CN104993058B - A kind of laminated perovskite structure material and the application in methylamine lead iodine perovskite thin film solar cell - Google Patents

A kind of laminated perovskite structure material and the application in methylamine lead iodine perovskite thin film solar cell Download PDF

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CN104993058B
CN104993058B CN201510277550.2A CN201510277550A CN104993058B CN 104993058 B CN104993058 B CN 104993058B CN 201510277550 A CN201510277550 A CN 201510277550A CN 104993058 B CN104993058 B CN 104993058B
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polymer
lead
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side chain
iodine
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CN104993058A (en
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李璠
姚凯
王晓峰
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Nanchang University
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    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/50Organic perovskites; Hybrid organic-inorganic perovskites [HOIP], e.g. CH3NH3PbI3
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/10Organic polymers or oligomers
    • 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

A kind of laminated perovskite structure material and the application in methylamine lead iodine perovskite thin film solar cell.Chemical structure of general formula is:A2PbX4, wherein A is polymer of the side chain with primaquine group comprising main chain is the polymer of conjugated structure and the polymer that main chain is saturated carbon carbon or carbon nitrogen chain;X is one or more in chlorine, bromine or iodine.The material is applied in methylamine lead iodine perovskite thin film solar cell.The present invention effectively improves the quality of forming film of methylamine lead iodine perovskite active layer, the optical property having had, uniform pattern, and crystal particle scale reaches micron dimension;Interface energy level can be regulated and controled, realize preferable level-density parameter, reduce interface energy level potential barrier, improve device performance, energy conversion efficiency is up to 16.0%, and repeatability is good;And blocking capability of the device to water vapor in air can be improved, improve the stability of battery.

Description

A kind of laminated perovskite structure material and in methylamine lead iodine perovskite thin film solar-electricity Application in pond
Technical field
The invention belongs to technical field of solar batteries.
Background technology
In numerous novel solar batteries, the methylamine lead iodine based on organic inorganic hybridization is the Ca-Ti ore type of active layer Thin-film solar cells due to it with high absorptivity, exciton lifetime is long and binding energy is low, excellent carrier transport it is special Property and it is at low cost, preparation process is simple, photoelectric conversion rate is high, be easily achieved the advantages that large area flexible device, it can be achieved that with The photoelectric conversion efficiency that silica-based solar cell is equal to, and as the battery class of current film photovoltaic technical field most competitiveness Type.Currently, the efficiency for having such Ca-Ti ore type solar cell certification of document report has been up to 17.9% [Nat.Photon, 2014,8,506-514] should according to the battery efficiency data of the newest announcement in U.S. regenerative resource laboratory The peak efficiency of class battery records more than 20% [National Renewable Energy Laboratory.http:// www.nrel.gov/ncpv/images/efficiency_chart.jpg(2015)].However, current methylamine lead iodine perovskite Field of thin film solar cells still suffers from two main problems:1) nucleation of methylamine lead iodine film is difficult to control with crystallization process System;2) methylamine lead iodine perovskite thin film stability of material is poor, especially sensitive to the water oxygen in humid air.These problems are all tight Ca-Ti ore type thin-film solar cells efficiency is affected again to improve and use, and is further applied to limit it.
In order to regulate and control nucleation, the crystallization process of perovskite thin film material, to improve it into film uniformity, crystal grain ruler Very little and crystalline quality, and then device performance is improved, people use the preparation process that many measures improve perovskite thin film, such as Regulate and control presoma chemical constituent with Optimal Growing dynamics [Adv.Funct.Mater.2014,24,151, Chem.Mater.2014,26,7145], select different solvents [Nat.Mater.2014,13,897, Adv.Mater.2014, 26,3748], [2015,347,522, Acs Nano 2015,9,639 of Science] is made annealing treatment, different deposition methods [J.Am.Chem.Soc.2014,136,622, Angew Chem.Int.Ed.2014,53,9898] etc..In addition to improving perovskite Outside film-forming process, numerous studies, it was also found that interface modification for regulate and control the also helpful [Science of perovskite film forming procedure 2014,345,295, Nanoscale 2014,6,1508, J.Phys.Chem.C 2014,118,16651].Further, since first Amine lead iodine perovskite material itself is sensitive to water, the oxygen in air, to bring the problem of battery device stability difference, influences Battery.Although there is a small amount of document report at present, the presence of low content vapor has conducive to the crystallization of methylamine lead iodine [Science 2014,345,542, Chem.Commun.2014,50,15819], but most of research group is still in gloves The deposition of methylamine lead iodine film is carried out in case under dry atmosphere.Recently, it has been reported that by select larger organic sun from Perovskite material can be evolved into two-dimensional layered structure by son from three-dimensional structure, and such layered perovskites is in air Water, oxygen it is insensitive, stability is good [Angew Chem.Int.Ed.2014,53,11232], but due to such two-dimensional layer Structure causes exciton bind energy big, current-carrying there are the dielectric property mismatch between limited space and organic layer and inorganic layer Transport factor is low, limits its application as active layer in Ca-Ti ore type thin-film solar cells.
In the course of the research, it has been found that polymer of the side chain with primaquine group is through halogenation (including chlorination, bromination and iodine Change) after, is blended with lead halide (including lead chloride, lead bromide and lead iodide) can obtain it is a kind of it is novel based on side chain with primaquine The two-dimensional layer perovskite structure of the polymer of group.It is applied to methylamine using the two-dimensional layer perovskite structure as boundary material In lead iodine Ca-Ti ore type thin-film solar cells, can not only effectively regulation activity layer methylamine lead iodine film deposition growing mistake Journey obtains film uniform, fine and close and compared with big crystal grain, but also can regulate and control interface energy level, reduces interface carrier and transmits gesture It builds.In addition, the application of such two-dimensional layer perovskite structure can also effectively improve methylamine lead iodine Ca-Ti ore type thin film solar Battery is to the tolerance of water, oxygen in air, to improve the stability and service life of battery.Such is based on side chain band primaquine The laminated perovskite structure of the polymer of group is applied to methylamine lead iodine Ca-Ti ore type thin-film solar cells, up to the present, Have no pertinent literature and patent report both at home and abroad.
Invention content
The object of the present invention is to provide a kind of laminated perovskite structure material and its in methylamine lead iodine Ca-Ti ore type film Application in solar cell.After polymer halogenation (including chlorination, bromination and iodate) of the side chain with primaquine group, then with halogen Change lead (including lead chloride, lead bromide and lead iodide) be blended to get to a series of based on polymer of the side chain with primaquine group Two-dimensional layer perovskite structure, study its as boundary material answering in methylamine lead iodine Ca-Ti ore type thin-film solar cells With.
The present invention is achieved by the following technical solutions.
A kind of laminated perovskite structure material of the present invention, it is characterised in that it is with following chemical structure of general formula:
A2PbX4
Wherein, A is polymer of the side chain with primaquine group, including the side chain that main chain is conjugated structure is poly- with primaquine group It is to be saturated the side chain of carbon-to-carbon or carbon-to-nitrogen chain with the polymer of primaquine group to close object and main chain;X be chlorine, one kind in bromine or iodine or It is a variety of;
The main chain is side chain of the side chain of conjugated structure with the polymer of primaquine group, including main chain for conjugated structure With primaquine group conjugation homopolymer and main chain be conjugated structure side chain with the conjugated copolymer of primaquine group;
Wherein:Main chain is that conjugation homopolymer chemical structure of general formula of the side chain of conjugated structure with primaquine group is:
Main chain is that conjugated copolymer chemical structure of general formula of the side chain with primaquine group of conjugated structure is:
Unit B is:
D, E units are:
The main chain is that be saturated the side chain of carbon-to-nitrogen chain with the polymer of primaquine group be shown in following formula:
Wherein, n is the repetition number of polymer main chain units, is natural number 1-100;
The main chain is that be saturated the side chain of carbon carbon bond with the polymer of primaquine group be shown in following formula:
Wherein, n and m is the repetition number of polymer main chain units, is natural number 1-100.
A2PbX4The preparation method of laminated perovskite structure material is as follows:
Polymer of the side chain with primaquine group is carried out halogenation by the first step:At nitrogen protection, 0 DEG C, by 2g (2.5mmol) Polymer of the side chain with primaquine group, 10ml (0.04mol) hydroiodic acid and 100ml methanol be added 250 milliliters round bottom burn In bottle, continuously stir 12 hours.After reaction, reaction product rotates at 40 DEG C, is then cleaned with ether.And then use ethyl alcohol Recrystallization, is placed in vacuum drying chamber, in 40 DEG C of dried for standby.
Second step synthesizes A2PbX4Laminated perovskite structure material:Polymer of the side chain after halogenation with primaquine group is molten In the n,N-Dimethylformamide of certain volume, then in molar ratio 1:1 (the amino mole i.e. on polymer is rubbed with lead halide The ratio between your amount is 1:1) lead halide, stirring a period of time, you can obtain A is added2PbX4Laminated perovskite structure material.
From the A of attached drawing 1 and attached drawing 22PbX4The infrared suction of hydrogen nuclear magnetic resonance spectrogram and fourier of laminated perovskite structure material Spectrogram is received it can be proved that the present invention successfully synthesizes the laminated perovskite structure material and its chemical structural formula.
It is located at the diffraction maximum explanation that 8.07 ° of places occur in attached drawing 4, which is typical layer structure.
Laminated perovskite structure material of the present invention is as boundary material in the methylamine lead iodine Ca-Ti ore type film sun Application in energy battery structure, prepares solar cell device.
Solar battery structure of the present invention is as shown in figure 4, include host glass or plastic material (1), ito anode Layer (2), poly- (3,4- dichloroethanes thiophene)/(poly- (styrene sulfonate) (PEDOT:PSS) anode modification layer (3), be based on side chain Laminated perovskite structure material (4), methylamine lead iodine perovskite material (5), 1- (the 3- methoxyl group carbonyls of polymer with primaquine group Base) propyl -1- phenyl [6,6]-C-61 (PCBM) layer cathodic modification layers (6), Ag metal electrode layers (7).It is described based on side chain The laminated perovskite structure material of polymer with primaquine group is mainly used for the boundary layer of solar cell.
A kind of laminated perovskite structure material of the present invention is used as methylamine lead iodine Ca-Ti ore type thin-film solar cells Preparation method it is as follows:
Detergent, deionized water, isopropanol will be used to be cleaned by ultrasonic respectively very successively through the good ito glass of salt acid etch Clock is thoroughly put under ultraviolet lamp after cleaning and irradiates ten minutes, then in its surface spin coating PEDOT:The aqueous solution of PSS is to prepare The PEDOT of about 30-50nm thickness:PSS films are then put in 120 DEG C of heating 20min.Boundary layer and active layer are prepared again, it is living Property layer prepares and then 1- (3- methoxycarbonyls) propyl -1- phenyl [6,6]-C-61 (PCBM) is spin-coated on active layer, Later, it is put into vacuum coating equipment intracavitary, is evacuated to 4 × 10-4For Pa hereinafter, vapor deposition Ag electrodes, it is 100nm left to control its thickness It is right, you can to obtain methylamine lead iodine Ca-Ti ore type thin-film solar cells.In the present invention, in addition to Ag electrodes are deposited, other each layers Completed under the atmospheric atmosphere for having certain humidity.
The preparation of boundary layer and active layer of the present invention is will to be based on side chain band primaquine by one-step method or two-step method The laminated perovskite structure material of the polymer of group is introduced into methylamine lead iodine Ca-Ti ore type film solar battery structure Process.
The one-step method refers to that polymer of the side chain after halogenation with primaquine group is first spin-coated on PEDOT:PSS is buffered On layer, then (mass ratio is by the lead halide (including lead chloride, lead bromide and lead iodide) of certain mol proportion and methylamino iodine 45%) active layer precursor mixed solution is spin-coated on polymer of the side chain after halogenation with primaquine group, prepares active layer, The one-step method is while preparing active layer, in PEDOT:Base is formed in situ in interface between PSS buffer layers and active layer In the two-dimensional layer perovskite structure boundary material of polymer of the side chain with primaquine group.
The two step method refers to that lead halide (including lead chloride, lead bromide and lead iodide) is first spin-coated on PEDOT:PSS On buffer layer, then polymer of the side chain after halogenation with primaquine group be spin-coated on halogenation thin film lead, formed and be based on side chain band The two-dimensional layer perovskite structural material of the polymer of primaquine group, then by the lead halide of certain mol proportion (including lead chloride, bromine Change lead and lead iodide) it is spin-coated on based on polymer of the side chain with primaquine group with the active layer precursor mixed solution of methylamino iodine Two-dimensional layer perovskite structural material on, prepare active layer, thickness control is in 400nm or so.
Beneficial effects of the present invention:Laminated perovskite structure material of the present invention is applied to methylamine as boundary material PEDOT in lead iodine Ca-Ti ore type thin-film solar cells:Between PSS buffer layers and active layer, crystal seed can not only be used as Layer effectively improves the quality of forming film of methylamine lead iodine perovskite active layer, the optical property that prepared active layer has had, uniformly Pattern, crystal particle scale reaches micron dimension;Meanwhile the bed boundary material have higher work function, application can also Regulate and control interface energy level, realize preferable level-density parameter, reduces interface energy level potential barrier.Therefore, it is effectively improved device performance, Energy conversion efficiency was up to for 16.0% (flexible device efficiency reaches 12.5%), and repeatability is good for battery making.In addition, should The application of boundary material can also improve blocking capability of the battery device to water vapor in air, to improve the stability of battery And service life still keeps 80% energy conversion efficiency after unencapsulated 100 hours of placement in air.
Description of the drawings
Fig. 1 is A2PbX4The hydrogen nuclear magnetic resonance spectrogram of laminated perovskite structure material.
Fig. 2 is A2PbX4The fourier infrared absorpting light spectra of laminated perovskite structure material.
Fig. 3 is A2PbX4The X ray diffracting spectrum of laminated perovskite structure material.
Fig. 4 is the structural schematic diagram of methylamine lead iodine Ca-Ti ore type thin-film solar cells.1 is host glass or plastics material Material, 2 be ito anode layer, and 3 be poly- (3,4- dichloroethane thiophene)/poly- (styrene sulfonate) (PEDOT:PSS) anode modification Layer, 4 be the laminated perovskite structure material based on polymer of the side chain with primaquine group;5 be methylamine lead iodine perovskite material, 6 It is Ag metal electrode layers for 1- (3- methoxycarbonyls) propyl -1- phenyl [6,6]-C-61 (PCBM) layer cathodic modification layer, 7.
Fig. 5 is embodiment 1 using the two-dimensional layer perovskite structure based on polyethyleneimine polymers as boundary material one The voltage-current curve of methylamine lead iodine Ca-Ti ore type thin-film solar cells prepared by footwork.
Fig. 6 is embodiment 1 using the two-dimensional layer perovskite structure based on polyethyleneimine polymers as boundary material one The device energy conversion efficiency of methylamine lead iodine Ca-Ti ore type thin-film solar cells prepared by footwork changes with time tendency chart.
Fig. 7 is embodiment 2 using the two-dimensional layer perovskite structure based on polyethyleneimine polymers as boundary material two The voltage-current curve of methylamine lead iodine Ca-Ti ore type thin-film solar cells prepared by footwork.
Fig. 8 is embodiment 3 using the two-dimensional layer perovskite structure based on polythiophene of the side chain with primaquine group as interface The voltage-current curve of methylamine lead iodine Ca-Ti ore type thin-film solar cells prepared by material two-step method.
Specific implementation mode
The present invention will be described further by following embodiment.
Embodiment 1:One-step method prepares methylamine lead iodine Ca-Ti ore type thin-film solar cells device.
By PbCl2, PbI2And CH3NH3I is 1 according to molar ratio:1:4, the concentration that total mass fraction is 45% is dissolved in In n,N-Dimethylformamide (DMF) solution, 12h is stirred at room temperature.Ito glass surface is cleaned, table is cleaned in UV ozone After the 10min of face, using the rotating speed of 4000rpm conducting polymer PEDOT:PSS is spin-coated on glass, then 140 DEG C of heating 10min, and then in PEDOT:The surface of PSS is carried out with the rotating speed spin coating PEIHI (10mg/ml, methanol solution) of 3000rpm Modification.Then perovskite thin film is prepared on its surface with the rotating speed spin coating of 4000rpm in perovskite solution.Substrate after spin coating It is placed in thermal station, 100 DEG C of heating 60min.Perovskite thin film surface with the rotating speed spin coating PCBM of 1500rpm (20mg/ml, Chlorobenzene solution).Finally in high vacuum conditions, Ag electrodes are deposited, obtain solar cell.
Device performance is:Standard analog sunlight (AM 1.5G, 100mW/cm2) under irradiation, open-circuit voltage=1.08V;It is short Road electric current=19.61mA/cm2;Fill factor=70.5%;Energy conversion efficiency=15.0%.Its current -voltage curve is for example attached Shown in Fig. 5, device performance stability is as shown in Figure 6.
Embodiment 2:Two-step method prepares methylamine lead iodine Ca-Ti ore type thin-film solar cells device.
The PbI of 462mg/ml is respectively configured2The CH of/DMF solution and 20mg/ml3NH3I/ aqueous isopropanols.Same cleaning Ito glass surface, after UV ozone cleans surface 10min, using the rotating speed of 4000rpm conducting polymer PEDOT:PSS It is spin-coated on glass, then 140 DEG C of heating 10min, in PEDOT:The surface of PSS is with the rotating speed spin coating PEIHI of 3000rpm (10mg/ml, methanol solution) is modified.Then PbI2Solution is with the rotating speed spin coating of 4000rpm, and then spin coating on it CH3NH3I solution.Substrate is placed in thermal station after spin coating, 100 DEG C of heating 10min.On perovskite thin film surface with 1500rpm Rotating speed spin coating PCBM (20mg/ml, chlorobenzene solution).Finally in high vacuum conditions, Ag electrodes are deposited, obtain solar-electricity Pond.
Device performance is:Standard analog sunlight (AM 1.5G, 100mW/cm2) under irradiation, open-circuit voltage=1.06V;It is short Road electric current=19.66mA/cm2;Fill factor=72.1%;Energy conversion efficiency=14.9%, current -voltage curve are for example attached Shown in Fig. 7.
Embodiment 3:The preparation of methylamine lead iodine Ca-Ti ore type thin-film solar cells device.
By PbCl2, PbI2And CH3NH3I is 1 according to molar ratio:1:4, the concentration that total mass fraction is 45% is dissolved in In n,N-Dimethylformamide (DMF) solution, 12h is stirred at room temperature.Ito glass surface is cleaned, table is cleaned in UV ozone After the 10min of face, using the rotating speed of 4000rpm conducting polymer PEDOT:PSS is spin-coated on glass, then 140 DEG C of heating 10min, and then in PEDOT:The surface of PSS with the rotating speed spin coating PTNHI (10mg/ml, aqueous isopropanol) of 3000rpm into Row modification.Then perovskite thin film is prepared on its surface with the rotating speed spin coating of 4000rpm in perovskite solution.Base after spin coating Piece is placed in thermal station, 100 DEG C of heating 60min.On perovskite thin film surface with the rotating speed spin coating PCBM (20mg/ of 1500rpm Ml, chlorobenzene solution).Finally in high vacuum conditions, steaming degree Ag electrodes obtain solar cell.
Device performance is:Standard analog sunlight (AM 1.5G, 100mW/cm2) under irradiation, open-circuit voltage=1.10V;It is short Road electric current=20.20mA/cm2;Fill factor=71.9%;Energy conversion efficiency=16.0%, current -voltage curve are for example attached Shown in Fig. 8.

Claims (2)

1. a kind of laminated perovskite structure material is used as the preparation method of methylamine lead iodine Ca-Ti ore type thin-film solar cells, special Sign is:Steps are as follows:
Detergent will be used successively through the good ito glass of salt acid etch, deionized water, isopropanol is cleaned by ultrasonic ten minutes respectively, thorough It is put under ultraviolet lamp and irradiates ten minutes after the cleaning of bottom, then in its surface spin coating PEDOT:The aqueous solution of PSS is to prepare 30- The PEDOT of 50nm thickness:PSS films are then put in 120 DEG C of heating 20min;Boundary layer and active layer, active layer are prepared again It prepares and then 1- (3- methoxycarbonyls) propyl -1- phenyl [6,6]-C-61 (PCBM) is spin-coated on active layer, it Afterwards, it is put into vacuum coating equipment intracavitary, is evacuated to 4 × 10-4For Pa hereinafter, vapor deposition Ag electrodes, it is 100nm to control its thickness, you can Obtain methylamine lead iodine Ca-Ti ore type thin-film solar cells;
The preparation of the boundary layer and active layer is will be based on polymerization of the side chain with primaquine group by one-step method or two-step method The laminated perovskite structure material of object is introduced into the process in methylamine lead iodine Ca-Ti ore type film solar battery structure;
The one-step method refers to that polymer of the side chain after halogenation with primaquine group is first spin-coated on PEDOT:PSS buffer layers On, then the active layer precursor mixed solution for the methylamino iodine that lead chloride, lead bromide or lead iodide and mass ratio are 45% revolved Be coated on polymer of the side chain after halogenation with primaquine group, prepare active layer, the one-step method while preparing active layer, In PEDOT:The two dimension based on polymer of the side chain with primaquine group is formed in situ in interface between PSS buffer layers and active layer Laminated perovskite structure boundary material;
The two-step method refers to that lead chloride, lead bromide or lead iodide are first spin-coated on PEDOT:On PSS buffer layers, then by halogenation Polymer of the side chain afterwards with primaquine group is spin-coated on halogenation thin film lead, is formed based on polymer of the side chain with primaquine group Two-dimensional layer perovskite structural material, then lead chloride, lead bromide or lead iodide are mixed with the active layer precursor of methylamino iodine Solution is spin-coated on the two-dimensional layer perovskite structural material based on polymer of the side chain with primaquine group, prepares active layer, Its thickness control is in 400nm.
2. a kind of laminated perovskite structure material as described in claim 1 is used as methylamine lead iodine Ca-Ti ore type thin film solar electricity The preparation method in pond, it is characterised in that:The specific method is as follows:
The PbI of 462mg/ml is respectively configured2The CH of/DMF solution and 20mg/ml3NH3I/ aqueous isopropanols are cleaned in UV ozone After the 10min of ito glass surface, using the rotating speed of 4000rpm conducting polymer PEDOT:PSS is spin-coated on glass, and then 140 DEG C heating 10min, in PEDOT:The surface of PSS is molten with the PEIHI methanol of a concentration of 10mg/ml of rotating speed spin coating of 3000rpm Liquid is modified;Then PbI2Solution is with the rotating speed spin coating of 4000rpm, and then spin coating CH on it3NH3I solution;Spin coating Substrate is placed in thermal station afterwards, 100 DEG C of heating 10min;It is a concentration of with the rotating speed spin coating of 1500rpm on perovskite thin film surface The PCBM chlorobenzene solutions of 20mg/ml;Finally in high vacuum conditions, Ag electrodes are deposited, obtain solar cell.
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