photoluminescence film.
The embodiment of the invention also provides a photoluminescent film prepared by any one of the methods.
The embodiment of the invention also provides a preparation method of the quantitative photochromic test strip, which comprises the steps of irradiating the photoluminescent films by a light source under different intensities and/or different distances to slowly change colors of the photoluminescent films to obtain the quantitative photochromic test strip, wherein the photoluminescent films are the photoluminescent films.
The embodiment of the invention also provides a quantitative photochromic test strip which is prepared by the method.
The embodiment of the invention also provides the application of the photoluminescence film or the quantitative photochromic test strip in the quantitative indication of the illumination energy.
Compared with the prior art, the invention has the beneficial effects that:
the invention prepares the photoluminescence film by introducing the free radical initiator into the quantum dot film. The free radical initiator is utilized to destroy the mixed quantum dots through the free radicals formed by light irradiation decomposition, so that the light color conversion is realized through the destruction of single quantum dots, the stability difference of the quantum dots is realized by controlling the synthesis process of the quantum dots, the color of the photoluminescence film is quantitatively controlled, and the indirect quantitative sterilization effect is realized. The light source irradiates the photoluminescence film under different intensities and different distances to realize slow color change of the photoluminescence film, thereby realizing quantitative control of illumination energy.
In addition, the photoluminescence film or the quantitative photochromic test strip can also be used as a light energy indicator strip, and a standard color card is prepared according to different stability of quantum dots and lamp types and used for quantitatively judging the illumination energy, so that the illumination intensity and the illumination time can be monitored in a simplified manner.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1a is a color chart of a photoluminescent film before illumination by a light source according to an exemplary embodiment of the invention;
FIG. 1b is a color chart of a photoluminescent film after illumination by a light source according to an exemplary embodiment of the invention;
FIG. 2a is a spectrum of a photoluminescent film before illumination by a light source in an exemplary embodiment of the invention;
FIG. 2b is a spectrum of a photoluminescent film after illumination by a light source in an exemplary embodiment of the invention.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
The preparation method of the photoluminescence film provided by the embodiment of the invention comprises the following steps: at least more than one quantum dot, photoinitiator, light scattering particles and resin are mixed and cured under the condition of keeping out of the sun to prepare the photoluminescence film.
In some embodiments, the quantum dots include any one or a combination of two or more of group II-VI quantum dots, group III-V quantum dots, group IV-VI quantum dots, and perovskite quantum dots.
Further, the II-VI group quantum dots include one or a combination of two or more of CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdZnS, CdZnSe, CdZnTe, ZnSeTe, ZnTeS, CdSeS, CdSeTe, CdTeS, CdZnSeS, CdZnSeTe, CdZnSTe, CdSeSTe, ZnSeTe and CdZnSeTe.
Further, the III-V group quantum dots comprise any one or a combination of more than two of InP, InAs and InAsP.
Further, the IV-VI group quantum dots comprise any one or the combination of more than two of PbS, PbSe, PbTe, PbSeS, PbSeTe and PbSTe.
In some embodiments, the photoinitiator comprises any one or a combination of two or more of Benzoin (BE) or a derivative thereof, benzil or a derivative thereof, an α -hydroxyketone derivative, an α -aminoketone derivative, an acylphosphine oxide, and a titanocene.
Wherein, benzil or a derivative thereof is, for example, BDK; alpha-hydroxyketone derivatives of the type, for example, Darocur1173, Irgacure184, Irgacure 2959; alpha-aminoketone derivatives are, for example, Irgacure907, Irgacure 369; acylphosphine oxides of the type TEPO, Darocur TPO, Irgacure819, for example; titanocenes are for example 784.
In some embodiments, the resin comprises PMMA, PVDF, PU, or PET resin.
In some embodiments, the mass ratio of the quantum dots, photoinitiator, light scattering particles, and resin is from 2 to 5: 2-5: 5-10: 80-90.
In some embodiments, the light scattering particles comprise nano-SiO2TiO 2 nanoparticles2Nano ZrO 22Nano Al2O3Nano Fe3O4Nano ZnO2Nano AlN and nano Si3N4And any one or a combination of two or more of nano TiN.
In some embodiments, specifically including: mixing one or two kinds of quantum dots with different stable states, a photoinitiator, light scattering particles, resin and a solvent, mixing for 30min-1h at the rotating speed of 1000-2000rmp, removing part of the solvent in vacuum to obtain a glue solution, coating the glue solution in an inert gas atmosphere to form a uniform film with the thickness of 15-40 mu m, and then removing the residual solvent at the temperature of 500-2000pa and 25-50 ℃ to obtain the photoluminescent film.
In some embodiments, the photoluminescent film has a thickness of 10 to 30 μm.
Correspondingly, the embodiment of the invention also provides a photoluminescent film which is prepared by any one of the preparation methods.
The embodiment of the invention also provides a preparation method of the quantitative photochromic test strip, which comprises the following steps: and (2) irradiating the photoluminescence film by a light source under different intensities and/or different distances to slowly change the color of the photoluminescence film to obtain the quantitative photochromic test strip, wherein the photoluminescence film is the photoluminescence film.
Referring to fig. 1 a-1 b, the color change of the photoluminescent film of the present invention before and after light source irradiation is shown, and fig. 2 a-2 b are the spectrum change of the photoluminescent film of the present invention before and after light source irradiation. It can be seen that under the irradiation of the blue light source, the color of the photoluminescent film changes from yellow to red.
Correspondingly, the embodiment of the invention also provides a quantitative photochromic test strip which is prepared by the preparation method.
Correspondingly, the embodiment of the invention also provides the application of the photoluminescence film or the quantitative photochromic test strip in the quantitative indication of the illumination energy.
For example, a standard color rendering card is prepared according to the stability of quantum dots and different lamp types, and is used for quantitatively judging the illumination energy, so that the illumination intensity and the illumination time are monitored in a simplified mode.
The technical solution of the present invention will be described in further detail below with reference to examples. However, the examples are chosen only for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
Various reagents, such as quantum dots, used in the following examples of the present invention can be obtained from commercially available sources, or can be synthesized by reference to existing methods.
Example 1
Putting 4mmol of zinc acetate, 0.2mmol of cadmium oxide, 4ml of oleic acid and 15ml of octadecene into a 100ml three-neck flask, heating to 120 ℃, vacuumizing for 30min, and introducing argon; heating to 320 ℃, and injecting 1.5ml of 2M tri-n-octylphosphine selenium solution at 320 ℃ for 30 min; cooling to 300 ℃, dropwise adding 1ml of octyl mercaptan at 300 ℃, maintaining at 300 ℃ for 10min, cooling to room temperature, and finishing the reaction; purifying by using n-heptane and ethanol to obtain green light quantum dots (GQD) with the wavelength of 522nm, the half-peak width of 25nm and the light effect of 85%;
1mmol of Zn (OA)2、1.5mmol Cd(OA)2Vacuumizing 4ml of oleic acid and 15ml of octadecene at 90 ℃ to remove water and oxygen, heating the precursor to 300 ℃, quickly injecting 1.2ml of 2M TBP/Se when the temperature reaches 300 ℃, and preserving the temperature at 300 ℃ for 35-40 minutes; after the heat preservation time, the temperature is reduced to 260 ℃, 2ml of 1M TBP/S and 6.7ml of 0.3M Cd (OA) are dripped into the reaction system at a certain speed2Dripping off in 30 min; after dropping, the temperature is reduced to be below 100 ℃, and 6mmol Zn (OA) is added2Heating at 90 ℃ and simultaneously vacuumizing to remove water and remove oxygen for 1 h; after water removal and oxygen removal, the reaction system is quickly heated to 260 ℃ and is dripped12ml of 0.4M sulfur/oleylamine solution, and dripping off after 30 min; after the reaction is finished, purifying to obtain red light quantum dots (RQD) with the wavelength of 529nm, the half-peak width of 28nm and the light effect of 80%;
1 part of GQD, 0.3 part of RQD, 3 parts of TPO, 0.7 part of 819, and 5 parts of TiO2And 90 parts of modified PMMA, which is dissolved in dimethylbenzene and trimethylbenzene, mixed for 1h at the rotating speed of 1000rmp by a Cowles disperser, part of the solvent is removed in vacuum, the glue solution is coated on a glass or PET base film by a coater in the argon atmosphere to form a uniform film with the thickness of 15 mu m, and the residual solvent is slowly removed under the conditions of 1000Pa and 50 ℃ to obtain a yellow film visible to the naked eye, wherein the thickness of the film is 10 mu m. The film is placed under the conditions of 10w 365nm ultraviolet and 80w mercury lamp and irradiated at a position of 10cm for 18min, the color of the film is gradually changed from yellow to red, a spectrometer is used for detecting that a green light wave band is basically disappeared, and the film is irradiated at a position of 20cm for 42min, and the color of the film is gradually changed from yellow to red.
Example 2
Putting 200mg of lead bromide, 1.5ml of oleic acid, 3ml of oleylamine and 15ml of octadecene into a 100ml three-neck flask, heating to 120 ℃, and vacuumizing for 30 min; heating to 170 deg.C, injecting Cs (OA)2The solution is 0.55m, l5s and then cooled in an ice-water bath. Wherein Cs (OA)2The preparation method comprises the steps of putting CsCO33mmol, oleic acid 4ml and octadecene 4ml in a 100ml three-neck flask, heating to 100 ℃, vacuumizing for 30min to obtain colorless transparent liquid, and obtaining perovskite quantum dots (GQD) with the wavelength of 519nm and the half-peak width of 18 nm;
1mmol of Zn (OA)2、1mmol Cd(OA)23ml of oleic acid and 15ml of octadecene, and vacuumizing at 90 ℃ to remove water and oxygen; heating the precursor to 300 ℃, quickly injecting 1.3ml of 2M TBP/SeS (Se: S is 8:2) when the temperature reaches 300 ℃, and preserving the temperature at 300 ℃ for 30-35 minutes; after the heat preservation time, the temperature is reduced to 270 ℃, 6ml of 1M sulfur/oleylamine and 10ml of 0.3M Cd (OA) are dropwise added into the reaction system at a certain speed2And 15ml of 0.22M zinc stearate/octadecylene suspension, and dripping off for 30 min; after dropping, the temperature is reduced to be below 100 ℃, and 5mmol Zn (OA) is added2Heating at 90 ℃ and simultaneously vacuumizing to remove water and remove oxygen for 1 h; after water removal and oxygen removal, quickly heating the reaction system to 260 ℃, dropwise adding 13ml of 0.4M sulfur/oleylamine solution, and finishing dropping within 30 min; after the reaction, purification is carried out to obtain the wavelength of 622nm, Red Quantum Dots (RQD) with a half-peak width of 26 nm;
taking 4 parts of GQD, 1 part of RQD, 1 part of 819, 1 part of titanocene and 8 parts of Al2O3And 84 parts of modified PVDF, which is dissolved in dimethylbenzene and DMF, are mixed for 1 hour at the rotating speed of 2000rmp by a Cowles disperser, part of solvent is removed in vacuum, glue solution is coated on a glass or PET base film by a coating machine under the argon atmosphere to form a uniform film with the thickness of 40 mu m, and residual solvent is slowly removed under the conditions of 500pa and 25 ℃ to obtain a yellow film visible to naked eyes, wherein the thickness of the film is 30 mu m. And (3) placing the film under the conditions of 10w 440nm ultraviolet and 80w white light LED lamp for irradiating for 13min at a position of 10cm, gradually changing the color of the film from yellow to red, detecting that the green light wave band basically disappears by using a spectrometer, and irradiating for 24min at a position of 20cm, wherein the color of the film gradually changes from yellow to red.
Example 3
Taking in (Ac)3 0.5mmol、Zn(OA)2 1mmol、Zn(st)21mmol and ODE20ml, vacuum pumping at 120 ℃; adding 0.5ml PTMS at 200 ℃ for reaction for 10 min; heating to 220 ℃, and adding se-top 1mmol for reaction for 20 min; dropwise addition of Zn (ex)22mmol of the active carbon; heating to 280 ℃, adding DDT1ml and reacting for 30 min; cooling RT, finishing the reaction, and purifying to obtain green light quantum dots (GQD) with the wavelength of 522nm and the half-peak width of 53 nm;
taking in (Ac)3 0.5mmol、Zn(OA)2Vacuumizing 2mmol and ODE20ml at 120 ℃, adding 2.5ml PTMS at 200 ℃ for reaction for 10 min; heating to 220 ℃, adding se-top 1mmol, and reacting for 20 min; dropwise addition of Zn (ex)22mmol of the active carbon; heating to 280 ℃, adding 1ml of DDT, and reacting for 30 min; cooling RT, finishing the reaction, and purifying to obtain Red Quantum Dots (RQD) with the wavelength of 624nm and the half-peak width of 51 nm;
taking 3 parts of GQD, 2 parts of RQD, 1 part of 184, 2 parts of titanocene and 5 parts of SiO2And 87 parts of modified PU, which is dissolved in dimethylbenzene and DMF, mixed for 1 hour at the rotating speed of 1500rmp by a Cowles disperser, part of the solvent is removed in vacuum, the glue solution is coated on a glass or PET base film by a coater in the argon atmosphere to form a uniform film with the thickness of 30 μm, and the residual solvent is slowly removed under the conditions of 1000pa and 50 ℃ to obtain a yellow film visible to the naked eye, wherein the thickness of the film is 20 μm. Placed under a 10w 440nm ultraviolet and 80w white light LED lamp conditionIrradiating at 10cm for 11min to gradually change the color of the film from yellow to red, detecting the substantial disappearance of the green light wave band by a spectrometer, and irradiating at 20cm for 25min to gradually change the color of the film from yellow to red.
Example 4
Putting 200mg of lead bromide, 1.5ml of oleic acid, 3ml of oleylamine and 15ml of octadecene into a 100ml three-neck flask, heating to 120 ℃, and vacuumizing for 30 min; heating to 170 deg.C, injecting Cs (OA)2The solution is 0.55m, l5s and then cooled in an ice-water bath. Wherein Cs (OA)2The preparation method comprises the steps of putting CsCO33mmol, oleic acid 4ml and octadecene 4ml in a 100ml three-neck flask, heating to 100 ℃, vacuumizing for 30min to obtain colorless transparent liquid, and obtaining perovskite quantum dots (GQD) with the wavelength of 519nm and the half-peak width of 18 nm;
1mmol of Zn (OA)2、1.5mmol Cd(OA)2Vacuumizing 4ml of oleic acid and 15ml of octadecene at 90 ℃ to remove water and oxygen, heating the precursor to 300 ℃, quickly injecting 1.2ml of 2M TBP/Se when the temperature reaches 300 ℃, and preserving the temperature at 300 ℃ for 35-40 minutes; after the heat preservation time, the temperature is reduced to 260 ℃, 2ml of 1M TBP/S and 6.7ml of 0.3M Cd (OA) are dripped into the reaction system at a certain speed2Dripping off in 30 min; after dropping, the temperature is reduced to be below 100 ℃, and 6mmol Zn (OA) is added2Heating at 90 ℃ and simultaneously vacuumizing to remove water and remove oxygen for 1 h; after water and oxygen are removed, the reaction system is quickly heated to 260 ℃, 12ml of 0.4M sulfur/oleylamine solution is dripped, and dripping is finished within 30 min; after the reaction is finished, purifying to obtain red light quantum dots (RQD) with the wavelength of 529nm, the half-peak width of 28nm and the light effect of 80%;
taking 4.5 parts of GQD, 0.5 part of RQD, 3 parts of TPO, 2 parts of 819 and 10 parts of ZrO2And 80 parts of modified PMMA, which are dissolved in dimethylbenzene and trimethylbenzene, mixed for 30min at 2000rmp of rotation speed by a Cowles disperser, part of solvent is removed in vacuum, glue solution is coated on a glass or PET base film by a coater in the argon atmosphere to form a uniform film with the thickness of 30 mu m, and the residual solvent is slowly removed under the conditions of 1000Pa and 50 ℃ to obtain a yellow film visible to naked eyes, wherein the thickness of the film is 20 mu m. Irradiating with 10w 365nm ultraviolet lamp and 80w mercury lamp at 10cm for 12min to change the color of the film from yellow to red, detecting the disappearance of green light band by spectrometer, irradiating at 20cm for 36min to obtain the color of the filmThe color gradually changed from yellow to red.
Comparative example 1
This comparative example is substantially the same as example 1 except that a photoinitiator was not added, and a photoluminescent film was prepared. The photoluminescence film is placed under the conditions of 10w 365nm ultraviolet and 80w mercury lamp and is irradiated at a position of 10cm for 5 hours, the color of the film has no visible change, and no obvious difference exists in a spectrum test.
In addition, the inventors also conducted experiments with other materials and conditions, etc. listed in the present specification by way of the above examples, and quantum dots with high quantum yield can be similarly produced.
It should be understood that the above describes only some embodiments of the present invention and that various other changes and modifications may be affected therein by one of ordinary skill in the related art without departing from the scope or spirit of the invention.

Claims (11)

1. A method for preparing a photoluminescent film, comprising: mixing more than two kinds of quantum dots with different stable states with a photoinitiator, light scattering particles and resin, and curing under a dark condition to prepare a photoluminescent film;
the quantum dots are selected from II-VI group quantum dots, III-V group quantum dots, IV-VI group quantum dots or perovskite quantum dots;
the mass ratio of the quantum dots, the photoinitiator, the light scattering particles and the resin is (2-5): 2-5: 5-10: 80-90;
the photoinitiator is selected from any one or the combination of more than two of benzoin or derivatives thereof, benzil or derivatives thereof, alpha-hydroxy ketone derivatives, alpha-amino ketone derivatives, acyl phosphine oxides and titanocene;
the light scattering particles are selected from nano SiO2TiO 2 nanoparticles2Nano ZrO 22Nano Al2O3Nano Fe3O4Nano ZnO2Nano AlN and nano Si3N4And any one or a combination of two or more of nano TiN.
2. The method of claim 1, wherein: the II-VI group quantum dots include CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdZnS, CdZnSe, CdZnTe, ZnSeS, ZnSeTe, ZnTeS, CdSeS, CdSeTe, CdTeS, CdZnSeS, CdZnSeTe, CdZnSTe, CdSeSTe, ZnSeTe or CdZnSeTe.
3. The method of claim 1, wherein: the group III-V quantum dots comprise InP, InAs or InAsP.
4. The method of claim 1, wherein: the IV-VI group quantum dots comprise PbS, PbSe, PbTe, PbSeS, PbSeTe or PbSTe.
5. The method of claim 1, wherein: the resin comprises PMMA, PVDF, PU or PET resin.
6. The method according to claim 1, comprising: mixing two kinds of quantum dots with different stable states, a photoinitiator, light scattering particles, resin and a solvent, mixing for 30-60min at the rotation speed of 1000-2000rmp, removing part of the solvent in vacuum to obtain a glue solution, coating the glue solution in an inert gas atmosphere to form a uniform film with the thickness of 15-40 mu m, and removing the residual solvent at the temperature of 25-50 ℃ at the temperature of 500-2000pa to obtain the photoluminescent film.
7. The method of claim 1, wherein: the thickness of the photoluminescence film is 10-30 mu m.
8. A photoluminescent film prepared by the method of any one of claims 1 to 7.
9. A method of preparing a quantitative photochromic test strip, comprising: and (3) irradiating the photoluminescence film by a light source under different intensities and/or different distances to slowly change the color of the photoluminescence film to obtain the quantitative photochromic test strip, wherein the photoluminescence film is the photoluminescence film as claimed in claim 8.
10. A quantitative photochromic test strip made by the method of claim 9.
11. Use of the photoluminescent film of claim 8 or the quantitative photochromic test strip of claim 10 for quantitative indication of illumination energy.
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