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CN104934503A - Preparation method of perovskite solar cell light absorption layer material methylamine lead dibromide - Google Patents

Preparation method of perovskite solar cell light absorption layer material methylamine lead dibromide Download PDF

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Publication number
CN104934503A
CN104934503A CN201510330755.2A CN201510330755A CN104934503A CN 104934503 A CN104934503 A CN 104934503A CN 201510330755 A CN201510330755 A CN 201510330755A CN 104934503 A CN104934503 A CN 104934503A
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preparation
reaction solution
spin coating
solar cell
electromagnetic field
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CN104934503B (en
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唐立丹
梅海林
王冰
彭淑静
齐锦刚
王建中
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Liaoning University of Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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  • Condensed Matter Physics & Semiconductors (AREA)
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Abstract

The invention relates to a preparation method of a perovskite solar cell light absorption layer material methylamine lead dibromide. The preparation method comprises the following steps: mixing solid methyl ammonium bromide and solid lead dibromide, adding the mixture into a N,N-dimethyl formamide solvent, stirring uniformly to obtain a reaction solution, pouring the reaction solution in a container, applying a pulse electromagnetic field to treat the reaction solution, dropwise adding the treated reaction solution on a clean conducting glass substrate, performing low-speed spin coating and high-speed spin coating respectively to form a perovskite film with the thickness of 500-800 nm, then putting the perovskite film in a vacuum drying oven, and performing annealing treatment to obtain a methylamine lead dibromide film. The preparation method has the advantages that the preparation technology is simple, the preparation cost is low, the degree of crystallinity of the product can be improved by adopting the treatment of the pulse electromagnetic field, and the heat preservation time of annealing treatment is greatly shortened and is only 1/6 of that when the treatment of the pulse electromagnetic field is unadopted, so that the production cycle of the product is shortened, the energy resources are saved, and the preparation method is beneficial for industrial production.

Description

A kind of preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide
Technical field
The invention belongs to solar cell material preparation field, relate to a kind of preparation method of high-crystallinity perovskite solar battery obsorbing layer material methyl amine lead bromide, particularly relate to a kind of pulse electromagnetic field assisted solution legal system that adopts for the method for high-crystallinity perovskite solar battery obsorbing layer material methyl amine lead bromide.
Background technology
Along with lack of energy and ecological deterioration, people are badly in need of the new cleaning fuel finding a kind of alternative traditional fossil energy, solar energy has sustainability and the advantage such as pollution-free, be the important component part of countries in the world sustainable development source strategy, solar cell is the Main Means utilizing solar energy at present.Current solar cell is main mainly with the monocrystalline silicon of the second generation or polysilicon solar cell, and this battery exists that the production cycle is long, cost is high, there is the problems such as the higher and environmental pollution of energy consumption in crystal silicon preparation process simultaneously.Perovskite solar cell is a kind of novel solar cell, this battery principle is different from traditional crystal silicon based on pn knot and hull cell, there is the advantages such as high efficiency, low cost, simple preparation, the continuous fast lifting of its battery efficiency simultaneously, be 3.8% battery efficiency being promoted to perovskite solar cell in 2015 by the battery efficiency of perovskite solar cell in 2009 be 20.2%, perovskite solar cell is the extremely potential novel solar battery of one.
Organic inorganic hybridization perovskite material is the important component part of perovskite solar cell, serves as the light absorbing zone part of battery, has bipolarity (electronics and hole) transfer function.The light absorbing zone of perovskite solar cell adopts the methyl amine lead iodide (CH of the perovskite structure with ABX3 usually 3nH 3pbI 3) or methyl amine lead bromide (CH 3nH 3pbBr 3), its wide material sources, low in raw material price also can prepare flexible battery.At present, the method preparing perovskite material mainly contains solwution method and coevaporation method, but single solwution method is difficult to the perovskite absorbed layer obtaining high-crystallinity, though coevaporation method can obtain the perovskite absorbed layer of high-crystallinity, but preparation cost valency is higher, above problem causes perovskite battery and cannot large-scale commercial produce.Therefore how to obtain low cost, high crystalline quality perovskite absorbed layer is the emphasis that current perovskite solar cell is studied.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of high-crystallinity perovskite solar battery obsorbing layer material methyl amine lead bromide, and the method preparation technology is simple, and preparation cost is cheap, can improve the degree of crystallinity of product.
Technical solution of the present invention is:
A preparation method for high-crystallinity perovskite solar battery obsorbing layer material methyl amine lead bromide, its concrete steps are as follows:
(1) substrate is cleaned
Using FTO electro-conductive glass as substrate, after acetone and washes of absolute alcohol, cleaner with deionized water rinsing, dry;
(2) reaction solution is prepared
By solid methyl ammonium bromide (CH 3nH 3and solid brominated sub-plumbous (PbBr Br) 2) mix, join N, in dinethylformamide (DMF) solvent, stir, obtain reaction solution, the mol ratio of described methyl bromide ammonium and protobromide lead is 1:2 ~ 2:1, and described methyl bromide ammonium is 1:1mol/L ~ 1:2mol/L with the molal volume ratio of DMF;
(3) pulse electromagnetic field process
Pour in container by the reaction solution that step (2) prepares, apply pulse electromagnetic field and carry out processing reaction solution, apply burst length 2min ~ 3min, pulse voltage is 500v ~ 700v, and pulse frequency is 3Hz ~ 5Hz;
(4) spin-coating film
Reaction solution through burst process is dripped on electro-conductive glass substrate, carry out low speed spin coating and high speed spin coating respectively, forming a layer thickness is the perovskite thin film of 500nm ~ 800nm, wherein, the revolution of low speed spin coating is 800r/min ~ 1200r/min, and spin-coating time is 20s ~ 30s; The revolution of high speed spin coating is 2500r/min ~ 3500r/min, and spin-coating time is 30s ~ 40s;
(5) annealing in process
Liquid film good for spin coating in step (4) is put into vacuum drying chamber, is heated to 70 DEG C ~ 80 DEG C, insulation 20min ~ 30min, obtains methyl amine lead bromide film.
The thickness of described FTO electro-conductive glass is 3mm ~ 5mm.
During cleaning FTO electro-conductive glass substrate, first ultrasonic cleaning 10min ~ 20min in acetone, then 10min ~ 20min is cleaned in absolute ethyl alcohol.
Beneficial effect of the present invention:
(1) the methyl amine lead bromide organic-inorganic hybrid material, adopting pulse electromagnetic technology to prepare has that degree of crystallinity is high, purity is high, the advantage of compactness; 381 DEG C are brought up to from 375 DEG C by the methyl amine lead bromide organic-inorganic hybrid material decomposition temperature of thermogravimetric analysis data display after burst process, UV-visible spectrometer data display extinction width brings up to 300nm-685nm from 300nm-674nm, this material has better stability and absorbing properties, be assembled into perovskite solar cell, be conducive to improving battery efficiency and stability.
(2), pulse electromagnetic field technology energy consumption is low, Dynamic System is simple, operating cost is low, occupation area of equipment is little, parameter easily regulates, do not pollute the object handled by it and surrounding environment, is a kind of processing method of cleaner environmental protection; After adopting pulse electromagnetic field process, shorten the temperature retention time of annealing in process greatly, the temperature retention time of annealing in process is only and does not adopt 1/6 of pulse electromagnetic field process, thus shortens the production cycle of product, energy savings, is conducive to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is methyl amine lead bromide (CH prepared by the present invention's (corresponding embodiment 1 ~ embodiment 3) 3nH 3pbBr 3) the XRD collection of illustrative plates of hybrid material;
Fig. 2 is the methyl amine lead bromide (CH adopting common liquid phase method (corresponding comparative example 1) to prepare 3nH 3pbBr 3) the XRD collection of illustrative plates of hybrid material.
Embodiment
Embodiment 1
(1) substrate is cleaned
With thickness be the FTO electro-conductive glass of 3mm as substrate, first ultrasonic cleaning 10min in acetone, then clean 10min in absolute ethyl alcohol, finally clean with deionized water rinsing, dry;
(2) reaction solution is prepared
Get the solid methyl ammonium bromide (CH of 0.01mol 3nH 3and the solid brominated sub-plumbous (PbBr of 0.02mol Br) 2), add DMF (DMF) solution of 20mL, be stirred to pressed powder and all dissolve, obtain reaction solution;
(3) pulse electromagnetic field process
Pour in beaker by the reaction solution that step (2) prepares, reaction solution being applied pulse voltage is 500v, and electrical impulse frequency is the pulse electromagnetic field process 3min of 3Hz;
(4) spin-coating film
Reaction solution through burst process is dripped on electro-conductive glass substrate, carry out low speed spin coating and high speed spin coating respectively with sol evenning machine, forming a layer thickness is the perovskite thin film of 500nm ~ 600nm, wherein, the revolution of low speed spin coating is 800r/min, and spin-coating time is 30s; The revolution of high speed spin coating is 2500r/min, and spin-coating time is 40s;
(5) annealing in process
Liquid film good for spin coating in step (4) is put into vacuum drying chamber, is heated to 70 DEG C, insulation 20min, obtains methyl amine lead bromide (CH 3nH 3pbBr 3) film, as shown in Figure 1, as seen from the figure, obviously find that diffraction peak intensity is higher, wherein the diffraction maximum relative intensity of major diffraction face (110) and (220) is about 11000 ~ 14000 to its XRD collection of illustrative plates; Calculated known by XRD, its crystallite dimension is about 96nm; By thermogravimetric analysis, its decomposition temperature is 381 DEG C; Detect through UV-visible spectrometer, it shows that extinction width is 300nm-685nm.
Embodiment 2
(1) substrate is cleaned
With thickness be the FTO electro-conductive glass of 4mm as substrate, first ultrasonic cleaning 15min in acetone, then clean 15min in absolute ethyl alcohol, finally clean with deionized water rinsing, dry;
(2) reaction solution is prepared
Get the solid methyl ammonium bromide (CH of 0.01mol 3nH 3and the solid brominated sub-plumbous (PbBr of 0.01mol Br) 2), add DMF (DMF) solution of 15mL, be stirred to pressed powder and all dissolve, obtain reaction solution;
(3) pulse electromagnetic field process
Pour in beaker by the reaction solution that step (2) prepares, reaction solution being applied pulse voltage is 600v, and electrical impulse frequency is the pulse electromagnetic field process 150s of 4Hz;
(4) spin-coating film
Reaction solution through burst process is dripped on electro-conductive glass substrate, carry out low speed spin coating and high speed spin coating respectively with sol evenning machine, forming a layer thickness is the perovskite thin film of 600nm ~ 700nm, wherein, the revolution of low speed spin coating is 1200r/min, and spin-coating time is 20s; The revolution of high speed spin coating is 3500r/min, and spin-coating time is 30s;
(5) annealing in process
Liquid film good for spin coating in step (4) is put into vacuum drying chamber, is heated to 75 DEG C, insulation 25min, obtain methyl amine lead bromide film, its XRD collection of illustrative plates as shown in Figure 1; By thermogravimetric analysis, its decomposition temperature is 381 DEG C; Detect through UV-visible spectrometer, it shows that extinction width is 300nm-685nm.
Embodiment 3
(1) substrate is cleaned
With thickness be the FTO electro-conductive glass of 5mm as substrate, first ultrasonic cleaning 20min in acetone, then clean 20min in absolute ethyl alcohol, finally clean with deionized water rinsing, dry;
(2) reaction solution is prepared
Get the solid methyl ammonium bromide (CH of 0.02mol 3nH 3and the solid brominated sub-plumbous (PbBr of 0.01mol Br) 2), add DMF (DMF) solution of 20mL, be stirred to pressed powder and all dissolve, obtain reaction solution;
(3) pulse electromagnetic field process
Pour in beaker by the reaction solution that step (2) prepares, reaction solution being applied pulse voltage is 700v, and electrical impulse frequency is the pulse electromagnetic field process 2min of 5Hz;
(4) spin-coating film
Reaction solution through burst process is dripped on electro-conductive glass substrate, carry out low speed spin coating and high speed spin coating respectively with sol evenning machine, forming a layer thickness is the perovskite thin film of 700nm ~ 800nm, wherein, the revolution of low speed spin coating is 1000r/min, and spin-coating time is 25s; The revolution of high speed spin coating is 3000r/min, and spin-coating time is 35s;
(5) annealing in process
Liquid film good for spin coating in step (4) is put into vacuum drying chamber, is heated to 80 DEG C, insulation 30min, obtain methyl amine lead bromide film, its XRD collection of illustrative plates as shown in Figure 1; By thermogravimetric analysis, its decomposition temperature is 381 DEG C; Detect through UV-visible spectrometer, it shows that extinction width is 300nm-685nm.
Comparative example 1
(1) substrate is cleaned
With thickness be the FTO electro-conductive glass of 4mm as substrate, first ultrasonic cleaning 15min in acetone, then clean 15min in absolute ethyl alcohol, finally clean with deionized water rinsing, dry;
(2) reaction solution is prepared
Get the solid methyl ammonium bromide (CH of 0.01mol 3nH 3and the solid brominated sub-plumbous (PbBr of 0.01mol Br) 2), add DMF (DMF) solution of 15mL, be stirred to pressed powder and all dissolve, obtain reaction solution;
(3) spin-coating film
Dripped on electro-conductive glass substrate by reaction solution, carry out low speed spin coating and high speed spin coating respectively with sol evenning machine, forming a layer thickness is the perovskite thin film of 700nm ~ 800nm, and wherein, the revolution of low speed spin coating is 1000r/min, and spin-coating time is 25s; The revolution of high speed spin coating is 3000r/min, and spin-coating time is 35s;
(4) annealing in process
Liquid film good for spin coating in step (3) is put into vacuum drying chamber, is heated to 70 DEG C, insulation 2h, obtains methyl amine lead bromide (CH 3nH 3pbBr 3) film.Its XRD collection of illustrative plates as shown in Figure 2, as seen from the figure, the diffraction peak intensity of this product is lower relative to the diffraction peak intensity of the product adopting burst process to obtain in Fig. 1, and wherein the diffraction maximum relative intensity of major diffraction face (110) and (220) is about 3800 ~ 5000; Calculated known by XRD, its crystallite dimension is about 53nm; By thermogravimetric analysis, its decomposition temperature is 375 DEG C; Detect through UV-visible spectrometer, it shows that extinction width is 300nm-674nm.
Contrasted can be obtained by Fig. 1 and Fig. 2, the crystallite dimension of the product that the crystallite dimension of the embodiment of the present invention 1 ~ embodiment 3 product is prepared much larger than common liquid phase method (comparative example 1), can know thus, its degree of crystallinity of product adopting pulse electromagnetic field technology to prepare is greatly improved.
These are only specific embodiments of the invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (3)

1. a preparation method for perovskite solar cell light absorption layer material methyl amine lead bromide, is characterized in that:
Concrete steps are as follows:
(1) substrate is cleaned
Using FTO electro-conductive glass as substrate, after acetone and washes of absolute alcohol, cleaner with deionized water rinsing, dry;
(2) reaction solution is prepared
Solid methyl ammonium bromide and solid brominated sub-lead are mixed, join N, in dinethylformamide solvent, stir, obtain reaction solution, the mol ratio of described methyl bromide ammonium and protobromide lead is 1:2 ~ 2:1, and described methyl bromide ammonium is 1:1mol/L ~ 1:2mol/L with the molal volume ratio of DMF;
(3) pulse electromagnetic field process
Pour in container by the reaction solution that step (2) prepares, apply pulse electromagnetic field and carry out processing reaction solution, apply burst length 2min ~ 3min, pulse voltage is 500v ~ 700v, and pulse frequency is 3Hz ~ 5Hz;
(4) spin-coating film
Reaction solution through burst process is dripped on electro-conductive glass substrate, carry out low speed spin coating and high speed spin coating respectively, forming a layer thickness is the perovskite thin film of 500nm ~ 800nm, wherein, the revolution of low speed spin coating is 800r/min ~ 1200r/min, and spin-coating time is 20s ~ 30s; The revolution of high speed spin coating is 2500r/min ~ 3500r/min, and spin-coating time is 30s ~ 40s;
(5) annealing in process
Liquid film good for spin coating in step (4) is put into vacuum drying chamber, is heated to 70 DEG C ~ 80 DEG C, insulation 20min ~ 30min, obtains methyl amine lead bromide film.
2. the preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide according to claim 1, is characterized in that: the thickness of described FTO electro-conductive glass is 3mm ~ 5mm.
3. the preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide according to claim 1, it is characterized in that: during cleaning FTO electro-conductive glass substrate, first ultrasonic cleaning 10min ~ 20min in acetone, then 10min ~ 20min is cleaned in absolute ethyl alcohol.
CN201510330755.2A 2015-06-12 2015-06-12 A kind of preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide Expired - Fee Related CN104934503B (en)

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Cited By (7)

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CN105576133A (en) * 2015-12-21 2016-05-11 成都新柯力化工科技有限公司 Sprayable photovoltaic material of perovskite structure and preparation method thereof
CN107134531A (en) * 2017-05-11 2017-09-05 陕西师范大学 One kind increase perovskite CH3NH3PbI3Crystal grain is to improve the method for thin film crystallization quality
CN107482121A (en) * 2017-08-01 2017-12-15 厦门大学 A kind of preparation method of the perovskite thin film based on magnetic field regulation and control
WO2018000294A1 (en) * 2016-06-30 2018-01-04 The University Of Hong Kong An organolead halide perovskite film and the method of making the same
CN108780759A (en) * 2016-03-09 2018-11-09 牛津大学科技创新有限公司 The method for manufacturing A/M/X materials using alkylamine
CN109037459A (en) * 2018-08-03 2018-12-18 辽宁工业大学 A kind of high-purity perovskite thin film preparation method
CN109449295A (en) * 2018-10-30 2019-03-08 暨南大学 Method for preparing perovskite film based on two-step printing

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CN104269452A (en) * 2014-10-11 2015-01-07 中国科学院半导体研究所 Perovskite solar battery made of silicon-based thin-film materials and manufacturing method thereof

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CN101091899A (en) * 2007-04-28 2007-12-26 王建中 Method for catalyzing chemical reaction through pulse electromagnetic field
WO2014045021A1 (en) * 2012-09-18 2014-03-27 Isis Innovation Limited Optoelectronic device
CN103956394A (en) * 2014-05-13 2014-07-30 国家纳米科学中心 Method for improving performance of light absorption layer of perovskite solar cell
CN104269452A (en) * 2014-10-11 2015-01-07 中国科学院半导体研究所 Perovskite solar battery made of silicon-based thin-film materials and manufacturing method thereof

Cited By (16)

* Cited by examiner, † Cited by third party
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CN105576133B (en) * 2015-12-21 2017-11-28 重庆盛瓒科技有限公司 A kind of sprayable photovoltaic material of perovskite structure and preparation method thereof
CN105576133A (en) * 2015-12-21 2016-05-11 成都新柯力化工科技有限公司 Sprayable photovoltaic material of perovskite structure and preparation method thereof
CN108780759A (en) * 2016-03-09 2018-11-09 牛津大学科技创新有限公司 The method for manufacturing A/M/X materials using alkylamine
CN108780759B (en) * 2016-03-09 2023-08-08 牛津大学科技创新有限公司 Method for producing A/M/X material using alkylamine
CN109564948A (en) * 2016-06-30 2019-04-02 香港大学 Organic leadP halide perovskite thin film and the method for manufacturing it
WO2018000294A1 (en) * 2016-06-30 2018-01-04 The University Of Hong Kong An organolead halide perovskite film and the method of making the same
US10840030B2 (en) 2016-06-30 2020-11-17 The University Of Hong Kong Organolead halide perovskite film and the method of making the same
CN109564948B (en) * 2016-06-30 2022-06-21 香港大学 Organolead halide perovskite thin films and methods of making the same
CN107134531B (en) * 2017-05-11 2019-06-28 陕西师范大学 A kind of increase perovskite CH3NH3PbI3Crystal grain is to improve the method for film crystalline quality
CN107134531A (en) * 2017-05-11 2017-09-05 陕西师范大学 One kind increase perovskite CH3NH3PbI3Crystal grain is to improve the method for thin film crystallization quality
CN107482121A (en) * 2017-08-01 2017-12-15 厦门大学 A kind of preparation method of the perovskite thin film based on magnetic field regulation and control
CN107482121B (en) * 2017-08-01 2019-09-17 厦门大学 A kind of preparation method of the perovskite thin film based on magnetic field regulation
CN109037459A (en) * 2018-08-03 2018-12-18 辽宁工业大学 A kind of high-purity perovskite thin film preparation method
CN109037459B (en) * 2018-08-03 2022-03-11 辽宁工业大学 Preparation method of high-purity perovskite film
CN109449295A (en) * 2018-10-30 2019-03-08 暨南大学 Method for preparing perovskite film based on two-step printing
CN109449295B (en) * 2018-10-30 2023-09-22 麦耀华 Method for preparing perovskite film based on two-step printing

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