CN109054062A - Photoluminescence thin film and the preparation method and application thereof - Google Patents

Photoluminescence thin film and the preparation method and application thereof Download PDF

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Publication number
CN109054062A
CN109054062A CN201811179235.6A CN201811179235A CN109054062A CN 109054062 A CN109054062 A CN 109054062A CN 201811179235 A CN201811179235 A CN 201811179235A CN 109054062 A CN109054062 A CN 109054062A
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thin film
quantum dot
photoluminescence thin
light
photoluminescence
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CN109054062B (en
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张孟
周群刚
汪红
王明元
郑然�
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Suzhou central blood station
Jiaxing Nding Photoelectric Technology Co Ltd
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Suzhou central blood station
Jiaxing Nding Photoelectric Technology Co Ltd
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Abstract

The present invention discloses a kind of Photoluminescence thin film and the preparation method and application thereof, and the preparation method of Photoluminescence thin film includes: at least to make more than one quantum dots, photoinitiator, light diffusing particles and resin mixing, solidifies under the conditions of being protected from light, Photoluminescence thin film is made.Photoluminescence thin film is made by the way that radical initiator to be introduced into quantum dot film in the present invention.Mixing quantum dot is destroyed by the free radical that light irradiation is decomposed to form using radical initiator, so that wherein single quantum dot destroys to realize photochromic transformation, quantum dot stability difference is realized by control quantum dot synthesis technology to realize that quantification controls the color of Photoluminescence thin film, to realize indirect quantification light energy.Photoluminescence thin film is irradiated under varying strength, different distance by light source, realizes that Photoluminescence thin film slowly changes colour, to realize that quantification controls light energy.

Description

Photoluminescence thin film and the preparation method and application thereof
Technical field
The present invention relates to quantum dot light emitting technical fields, and in particular to a kind of Photoluminescence thin film and preparation method thereof with answer With.
Background technique
Quantum dot is, because it is with quantum local effect, to make its tool by the semiconductor crystal of the molecular one kind of several originals There are good luminescent properties.In modern society, having many occasions needs to use looks for energy to carry out quantitative detection light, such as goes out Bacterium disinfection, especially such as hospital, blood station easy infection, the crowd is dense and the higher place of operating environment requirements.Modern times are on the market Generally carried out disinfection sterilizing using ultraviolet lamp, however human body or cell can not be exposed to for a long time in ultraviolet or strong light environment, this When how quantitatively to sterilize energy, reduce human body and receive light energy, if can be replaced with the visible light of quantization, which becomes everybody, pays close attention to Emphasis.
Summary of the invention
The main purpose of the present invention is to provide a kind of Photoluminescence thin films and the preparation method and application thereof, existing to overcome Deficiency in technology.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the invention provides a kind of preparation methods of Photoluminescence thin film, comprising: at least makes more than one quantum Point, photoinitiator, light diffusing particles and resin mixing, solidify under the conditions of being protected from light, Photoluminescence thin film are made.
The embodiment of the present invention also provides a kind of Photoluminescence thin film, is prepared by above-mentioned any method.
The embodiment of the present invention also provides a kind of preparation method for quantifying photochromic calibration tape, including by light source different strong Photoluminescence thin film is irradiated under degree and/or different distance, the Photoluminescence thin film is made slowly to change colour, it is photochromic to obtain quantization Calibration tape, the Photoluminescence thin film are Photoluminescence thin film above-mentioned.
The embodiment of the present invention also provides a kind of photochromic calibration tape of quantization, is prepared by above-mentioned method.
The embodiment of the present invention also provides the Photoluminescence thin film or the photochromic calibration tape of the quantization in illumination The purposes of Energy Quantization instruction.
Compared with prior art, the beneficial effect comprise that
Photoluminescence thin film is made by the way that radical initiator to be introduced into quantum dot film in the present invention.Utilize free radical Initiator destroys mixing quantum dot by the free radical that light irradiation is decomposed to form, so that wherein single quantum dot destroys to realize Photochromic transformation realizes quantum dot stability difference by control quantum dot synthesis technology to realize that quantification controls photic hair The color of optical thin film, to realize indirect quantification sterilization effect.Photic hair is irradiated under varying strength, different distance by light source Optical thin film realizes that Photoluminescence thin film slowly changes colour, to realize that quantification controls light energy.
In addition, Photoluminescence thin film or the photochromic calibration tape of quantization can also indicate band as light energy, for quantum The stability difference of point and the classification of lamp prepare standard coloration card, for the quantization judgement to light energy, to realize brief Change monitoring intensity of illumination and light application time.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this The some embodiments recorded in invention, for those of ordinary skill in the art, without creative efforts, It is also possible to obtain other drawings based on these drawings.
Fig. 1 a is chromaticity diagram of the Photoluminescence thin film before light source irradiation in an exemplary embodiments of the invention；
Fig. 1 b is chromaticity diagram of the Photoluminescence thin film after light source irradiation in an exemplary embodiments of the invention；
Fig. 2 a is spectrogram of the Photoluminescence thin film before light source irradiation in an exemplary embodiments of the invention；
Fig. 2 b is spectrogram of the Photoluminescence thin film after light source irradiation in an exemplary embodiments of the invention.
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose of the invention Technical solution.The technical solution, its implementation process and principle etc. will be further explained as follows.
The preparation method of a kind of Photoluminescence thin film provided in an embodiment of the present invention, comprising: at least make more than one quantum Point, photoinitiator, light diffusing particles and resin mixing, solidify under the conditions of being protected from light, Photoluminescence thin film are made.
In some embodiments, the quantum dot includes II-VI group quantum dot, iii-v quantum dot, group IV-VI amount Any one in son point and perovskite quantum dot or two or more combinations.
Further, the II-VI group quantum dot include CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdZnS, CdZnSe、CdZnTe、ZnSeS、ZnSeTe、ZnTeS、CdSeS、CdSeTe、CdTeS、CdZnSeS、CdZnSeTe、CdZnSTe、 Any one in CdSeSTe, ZnSeSTe and CdZnSeSTe or two or more combinations.
Further, the iii-v quantum dot include in InP, InAs and InAsP any one or it is two or more Combination.
Further, the group IV-VI quantum dot includes appointing in PbS, PbSe, PbTe, PbSeS, PbSeTe and PbSTe Meaning a combination of one or more.
In some embodiments, the photoinitiator includes benzoin (BE) or derivatives thereof, benzil or its derivative Any one in object, alpha-alcohol ketone derivative, α-amido ketone derivatives, acylphosphine oxide and titanium cyclopentadienyl or two or more groups It closes.
Wherein, benzil or derivatives thereof is, for example, BDK；Its model of alpha-alcohol ketone derivative be, for example, Darocur1173, Irgacure184,Irgacure 2959；Its model of α-amido ketone derivatives is, for example, Irgacure907, Irgacure369； Its model of acylphosphine oxide is, for example, TEPO, Darocur TPO, Irgacure819；Its model of titanium cyclopentadienyl is, for example, 784.
In some embodiments, the resin includes PMMA, PVDF, PU or PET resin.
In some embodiments, the mass ratio of the quantum dot, photoinitiator, light diffusing particles and resin is 2-5:2- 5:5-10:80-90.
In some embodiments, the light diffusing particles include Nano-meter SiO_22, nano-TiO2, nanometer ZrO2, nanometer Al2O3, nanometer Fe3O4, nano-ZnO2, nano-aluminum nitride, nano Si3N4With any one or the two or more groups in nano TiN It closes.
In some embodiments, it specifically includes: dissipating quantum dot, photoinitiator, the light of one or two kinds of different stable states Radion, resin and solvent mixing, mix 30min-1h under 1000-2000rmp revolving speed, partial solvent are removed in vacuum, obtain Glue makes the glue be coated with the uniform film formed with a thickness of 15-40 μm under atmosphere of inert gases, later in 500- Residual solvent is removed at 2000pa, 25-50 DEG C, Photoluminescence thin film is made.
In some embodiments, the Photoluminescence thin film with a thickness of 10-30 μm.
Correspondingly, the embodiment of the present invention also provides a kind of Photoluminescence thin film, by above-mentioned any preparation method system It is standby to form.
The embodiment of the present invention also provides a kind of preparation method for quantifying photochromic calibration tape, comprising: by light source in difference Photoluminescence thin film is irradiated under intensity and/or different distance, the Photoluminescence thin film is made slowly to change colour, obtains quantization light-induced variable Color calibration tape, the Photoluminescence thin film are Photoluminescence thin film above-mentioned.
It is color change figure of the Photoluminescence thin film of the present invention before and after light source irradiation, Fig. 2 a- Fig. 2 b referring to Fig. 1 a- Fig. 1 b It is spectrum change figure of the Photoluminescence thin film of the present invention before and after light source irradiation.As it can be seen that under blue light source irradiation, luminescence generated by light The color of film becomes red from yellow.
Correspondingly, the embodiment of the present invention also provides a kind of photochromic calibration tape of quantization, by above-mentioned preparation method system It is standby to form.
Correspondingly, the embodiment of the present invention also provides the Photoluminescence thin film or the photochromic calibration tape of the quantization In the purposes of light energy quantization instruction.
For example, the different preparation standard coloration cards of stability and lamps and lanterns type for quantum dot, for light energy Quantization judgement, to realize simplification monitoring intensity of illumination and light application time.
The technical solution that present invention be described in more detail by the following examples.However, selected embodiment is only used for Illustrate the present invention, and does not limit the scope of the invention.
The classes of agents applied in following examples of the present invention, such as quantum dot can be obtained from commercially available approach, can also To be synthesized with reference to existing method.
Embodiment 1
It is placed in zinc acetate 4mmol, cadmium oxide 0.2mmol, oleic acid 4ml, octadecylene 15ml in 100ml three-neck flask, rises Temperature leads to argon gas after vacuumizing 30min to 120 DEG C；320 DEG C are warming up to, the tri-n-octyl phosphine selenium solution of 2M is injected in 320 DEG C 1.5ml maintains 30min；300 DEG C are cooled to, in 300 DEG C of dropwise addition spicy thioalcohol 1ml, is cooled to room temperature after 300 DEG C of maintenance 10min, Reaction terminates；Wavelength 522nm, half-peak breadth 25nm, the green light quantum point of light efficiency 85% are obtained using normal heptane and ethanol purification (GQD)；
By 1mmol Zn (OA)2、1.5mmol Cd(OA)2, 4ml oleic acid, 15ml octadecylene, vacuumize water removal in 90 degree and remove Presoma is warming up to 300 degree by oxygen, and fast injection enters 1.2ml 2M TBP/Se when temperature reaches 300 DEG C, keeps the temperature 35 in 300 DEG C ~40 minutes；After soaking time, 260 DEG C are cooled to, 2ml 1M TBP/S and 6.7ml is added dropwise to reaction system with certain speed The Cd (OA) of 0.3M2, 30min drips off；It drips off and is cooled to 100 DEG C hereinafter, 6mmol Zn (OA) is added2, 90 DEG C are heated while being taken out very Sky water removal deoxygenation 1h；Reaction system is rapidly heated to 260 DEG C after water removal deoxygenation, 12ml 0.4M sulphur/oleyl amine solution is added dropwise, 30min is dripped off；Reaction terminates, and purifying obtains wavelength 529nm, half-peak breadth 28nm, the red light quantum point (RQD) of light efficiency 80%；
Take 1 part of GQD, 0.3 part of RQD, 3 parts of TPO, 0.7 part 819,5 parts of TiO2And 90 parts of modified PMMAs, it is dissolved in dimethylbenzene In trimethylbenzene, 1h is mixed under 1000rmp revolving speed with Cowles disperser, partial solvent is removed in vacuum, by glue in argon gas The uniform film with a thickness of 15 μm is coated into coating machine under atmosphere on glass or PET basement membrane, under the conditions of 1000pa, 50 DEG C Slowly remove residual solvent, obtain the visible yellow light film of naked eyes, film with a thickness of 10 μm.It is placed in that 10w 365nm is ultraviolet and 80w 18min is irradiated under the conditions of mercury lamp at 10cm, film color gradually becomes red from yellow, detects green light band base with spectrometer This disappearance, irradiates 42min at 20cm, and film color gradually becomes red from yellow.
Embodiment 2
Lead bromide 200mg, oleic acid 1.5ml, oleyl amine 3ml, octadecylene 15ml are placed in 100ml three-neck flask, are warming up to 120 DEG C, vacuumize 30min；170 DEG C are warming up to, is injected Cs (OA)2Ice-water bath cools down after solution 0.55m, l5s.Wherein Cs (OA)2 Configuration method be that CsCO33mmol, oleic acid 4ml, octadecylene 4ml are placed in 100ml three-neck flask to be warming up to 100 DEG C, take out true Empty 30min obtains colourless transparent liquid, and obtaining wavelength is 519nm, and half-peak breadth is the perovskite quantum dot (GQD) of 18nm；
By 1mmol Zn (OA)2、1mmol Cd(OA)2, 3ml oleic acid, 15ml octadecylene, vacuumize water removal deoxygenation in 90 degree； Presoma is warming up to 300 DEG C, fast injection enters the TBP/SeS (Se:S=8:2) of 1.3ml 2M when temperature reaches 300 DEG C, in 300 DEG C keep the temperature 30~35 minutes；After soaking time, 270 degree are cooled to, 6ml 1M is added dropwise to reaction system with certain speed Sulphur/oleyl amine and 10ml 0.3M Cd (OA)2And 15ml 0.22M zinc stearate/octadecylene suspension, 30min are dripped off；It drips off 100 DEG C are cooled to hereinafter, 5mmol Zn (OA) is added2, 90 DEG C are heated while being vacuumized water removal deoxygenation 1h；It will be anti-after water removal deoxygenation It answers system to be rapidly heated to 260 degree, 13ml 0.4M sulphur/oleyl amine solution is added dropwise, 30min is dripped off；Reaction terminates, and purifying obtains wave The red light quantum point (RQD) of a length of 622nm, half-peak breadth 26nm；
Take 4 parts of GQD, 1 part of RQD, 1 part 819,1 part of titanium cyclopentadienyl, 8 parts of Al2O3And 84 parts of modified PVDF, be dissolved in dimethylbenzene and In DMF, 1h is mixed under 2000rmp revolving speed with Cowles disperser, partial solvent is removed in vacuum, by glue under argon atmosphere The uniform film with a thickness of 40 μm is coated on glass or PET basement membrane with coating machine, is slowly removed under the conditions of 500pa, 25 DEG C Remove residual solvent, obtain the visible yellow light film of naked eyes, film with a thickness of 30 μm.It is placed in that 10w 440nm is ultraviolet and 80w white light 13min is irradiated under the conditions of LED light at 10cm, film color gradually becomes red from yellow, detects green light band with spectrometer It is basic to disappear, 24min is irradiated at 20cm, film color gradually becomes red from yellow.
Embodiment 3
Take In (Ac)3 0.5mmol、Zn(OA)2 1mmol、Zn(st)21mmol and ODE20ml is vacuumized at 120 DEG C； 200 DEG C of addition 0.5ml PTMS react 10min；220 DEG C are warming up to, se-top 1mmol is added and reacts 20min；Zn is added dropwise (ex)22mmol；280 DEG C are warming up to, DDT1ml is added and reacts 30min；Cool down RT, and reaction terminates, and purifies, obtaining wavelength is The green light quantum point (GQD) of 522nm, half-peak breadth 53nm；
Take In (Ac)3 0.5mmol、Zn(OA)22mmol and ODE 20ml is vacuumized at 120 DEG C, is added in 200 DEG C 2.5ml PTMS reacts 10min；It is warming up to 220 DEG C of addition se-top 1mmol reaction 20min；It is added dropwise Zn (ex)22mmol；It rises Temperature is added DDT 1ml and reacts 30min to 280 DEG C；Cool down RT, and reaction terminates, and purifies, and obtaining wavelength is 624nm, half-peak breadth The red quantum dot (RQD) of 51nm；
Take 3 parts of GQD, 2 parts of RQD, 1 part 184,2 parts of titanium cyclopentadienyls, 5 parts of SiO2And 87 parts of modified PU, it is dissolved in dimethylbenzene and DMF In, 1h is mixed under 1500rmp revolving speed with Cowles disperser, partial solvent is removed in vacuum, glue is used under argon atmosphere The uniform film that coating machine is coated into a thickness of 30 μm on glass or PET basement membrane slowly removes under the conditions of 1000pa, 50 DEG C Residual solvent, obtains the visible yellow light film of naked eyes, film with a thickness of 20 μm.It is placed in that 10w 440nm is ultraviolet and 80w white light LEDs 11min is irradiated under the conditions of lamp at 10cm, film color gradually becomes red from yellow, basic with spectrometer detection green light band It disappears, 25min is irradiated at 20cm, film color gradually becomes red from yellow.
Embodiment 4
Lead bromide 200mg, oleic acid 1.5ml, oleyl amine 3ml, octadecylene 15ml are placed in 100ml three-neck flask, are warming up to 120 DEG C, vacuumize 30min；170 DEG C are warming up to, is injected Cs (OA)2Ice-water bath cools down after solution 0.55m, l5s.Wherein Cs (OA)2 Configuration method be that CsCO33mmol, oleic acid 4ml, octadecylene 4ml are placed in 100ml three-neck flask to be warming up to 100 DEG C, take out true Empty 30min obtains colourless transparent liquid, and obtaining wavelength is 519nm, and half-peak breadth is the perovskite quantum dot (GQD) of 18nm；
By 1mmol Zn (OA)2、1.5mmol Cd(OA)2, 4ml oleic acid, 15ml octadecylene, vacuumize water removal in 90 degree and remove Presoma is warming up to 300 degree by oxygen, and fast injection enters 1.2ml 2M TBP/Se when temperature reaches 300 DEG C, keeps the temperature 35 in 300 DEG C ~40 minutes；After soaking time, be cooled to 260 DEG C, with certain speed to reaction system be added dropwise 2ml 1M TBP/S and The Cd (OA) of 6.7ml0.3M2, 30min drips off；It drips off and is cooled to 100 DEG C hereinafter, 6mmol Zn (OA) is added2, 90 DEG C of heating are together When vacuumize water removal deoxygenation 1h；Reaction system is rapidly heated to 260 DEG C after water removal deoxygenation, it is molten that 12ml 0.4M sulphur/oleyl amine is added dropwise Liquid, 30min are dripped off；Reaction terminates, and purifying obtains wavelength 529nm, half-peak breadth 28nm, the red light quantum point of light efficiency 80% (RQD)；
Take 4.5 parts of GQD, 0.5 part of RQD, 3 parts of TPO, 2 part 819,10 parts of ZrO2And 80 parts of modified PMMAs, it is dissolved in dimethylbenzene In trimethylbenzene, 30min is mixed under 2000rmp revolving speed with Cowles disperser, partial solvent is removed in vacuum, by glue in argon Atmosphere encloses the lower uniform film being coated on glass or PET basement membrane with coating machine with a thickness of 30 μm, in 1000pa, 50 DEG C of conditions It is lower slowly to remove residual solvent, obtain the visible yellow light film of naked eyes, film with a thickness of 20 μm.Be placed in 10w 365nm it is ultraviolet and 12min is irradiated under the conditions of 80w mercury lamp at 10cm, film color gradually becomes red from yellow, detects green light wave with spectrometer Duan Jiben disappears, and 36min is irradiated at 20cm, and film color gradually becomes red from yellow.
Reference examples 1
The reference examples are substantially the same manner as Example 1, and difference is that photoinitiator is not added, and Photoluminescence thin film is made.It will The Photoluminescence thin film is placed under the conditions of 10w 365nm is ultraviolet and 80w mercury lamp irradiates 5h 10cm at, and film color is without visually can See variation, spectrum test is also without significant difference.
In addition, inventor also refers to the mode of above embodiments, with the other raw materials and item listed in this specification Part etc. is tested, and the quantum dot of high quantum production rate can equally be made.
It should be appreciated that above-described is only some embodiments of the present invention, it is noted that for the common of this field For technical staff, under the premise of not departing from concept of the invention, other modification and improvement can also be made, these are all It belongs to the scope of protection of the present invention.

Claims (10)

1. a kind of preparation method of Photoluminescence thin film, characterized by comprising: at least make more than one quantum dots, light-initiated Agent, light diffusing particles and resin mixing, solidify under the conditions of being protected from light, Photoluminescence thin film are made.
2. preparation method according to claim 1, it is characterised in that: the quantum dot include II-VI group quantum dot, Any one in iii-v quantum dot, group IV-VI quantum dot and perovskite quantum dot or two or more combinations；Preferably, The II-VI group quantum dot include CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdZnS, CdZnSe, CdZnTe, ZnSeS, ZnSeTe, ZnTeS, CdSeS, CdSeTe, CdTeS, CdZnSeS, CdZnSeTe, CdZnSTe, CdSeSTe, ZnSeSTe and Any one in CdZnSeSTe or two or more combinations；Preferably, the iii-v quantum dot include InP, InAs and Any one in InAsP or two or more combinations；Preferably, the group IV-VI quantum dot include PbS, PbSe, PbTe, Any one in PbSeS, PbSeTe and PbSTe or two or more combinations.
3. preparation method according to claim 1, it is characterised in that: the photoinitiator includes benzoin or its derivative It is any in object, benzil or derivatives thereof, alpha-alcohol ketone derivative, α-amido ketone derivatives, acylphosphine oxide and titanium cyclopentadienyl A combination of one or more；And/or the resin includes PMMA, PVDF, PU or PET resin.
4. preparation method according to claim 1, it is characterised in that: the quantum dot, photoinitiator, light diffusing particles Mass ratio with resin is 2-5:2-5:5-10:80-90.
5. preparation method according to claim 1, it is characterised in that: the light diffusing particles include Nano-meter SiO_22, nanometer TiO2, nanometer ZrO2, nanometer Al2O3, nanometer Fe3O4, nano-ZnO2, nano-aluminum nitride, nano Si3N4With it is any one in nano TiN Kind or two or more combinations.
6. preparation method according to claim 1, it is characterised in that specifically include: making one or two kinds of different stable states Quantum dot, photoinitiator, light diffusing particles, resin and solvent mixing, mix 30-60min, very under 1000-2000rmp revolving speed Sky removes partial solvent, obtains glue, so that the glue be coated with formation under atmosphere of inert gases uniform with a thickness of 15-40 μm Film removes residual solvent at 500-2000pa, 25-50 DEG C later, and Photoluminescence thin film is made；And/or the photic hair Optical thin film with a thickness of 10-30 μm.
7. the Photoluminescence thin film prepared by method according to any one of claims 1 to 6.
8. a kind of preparation method for quantifying photochromic calibration tape, characterized by comprising: by light source in varying strength and/or not Photoluminescence thin film is irradiated under same distance, the Photoluminescence thin film is made slowly to change colour, obtains and quantifies photochromic calibration tape, institute Stating Photoluminescence thin film is Photoluminescence thin film as claimed in claim 7.
9. by the photochromic calibration tape of quantization prepared by method according to any one of claims 8.
10. Photoluminescence thin film as claimed in claim 7 or the photochromic calibration tape of quantization as claimed in claim 9 are in illumination energy The purposes of amount quantization instruction.
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CN106967417A (en) * 2017-03-28 2017-07-21 华东师范大学 A kind of luminescence generated by light composite and its preparation method and application
CN107089039A (en) * 2017-04-24 2017-08-25 宁波东旭成新材料科技有限公司 A kind of multi-functional quantum dot film and preparation method thereof
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US20150177230A1 (en) * 2013-06-12 2015-06-25 The Mitre Corporation Quantum dot - polymer nanocomposite for optical sensing
CN106188398A (en) * 2014-12-08 2016-12-07 Lg电子株式会社 Quantum dots-polymer complex and preparation method thereof, there is the light conversion film of this complex, back light unit and display device
CN106967417A (en) * 2017-03-28 2017-07-21 华东师范大学 A kind of luminescence generated by light composite and its preparation method and application
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