CN110729419A - Method for packaging perovskite material by using TPU at room temperature and application thereof - Google Patents

Method for packaging perovskite material by using TPU at room temperature and application thereof Download PDF

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Publication number
CN110729419A
CN110729419A CN201910979033.8A CN201910979033A CN110729419A CN 110729419 A CN110729419 A CN 110729419A CN 201910979033 A CN201910979033 A CN 201910979033A CN 110729419 A CN110729419 A CN 110729419A
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Prior art keywords
perovskite
tpu
room temperature
polymer
magnetic stirring
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CN201910979033.8A
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Inventor
葛万银
施金豆
高文兴
徐美美
张塨凡
常哲
焦思怡
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/50Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for light emission, e.g. organic light emitting diodes [OLED] or polymer light emitting devices [PLED]
    • H01L51/52Details of devices
    • H01L51/5237Passivation; Containers; Encapsulation, e.g. against humidity
    • H01L51/524Sealing arrangements having a self-supporting structure, e.g. containers
    • H01L51/5246Sealing arrangements having a self-supporting structure, e.g. containers characterised by the peripheral sealing arrangements, e.g. adhesives, sealants
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/0001Processes specially adapted for the manufacture or treatment of devices or of parts thereof
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/42Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for sensing infra-red radiation, light, electro-magnetic radiation of shorter wavelength or corpuscular radiation and adapted for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation using organic materials as the active part, or using a combination of organic materials with other material as the active part; Multistep processes for their manufacture
    • H01L51/44Details of devices
    • H01L51/448Passivation, containers, encapsulations
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/50Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for light emission, e.g. organic light emitting diodes [OLED] or polymer light emitting devices [PLED]
    • H01L51/56Processes or apparatus specially adapted for the manufacture or treatment of such devices or of parts thereof
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/549Organic PV cells

Abstract

The invention discloses a method for encapsulating perovskite material by using TPU at room temperature and application thereof. The invention adopts TPU as perovskite packaging material, the TPU has reproducibility and environmental protection, does not influence reaction and is harmless to human body, and the perovskite/TPU composite material can be directly placed in the air for long-term storage without involving any other protection measures and has no pollution to the environment.

Description

Method for packaging perovskite material by using TPU at room temperature and application thereof
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a method for packaging a perovskite material by using TPU at room temperature and application thereof.
Background
Halogenated perovskites have received considerable attention for their unique optical and electronic properties for potential use in solar cells, Light Emitting Diodes (LEDs), photodetectors and lasers. In recent years, colloidal CsPbX3(X ═ Br, I, Cl) perovskite Nanocrystals (NCs) and hybrid perovskite MAPbX3(X ═ Br, I, Cl) is a spongish material of interest due to its high photoluminescence quantum yield (PLQY), tunable emission wavelength and narrow emission bandwidth.
However, CsPbX3The stability problems of perovskite materials such as (X ═ Br, I, Cl) NCs severely hinder their application, mainly due to thermal degradation and atmospheric humidity. To address this problem, various encapsulation strategies have been proposed to protect the perovskite NCs from decomposition in practical applications. Efficient encapsulation may improve its resistance to temperature and humidity by introducing additional matrix to form a barrier between the perovskite material and atmospheric humidity.
The thermal degradation effect of perovskite materials is a major bottleneck, which severely hampers their development, especially in regions with high annual average temperatures. Therefore, various encapsulating materials have been studied in recent years to reduce the influence of thermal degradation. Among them, the main common materials include oxides, inorganic salts, organic polymers, inorganic polymers (PMMA/PC/PS, etc.) and Metal Organic Frameworks (MOFs). For example, in the completion of SiO2For MAPbBr3After the encapsulation of Quantum Dots (QDs), the thermal degradation of the material in air is significantly reduced. CsPbX after encapsulation with borosilicate glass3(X ═ Br, I) QDs exhibit excellent thermal cycling at high temperatures. Encapsulation of CsPbBr Using Polydimethylsiloxane (PDMS)3Quantum dots, which have been found to be effective in increasing the thermal stability of the material. Therefore, it is necessary to research new encapsulation materials for perovskite protection.
The currently used packaging materials all have certain limitations. For example, PMMA is transparent, but is too brittle to be used in flexible applications. Although there is a concern about encapsulating hybrid calcium using TPUTitanium ore MAPbX3However, the encapsulation process was above room temperature, for MAPbX during encapsulation3Some degradation has already occurred. Therefore, the development of the room-temperature packaging process has important application value.
In terms of material selection, the TPU is used for packaging and protecting the perovskite material, and the method is simpler, more efficient, safe and harmless. In addition, the encapsulated perovskite/TPU polymer has high elasticity, and the photoluminescence characteristic shows extremely high stability under the conditions of high temperature and high humidity.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for encapsulating a perovskite material by using TPU at room temperature and application thereof, and the method can grow a high-elasticity perovskite/TPU compound and has the advantages of thermal degradation resistance, water vapor resistance, high transparency, high tensile rate and the like.
The invention adopts the following technical scheme:
a method for encapsulating perovskite material by using TPU at room temperature is characterized in that tetrahydrofuran is added into thermoplastic polyurethane elastomer rubber at room temperature, stirred and dissolved to obtain fluid TPU high polymer, and then perovskite material is added, and the perovskite/TPU polymer is obtained after natural cooling.
Specifically, the method comprises the following steps:
s1, mixing the thermoplastic polyurethane elastomer rubber with the tetrahydrofuran solution, and then performing magnetic stirring at room temperature until the thermoplastic polyurethane elastomer rubber is completely dissolved to obtain a fluid TPU high polymer;
s2, adding a perovskite material into the fluid TPU high polymer obtained in the step S1, and then continuing to perform magnetic stirring at room temperature to obtain a fluid perovskite/TPU polymer;
s3, introducing the fluid perovskite/TPU polymer prepared in the step S2 into a mould, and naturally solidifying at room temperature to obtain the perovskite/TPU polymer.
Further, in step S1, the mass ratio of the thermoplastic polyurethane elastomer rubber to the tetrahydrofuran is 1 g: (1-20) mL.
Further, in step S1, the magnetic stirring time is 1-3 h.
Further, in step S2, the mass ratio of the thermoplastic polyurethane elastomer rubber to the perovskite material is 1 g: (1-1000) mg.
Further, the perovskite material comprises CsPbX3(X ═ Br, I, Cl) or hybrid perovskite MAPbX3(X=Br,I,Cl)。
Further, in step S2, the magnetic stirring time is 1-5 h.
Specifically, the perovskite/TPU polymer has a stretch ratio of 10 times or more its initial length.
The invention also provides an application of the prepared perovskite/TPU polymer in high-permeability and flexible packaging materials.
Compared with the prior art, the invention has at least the following beneficial effects:
the method is simpler, more efficient, safer and harmless by adopting the TPU as the packaging material to package and protect the perovskite material under the room temperature condition, and the packaged composite material has high elasticity and shows photoluminescence stability in water and at high temperature.
Furthermore, the perovskite/TPU composite material can be synthesized by simple dissolving and stirring processes at room temperature. The invention has the great advantages that the high-temperature condition and the use of complicated equipment are avoided, the whole process only needs to be carried out by magnetic stirring at room temperature, the time is relatively short, the high operation accessibility is provided, and the working cost is saved.
Further, the TPU encapsulating material was dissolved at room temperature using magnetic stirring. The high energy consumption of traditional high temperature dissolution has been avoided in such setting to magnetic stirring is safer, convenient relatively speaking operation, more is applicable to the industrialization large-scale production.
Further, a perovskite material is used as the encapsulated material. Perovskite materials have been considered as potential replacements for next generation optical devices due to their unique optical properties and high quantum yields. Therefore, solving the stability problem through encapsulation will expand the way for its commercial application.
Further, the perovskite was mixed with TPU using magnetic stirring at room temperature. The setting can avoid the agglomeration phenomenon of the perovskite/TPU polymer through the rotation speed adjustment, and simultaneously, the two materials are more fully mixed, so that the energy consumption is reduced.
Further, the perovskite was mixed with TPU using magnetic stirring at room temperature. The setting can avoid the agglomeration phenomenon of the perovskite/TPU polymer through the rotation speed adjustment, and simultaneously, the two materials are more fully mixed, so that the energy consumption is reduced.
Further, perovskite/TPU polymer properties. The encapsulated perovskite/TPU polymer has good heat resistance and water resistance. In addition, the polymer also exhibits high elasticity, and the elongation is 10 times or more the original length thereof.
In conclusion, the TPU is adopted as the perovskite packaging material, the TPU has the advantages of reproducibility and environmental protection, no influence on reaction and no harm to human bodies, and the perovskite/TPU composite material can be directly placed in the air for long-term storage without any other protection measures and has no pollution to the environment.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is an XRD spectrum of example 1;
FIG. 2 is a TEM photograph of example 1;
FIG. 3 is a photograph of the product of example 1 in sunlight and under a 365nm UV lamp;
FIG. 4 is a photoluminescence spectrum of example 1;
FIG. 5 is an XRD spectrum of example 2;
FIG. 6 is a TEM photograph of example 2;
FIG. 7 is a photograph of the product of example 2 in sunlight and under a 365nm UV lamp;
FIG. 8 is a photoluminescence spectrum of example 2;
FIG. 9 is a graph of the elongation of example 3;
FIG. 10 shows the stability of luminescence in water of example 4.
Detailed Description
The invention provides a method for encapsulating a perovskite material by using TPU at room temperature and application thereof. The invention has the great advantages that the high-temperature condition and the use of complicated equipment are avoided, the whole process only needs to be carried out by magnetic stirring at room temperature, the time is relatively short, the high operation accessibility is provided, and the working cost is saved. In addition, the thermoplastic polyurethane elastomer rubber (TPU) has the advantages of reproducibility and environmental protection, no influence on reaction and no harm to human bodies.
The invention discloses a method for packaging a perovskite material by using TPU (thermoplastic polyurethane) at room temperature, which comprises the following steps of:
s1, mixing the TPU with the tetrahydrofuran solution, and then carrying out magnetic stirring at room temperature until the TPU is completely dissolved to obtain a fluid TPU high polymer;
wherein the mass ratio of TPU to tetrahydrofuran is 1 g: (1-20) mL; the magnetic stirring time is 1-3 h.
S2, adding a perovskite material into the fluid TPU high polymer obtained in the step S1, and then continuing to perform magnetic stirring at room temperature to obtain a fluid perovskite/TPU polymer;
the ratio of TPU to perovskite material is 1 g: 1-1000 mg, and the magnetic stirring time is 1-5 h.
The perovskite material comprises CsPbX3(X ═ Br, I, Cl) or hybrid perovskite MAPbX3(X=Br,I,Cl)。
S3, introducing the fluid perovskite/TPU polymer prepared in the step S2 into a mould, and naturally solidifying at room temperature to obtain the perovskite/TPU polymer with high elasticity and high permeability.
After the perovskite/TPU polymer is packaged, perovskite powder materials can be directly seen, so that absorption of the perovskite materials to external radiation energy and emission of visible light of the perovskite materials in a photoluminescence process are guaranteed.
The elongation of the perovskite/TPU polymer is more than 10 times of the initial length of the perovskite/TPU polymer, the problem of water vapor decomposition of the perovskite material can be avoided, and the perovskite/TPU polymer can be used in occasions of high permeability and flexible use.
Under the effective protection of the perovskite/TPU polymer, the luminescent property of the perovskite material has long-term stability in water or at high temperature, so that the perovskite material can be used for a long time in an extreme environment, can bear the temperature of 0-100 ℃, and can be used for a long time in the environment exceeding room temperature and the like.
The encapsulated perovskite/TPU polymer has great commercial application prospect, and the high heat resistance can enable the perovskite/TPU polymer to be applied to the field of temperature sensing devices. In addition, the perovskite/TPU polymer also shows high elasticity, which lays a certain foundation for future flexible wearing fluorescent materials.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
First, in a 50mL beaker, a mixture of 1g of TPU and 10mL of tetrahydrofuran was added and placed on a magnetic stirring device and stirred at room temperature for 2h until all TPU was completely dissolved. Then, 1mg of perovskite CsPbBr was added3Placing the QDs material in dissolved TPU, stirring at room temperature for 2h, pouring into a prepared mold to obtain the product with high elasticity and high permeabilityThe perovskite/TPU composite of (a).
FIG. 1 shows CsPbBr added according to example 13The X-ray diffraction spectrum of the nano crystal has no impurity peak, and the product is pure CsPbBr3
FIG. 2 shows the addition of single crystal CsPbBr according to example 13TEM photograph of the nanocrystals, it can be seen that CsPbBr3Is in the shape of a cubic block.
Fig. 3 is a photograph of the perovskite/TPU composite synthesized according to example 1 in sunlight and under a 365nm ultraviolet lamp, showing good green light emission from the perovskite/TPU composite under the ultraviolet lamp, indicating that encapsulation of the TPU does not hinder the absorption of the ultraviolet radiation energy and visible light emission process by the perovskite material.
FIG. 4 is a spectrum diagram of the perovskite/TPU composite synthesized according to example 1 under the excitation of a 365nm ultraviolet lamp, the test wavelength range is 200-900 nm, the integration time is 100ms, and it can be seen from the spectrum that the perovskite/TPU composite does not have other additional emission peaks, which indicates that the TPU is a high-transmittance polymer, and this ensures the fluorescence purity of the encapsulated material.
Example 2
In a 50mL beaker, a mixture of 1g of TPU and 20mL of tetrahydrofuran was added and placed on a magnetic stirring apparatus and stirred at room temperature for 3h until all TPU was completely dissolved. Then, 1000mg of perovskite Cs was added4PbBr6Putting the QDs material into the dissolved TPU, stirring for 3h at room temperature, and pouring into a prepared mould to obtain the perovskite/TPU composite material with high elasticity and high permeability.
FIG. 5 shows the addition of single-crystal Cs according to example 24PbBr6The X-ray diffraction spectrum of the nano crystal does not have impurity peaks, and the product is pure Cs4PbBr6
FIG. 6 shows the addition of single-crystal Cs according to example 24PbBr6TEM photograph of the nanocrystal, it can be seen that Cs4PbBr6Is in the shape of an inclined rhombus square column.
FIG. 7 is a photograph of the perovskite/TPU composite synthesized according to example 2 in sunlight and under a 365nm ultraviolet lamp, the perovskite/TPU composite emitting green fluorescence under the ultraviolet lamp, which indicates that the photoluminescence process of the TPU encapsulated perovskite material is not affected.
Fig. 8 is a spectrogram of the perovskite/TPU composite synthesized in example 2 under the excitation of a 365nm ultraviolet lamp, the test wavelength range is 200-900 nm, the integration time is 200ms, and the emission peak of the perovskite/TPU composite is narrow as can be seen from the spectrum, which indicates that the intensity of the released fluorescence is high, which indicates that the TPU can effectively avoid the agglomeration effect of the perovskite material, thereby improving the quantum yield of the polymer.
Example 3
In a 50mL beaker, a mixture of 1g TPU and 15mL tetrahydrofuran was added and placed on a magnetic stirring apparatus and stirred at room temperature for 2.5h until all TPU was completely dissolved. Then, 500mg of perovskite CsPbBr was added3Putting the QDs material into the dissolved TPU, stirring for 1h at room temperature, and pouring into a prepared mould to obtain the perovskite/TPU composite material with high elasticity and high permeability.
FIG. 9 is a perovskite/TPU composite synthesized according to example 3, with a stretch ratio that can be more than 10 times the original length.
Example 4
In a 50mL beaker, a mixture of 1g of TPU and 5mL of tetrahydrofuran was added and placed on a magnetic stirring apparatus and stirred at room temperature for 1h until all TPU was completely dissolved. Then, 50mg of perovskite CsPbBr was added3Putting the QDs material into the dissolved TPU, stirring for 5h at room temperature, and pouring into a prepared mould to obtain the perovskite/TPU composite material with high elasticity and high permeability.
FIG. 10 shows the long-term stability (0-72 h) of the spectrum obtained by immersing the perovskite/TPU composite synthesized according to example 4 in water under the excitation of a 365nm ultraviolet lamp.
Example 5
In a 50mL beaker, a mixture of 1g TPU and 1mL tetrahydrofuran was added and placed on a magnetic stirring apparatus and stirred at room temperature for 1.5h untilUntil all TPU was completely dissolved. Then, 10mg of perovskite CsPbCl was added3Putting the QDs material into the dissolved TPU, stirring for 4h at room temperature, and pouring into a prepared mould to obtain the perovskite/TPU composite material with high elasticity and high permeability.
Example 6
In a 50mL beaker, a mixture of 1g TPU and 15mL tetrahydrofuran was added and placed on a magnetic stirring apparatus and stirred at room temperature for 2.5h until all TPU was completely dissolved. Then, 5mg of perovskite CsPbI was added3Putting the QDs material into the dissolved TPU, stirring for 1.5h at room temperature, and pouring into a prepared mould to obtain the perovskite/TPU composite material with high elasticity and high permeability.
The operational feasibility of the invention is demonstrated by a large number of examples, and is suitable for commercial mass production. From the result, the adaptability of the perovskite material to temperature, water vapor and some extreme conditions can be greatly improved by adopting TPU as the packaging protection material, and the packaged perovskite/TPU composite material is not influenced by TPU and still keeps good optical characteristics. The invention lays a foundation for the application and development of the next generation of optical devices.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (9)

1. A method for encapsulating a perovskite material by using TPU at room temperature is characterized in that tetrahydrofuran is added into thermoplastic polyurethane elastomer rubber under the condition of room temperature, stirred and dissolved to obtain a fluid TPU high polymer, and then the perovskite material is added to obtain the perovskite/TPU polymer after natural cooling.
2. The method of claim 1, comprising the steps of:
s1, mixing the thermoplastic polyurethane elastomer rubber with the tetrahydrofuran solution, and then performing magnetic stirring at room temperature until the thermoplastic polyurethane elastomer rubber is completely dissolved to obtain a fluid TPU high polymer;
s2, adding a perovskite material into the fluid TPU high polymer obtained in the step S1, and then continuing to perform magnetic stirring at room temperature to obtain a fluid perovskite/TPU polymer;
s3, introducing the fluid perovskite/TPU polymer prepared in the step S2 into a mould, and naturally solidifying at room temperature to obtain the perovskite/TPU polymer.
3. The method according to claim 2, wherein in step S1, the mass ratio of the thermoplastic polyurethane elastomer rubber to the tetrahydrofuran is 1 g: (1-20) mL.
4. The method of claim 2, wherein in step S1, the magnetic stirring time is 1-3 h.
5. The method according to claim 2, wherein in step S2, the mass ratio of the thermoplastic polyurethane elastomer rubber to the perovskite material is 1 g: (1-1000) mg.
6. The method of claim 5, wherein the perovskite material comprises CsPbX3(X ═ Br, I, Cl) or hybrid perovskite MAPbX3(X=Br,I,Cl)。
7. The method of claim 2, wherein in step S2, the magnetic stirring time is 1-5 h.
8. A process according to any of claims 1 to 7, characterised in that the perovskite/TPU polymer has a stretch of 10 times or more its initial length.
9. Use of the perovskite/TPU polymer prepared according to the method of claim 1 in high permeability and flexible packaging materials.
CN201910979033.8A 2019-10-15 2019-10-15 Method for packaging perovskite material by using TPU at room temperature and application thereof Pending CN110729419A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102336928A (en) * 2011-07-08 2012-02-01 北京理工大学 Flexible, environmentally-friendly, transparent and adjustable-illuminant-color film material and preparation method thereof
CN107611190A (en) * 2017-09-18 2018-01-19 南昌大学 A kind of perovskite solar cell resistant to bending and preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102336928A (en) * 2011-07-08 2012-02-01 北京理工大学 Flexible, environmentally-friendly, transparent and adjustable-illuminant-color film material and preparation method thereof
CN107611190A (en) * 2017-09-18 2018-01-19 南昌大学 A kind of perovskite solar cell resistant to bending and preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ENDER ERCAN, ET AL: "Stretchable and Ambient Stable Perovskite/Polymer Luminous Hybrid Nanofibers of Multicolor Fiber Mats and Their White LED Applications", 《ACS APPL. MATER. INTERFACES》 *

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