CN108922972A - Perovskite thin film, perovskite solar battery and preparation method thereof - Google Patents
Perovskite thin film, perovskite solar battery and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to perovskite thin films, perovskite solar battery and preparation method thereof.The perovskite thin film includes Ca-Ti ore type ABX3Hybrid inorganic-organic materials and polymer, the polymer are polymerize to obtain by acrylate monomer.Preparation method includes the following steps：By acrylate monomer, AX and BX2It is dissolved in solvent, obtains perovskite precursor solution；The perovskite precursor solution is formed in a substrate；Annealing and lighting process are successively carried out to the substrate with perovskite precursor solution, obtain perovskite thin film；Wherein, the acrylate carries out polymerization reaction during lighting process.Perovskite thin film of the invention protects perovskite crystal boundary, and the stability of perovskite thin film is good.It is applied in perovskite solar battery and preparation method thereof, perovskite solar battery can be made also with good stability while there is high transformation efficiency.
Description
Technical field
The present invention relates to technical field of solar batteries, more particularly to perovskite thin film, perovskite solar battery and
Preparation method.
Background technique
Perovskite solar battery efficiency is high, at low cost, receives the extensive concern of people in recent years.Currently, restricting calcium
The maximum bottleneck that titanium ore solar battery moves towards practical is its stability.Therefore, how to maintain its efficient simultaneously
Improving its stability to the maximum extent becomes a significantly research direction.
The stability of perovskite solar battery is somewhat dependent upon the stability of perovskite thin film.Traditional
In the preparation method of perovskite thin film, the perovskite thin film of solwution method preparation usually contains very more surface and grain boundary defects,
Cause the water in air, oxygen etc. that can penetrate into inside perovskite by these defects, and then causes the decomposition of perovskite.Meanwhile
Since boundary defect is unstable, the easy attack by extraneous factor (such as illumination, electric field, heating) on energy,
It can accelerate the decomposition of perovskite.Therefore, it in order to improve the stability of perovskite thin film, needs to protect the crystal boundary of perovskite
Shield.
Summary of the invention
Based on this, it is necessary to for the unstable problem of perovskite thin film, provide a kind of perovskite thin film and its preparation side
Method, the perovskite thin film protect perovskite crystal boundary, and the stability of perovskite thin film is good；It is applied to perovskite too
In positive energy battery and preparation method thereof, perovskite solar battery can be made also to have while there is high transformation efficiency good steady
It is qualitative.
A kind of perovskite thin film, the perovskite thin film include Ca-Ti ore type ABX3Hybrid inorganic-organic materials and polymerization
Object, the polymer are polymerize to obtain by acrylate monomer.
In above-mentioned perovskite thin film, polymer contains C=O functional group and C=C functional group, and wherein C=O functional group can be with
B ion (such as Pb of perovskite grain boundaries2+、Sn2+、Ge2+Deng) by coordinate bond generation weak interaction, it can effectively adjust calcium
The growth of titanium ore film, therefore the perovskite thin film even compact, without obvious cavity, the grain boundary defects of perovskite thin film are had
Effect passivation, to improve the stability of perovskite thin film.C=O functional group and B ion (such as Pb simultaneously2+、Sn2+、Ge2+Deng)
Coordination can make polymer be effectively adhered grain boundaries, to form fine and close protective layer in grain boundaries, and then stop
The decomposition of water, oxygen and additional factor to perovskite improves the stability of perovskite battery.Therefore, polymer not only may be used
Using the protective layer as perovskite crystal boundary, it can also be passivated the defect of crystal boundary, the stability for improving perovskite thin film can be cooperateed with.
The acrylate monomer is methyl methacrylate, ethyl methacrylate, cyanogen in one of the embodiments,
One of base ethyl acrylate is a variety of.
In one of the embodiments, the mass percent of polymer described in the perovskite thin film be 0.3%~
2%.
The Ca-Ti ore type ABX in one of the embodiments,3In hybrid inorganic-organic materials A be organic amine sun from
Son, B Pb2+、Sn2+、Ge2+In any one, X be halide anion or SCN-。
A kind of preparation method of perovskite thin film, the preparation method comprises the following steps：
By acrylate monomer, AX and BX2It is dissolved in solvent, obtains perovskite precursor solution；
The perovskite precursor solution is formed in a substrate；
Annealing and lighting process are successively carried out to the substrate with perovskite precursor solution, it is thin to obtain perovskite
Film；Wherein, the acrylate carries out polymerization reaction during lighting process.
In the preparation method of above-mentioned perovskite thin film, the acrylate monomer in perovskite precursor solution can be in illumination
Under the action of and polymerization reaction independently occurs, obtain polymer.The reaction step is simple, easy, is not necessarily to other reaction conditions,
It is easy to industrialize.
During the reaction, acrylate contains C=O functional group and C=C functional group, wherein C=O functional group and calcium titanium
B ion (such as Pb of mine grain boundaries2+、Sn2+、Ge2+Deng) by coordinate bond generation weak interaction, it is passivated grain boundary defects.C simultaneously
=O functional group and B (such as Pb2+、Sn2+、Ge2+Deng) coordination polymer can be made to be effectively adhered grain boundaries, by light
According to processing, polymerization reaction occurs for the C=C functional group in acrylate, thus in grain boundaries formation dense protective layer, blocking water,
The decomposition of oxygen and additional factor to perovskite, improves the stability of perovskite thin film.
The A in the AX is organic amine cation in one of the embodiments, and X is halide anion or SCN-；It is described
BX2In B be Pb2+、Sn2+、Ge2+In any one.
The temperature of the annealing is 80 DEG C~100 DEG C in one of the embodiments, and the time is 5min~10min.
The lighting process is that use is ultraviolet, infrared or sunlight irradiation, time are in one of the embodiments,
5min~30min.
A kind of perovskite solar battery, hole transmission layer, perovskite thin film and electron transfer layer including lamination setting,
The perovskite thin film includes Ca-Ti ore type ABX3Hybrid inorganic-organic materials and polymer, the polymer is by acrylate
Monomer polymerization obtains.
Above-mentioned perovskite thin film even compact, without apparent cavity, and perovskite thin film has excellent stability.Cause
This, not only has high transformation efficiency using the perovskite solar battery of above-mentioned perovskite thin film, while also having good steady
It is qualitative.
A kind of preparation method of perovskite solar battery, the preparation method comprises the following steps：
One substrate is provided；
Hole transmission layer is formed over the substrate；And
Perovskite thin film is formed using above-mentioned preparation method on the hole transport layer；And
Electron transfer layer is formed on the perovskite thin film；And
Electrode is formed on the electron transport layer.
The preparation method of above-mentioned perovskite solar battery has the advantages that simple, easy-operating.The obtained perovskite sun
Energy battery has high transformation efficiency and good stability.
Detailed description of the invention
Fig. 1 is the forward and backward infared spectrum figure of lighting process of the perovskite thin film of the embodiment of the present invention 1, and in figure, a is light
According to the infrared curve of perovskite thin film after processing, b is the infrared curve of perovskite thin film before lighting process；
Fig. 2 is the plane and cross-sectional scans electron microscope of perovskite thin film prepared by the embodiment of the present invention 1 and comparative example 1, figure
In, b is the flat scanning electron microscope of perovskite thin film prepared by embodiment 1, and d is cutting for perovskite thin film prepared by embodiment 1
Surface scan electron microscope, a are the flat scanning electron microscope of perovskite thin film prepared by comparative example 1, and c is calcium titanium prepared by comparative example 1
The cross-sectional scans electron microscope of mine film；
Fig. 3 is the steady-state fluorescence spectrogram of perovskite thin film prepared by the embodiment of the present invention 1 and comparative example 1, and in figure, c is
The fluorescence spectra of the perovskite thin film of comparative example 1, d are the fluorescence spectra of the perovskite thin film of embodiment 1；
Fig. 4 is the time resolution fluorescence spectral figure of perovskite thin film prepared by the embodiment of the present invention 1 and comparative example 1, in figure,
E is the time resolution fluorescence spectral of the perovskite thin film of embodiment 1, and f is the fluorescence spectra of the perovskite thin film of comparative example 1；
Fig. 5 is X-ray diffraction (XRD) the map comparison of perovskite thin film prepared by the embodiment of the present invention 1 and comparative example 1
Scheme, in figure, h is the X-ray diffraction curve of the perovskite thin film of comparative example 1, and g is that the X-ray of the perovskite thin film of embodiment 1 is spread out
Penetrate curve；
Fig. 6 is the structural schematic diagram of perovskite solar battery of the present invention, and in figure, 1 is substrate, and 2 be hole transmission layer, 3
It is electron transfer layer for perovskite thin film, 4,5 be electrode；
Fig. 7 is the stability contrast figure of the perovskite solar battery of the embodiment of the present invention 7 and comparative example 2, and in figure, i is
The aerial stability of perovskite solar battery of embodiment 7, j are the perovskite solar battery of comparative example 2 in air
In stability.
Specific embodiment
Perovskite thin film provided by the invention, perovskite solar battery and preparation method thereof will be made furtherly below
It is bright.
Perovskite thin film provided by the invention includes Ca-Ti ore type ABX3Hybrid inorganic-organic materials and polymer, it is described
Polymer is polymerize to obtain by acrylate monomer.
The mass percent of polymer described in the perovskite thin film is 0.3%~2%.Perovskite thin film is being applied
When, such as in perovskite solar battery in application, in view of polymer imitates the transformation efficiency of battery and the improvement of stability
Fruit, it is preferable that the mass percent of polymer described in the perovskite thin film is 0.3%~1%.
The Ca-Ti ore type ABX3A is organic amine cation, B Pb in hybrid inorganic-organic materials2+、Sn2+、Ge2+In
Any one, X be halide anion or SCN-.Preferably, the A is CH3NH3 +、HC(NH2)2 +、CH3CH2NH3 +In it is any
One kind, the X are Cl-、Br-、I-In any one.Due to CH3NH3PbI3Electrons and holes diffusion length be respectively
130nm and 100nm, forbidden bandwidth 1.51eV have good absorption within the scope of 400nm~800nm, therefore, the calcium
Titanium ore type ABX3Hybrid inorganic-organic materials are more preferably CH3NH3PbI3。
The acrylate monomer is methyl methacrylate, ethyl methacrylate, one in cyanacrylate
Kind is a variety of.Since cyano also can be with B ion (such as Pb in cyanacrylate2+、Sn2+、Ge2+Deng) weak interaction occurs,
Passivation grain boundary defects are more advantageous to, the stability of perovskite thin film is improved.Meanwhile cyanacrylate can be in mild item
(illumination or in air spontaneous polymerization) polymerize under part, it is easy to accomplish low temperature solution polycondensation prepares perovskite thin film.In addition,
Cyanacrylate is liquid at room temperature, it is easier to it is incorporated into perovskite precursor solution, it can be in the larger context
Adjust its content in perovskite thin film.Therefore, the acrylate is more preferably Methyl 2-cyanoacrylate.
In above-mentioned perovskite thin film, polymer contains C=O functional group and C=C functional group, and wherein C=O functional group can be with
B ion (such as Pb of perovskite grain boundaries2+、Sn2+、Ge2+Deng) by coordinate bond generation weak interaction, it can effectively adjust calcium
The growth of titanium ore film, therefore the perovskite thin film even compact, without obvious cavity, the grain boundary defects of perovskite thin film are had
Effect passivation, to improve the stability of perovskite thin film.C=O functional group and B ion (such as Pb simultaneously2+、Sn2+、Ge2+Deng)
Coordination can make polymer be effectively adhered grain boundaries, to form fine and close protective layer in grain boundaries, and then stop
The decomposition of water, oxygen and additional factor to perovskite improves the stability of perovskite battery.Therefore, polymer not only may be used
Using the protective layer as perovskite crystal boundary, it can also be passivated the defect of crystal boundary, the stability for improving perovskite thin film can be cooperateed with.
The present invention also provides a kind of preparation methods of perovskite thin film, and the preparation method comprises the following steps：
S1, by acrylate monomer, AX and BX2It is dissolved in solvent, obtains perovskite precursor solution；
The perovskite precursor solution is formed in a substrate by S2；
S3 successively carries out annealing and lighting process to the substrate with perovskite precursor solution, obtains perovskite
Film；Wherein, the acrylate carries out polymerization reaction during lighting process.
In step sl, the BX2Molar ratio with AX is 1:(0.8~1.2), preferably 1:1.
A in the AX is organic amine cation, and X is halide anion or SCN-.Preferably, the A is CH3NH3 +、HC
(NH2)2 +、CH3CH2NH3 +In any one, the X be Cl-、Br-、I-In any one.Due to the Ca-Ti ore type ABX3
Hybrid inorganic-organic materials are more preferably CH3NH3PbI3, therefore, the AX corresponding is preferably CH3NH3I。
The BX2In B be Pb2+、Sn2+、Ge2+In any one, X be halide anion or SCN-.Preferably, described
B is Pb2+、Sn2+One of, the X is Cl-、Br-、I-In any one.Due to the Ca-Ti ore type ABX3Organic and inorganic
Hybrid material is more preferably CH3NH3PbI3, therefore, the BX2Corresponding is preferably PbI2。
The solvent is n,N-Dimethylformamide and the mixed solvent that dimethyl sulfoxide forms, in the mixed solvent N, N- bis-
Methylformamide and the volume ratio of dimethyl sulfoxide are (3~5)：1, preferably 4:1.
In step s3, the temperature of the annealing is 80 DEG C~100 DEG C, and the time is 5min~10min.In substrate
It is made annealing treatment after forming perovskite precursor solution, crystallizes perovskite precursor solution, obtain perovskite thin film.Consider
To the requirement being sufficiently fully crystallized, preferable temperature is 100 DEG C, and the preferably time is 10min.
The lighting process is to be irradiated using ultraviolet, infrared or sunlight, and the time is 5min~30min.At annealing
The perovskite thin film further progress lighting process that formation is crystallized after reason occurs the acrylate in perovskite thin film in situ poly-
It closes, generates stable polymer.In view of sunlight be easily obtained and acrylate need completely polymerization, preferred illumination is the sun
Light, time 10min.
The acrylate be one of methyl methacrylate, ethyl methacrylate, cyanacrylate or
It is a variety of, preferably cyanacrylate.The reaction equation in situ of the cyanacrylate is as follows：
In the preparation method of above-mentioned perovskite thin film, the acrylate monomer in perovskite precursor solution can be in illumination
Under the action of and polymerization reaction independently occurs, obtain polymer.The reaction step is simple, easy, is not necessarily to other reaction conditions,
It is easy to industrialize.
During the reaction, acrylate contains C=O functional group and C=C functional group, wherein C=O functional group and calcium titanium
B ion (such as Pb of mine grain boundaries2+、Sn2+、Ge2+Deng) by coordinate bond generation weak interaction, it is passivated grain boundary defects.C simultaneously
=O functional group and B (such as Pb2+、Sn2+、Ge2+Deng) coordination polymer can be made to be effectively adhered grain boundaries, by light
According to processing, polymerization reaction occurs for the C=C functional group in acrylate, thus in grain boundaries formation dense protective layer, blocking water,
The decomposition of oxygen and additional factor to perovskite, improves the stability of perovskite thin film.
The present invention also provides a kind of perovskite solar batteries, hole transmission layer 2, perovskite thin film including lamination setting
3 and electron transfer layer 4, the perovskite thin film 3 includes Ca-Ti ore type ABX3Hybrid inorganic-organic materials and polymer, it is described
Polymer is polymerize to obtain by acrylate monomer.
The perovskite battery further includes substrate 1 and electrode 5.
Specifically, as shown in figure 4, the perovskite solar battery includes the substrate 1 that successively lamination is arranged, hole transport
Layer 2, perovskite thin film 3, electron transfer layer 4 and electrode 5.
The material of the substrate 1 is unlimited, can be any one in silicon wafer, glass, stainless steel substrates.Since ITO is a kind of
Metallic compound with good clear electric conductivity, has that forbidden band is wide, visible range light transmission is high low with resistivity etc.
Characteristic, therefore, the substrate 1 are preferably ITO electro-conductive glass.
The hole transmission layer 2 be poly- [3- (butyric acid methylamine salt) thiophene] (PSCT-N) material layer, with a thickness of 5nm~
20nm, relative to common hole transmission layer PEDOT:The energy level of PSS (energy level 5.11eV), P3CT-N are and selected in 5.26eV
Perovskite CH3NH3PbI3Valence band (5.3eV) more closely, can effectively avoid as energy level mismatch and caused by battery imitate
Rate decline.P3CT-N preferred thickness is 10nm.The chemical structural formula of the P3CT-N is as follows：
The perovskite thin film 3 with a thickness of 400nm~500nm.In view of the balance transmission of carrier, preferred thickness is
450nm。
The electron transfer layer 4 includes the PCBM layer that successively lamination is arranged, C60 layers and BCP layers, PCBM layers of the thickness
For 20nm~50nm, described C60 layers with a thickness of 20nm~40nm, described BCP layers with a thickness of 8nm~10nm, the electronics
Transport layer 4 with a thickness of 50nm~100nm.PCBM is prepared with solwution method spin coating, can effectively be penetrated into and be covered perovskite table
Face cavity that may be present, preferred thickness 20nm；And C60 is prepared by vacuum evaporation, the C60 layer obtained in this way is finer and close
Uniformly, preferred thickness 40nm；And to be then used as hole blocking layer to be able to suppress compound at electrode interface by BCP, improves device
Can, preferred thickness 8nm.
The electrode 5 with a thickness of 100nm~300nm, the material of the electrode 5 is unlimited, but in view of gold be used as electrode
Expensive, silver is short as electrode life, and therefore, the electrode 5 is preferably copper electrode.
Above-mentioned perovskite thin film even compact, without apparent cavity, and perovskite thin film has excellent stability.Cause
This, not only has high transformation efficiency using the perovskite solar battery of above-mentioned perovskite thin film, while also having good steady
It is qualitative.
The present invention also provides a kind of preparation methods of perovskite solar battery.The preparation method comprises the following steps：
One substrate 1 is provided；
Hole transmission layer 2 is formed on the substrate 1；And
Perovskite thin film 3 is formed using the preparation method of above-mentioned perovskite thin film on the hole transmission layer 2；And
Electron transfer layer 4 is formed on the perovskite thin film 3；And
Electrode 5 is formed on the electron transfer layer 4.
The substrate 1 is ITO electro-conductive glass, and the ITO electro-conductive glass is first washed with ITO cleaning agent and deionized water, gone
Except grease and organic matter, deionized water, acetone, isopropanol supersound washing are then successively used, is dried with nitrogen, using oxygen plasma
It is further processed.
The hole transmission layer 2 is P3CT-N material layer, and the P3CT-N material layer is formed using the spin coating of P3CT-N solution,
Revolving speed is 3000 revs/min~4000 revs/min, and the time is 45 seconds~60 seconds.The P3CT-N solution is the methanol of P3CT-N
Solution, the concentration of the P3CT-N are 1mg/mL~5mg/mL.
The electron transfer layer 4 includes the PCBM layer that successively lamination is arranged, C60 layers and BCP layers.The PCBM layers of use
PCBM solution spin coating is formed, and revolving speed is 1500 revs/min~2500 revs/min, and the time is 50 seconds~80 seconds.The PCBM solution
For the chlorobenzene solution of PCBM, the concentration of the PCBM is 10mg/mL~25mg/mL.Described C60 layers and described BCP layers using true
The method of empty hot evaporation is formed.
The electrode 5 is copper electrode, is formed using the method for vacuum thermal evaporation.
The preparation method of above-mentioned perovskite solar battery has the advantages that simple, easy-operating.The obtained perovskite sun
Energy battery has high transformation efficiency and good stability.
Hereinafter, will be by following specific embodiments to the perovskite thin film, perovskite solar battery and its preparation side
Method is described further.
Embodiment 1：
By molar ratio 1:1 PbI2(668.5mg) and CH3NH3The cyanacrylate of I (230.5mg) and 5mg is molten
Solution is 4 in 1mL volume ratio:1 n,N-Dimethylformamide and dimethyl sulfoxide in the mixed solvent, it is molten to obtain perovskite presoma
Liquid.Wherein, PbI2And CH3NH3The concentration of I is 1.45mmol/mL, and the concentration of cyanacrylate is 5mg/mL.
Then perovskite precursor solution being spin-coated on ito glass substrate with sol evenning machine, revolving speed is 4800 revs/min, when
Between be 20 seconds.
It is made annealing treatment 10 minutes at 100 DEG C again, forms perovskite thin film.Perovskite thin film formed after by solar irradiation
Processing polymerize, and light application time is 10 minutes.
Obtained perovskite thin film includes CH3NH3PbI3With the polymer of cyanacrylate, wherein cyanoacrylate
The mass percent of the polymer of acetoacetic ester is 0.5%.
The forward and backward infared spectrum figure of the lighting process of perovskite thin film is as shown in Figure 1.From fig. 1, it can be seen that calcium before lighting process
Cyanacrylate is implicitly present in titanium ore film.And after lighting process, the carbon-carbon double bond peak in perovskite thin film disappears, and says
Bright, cyanacrylate polymerize completely, forms polymer.
Embodiment 2：
By molar ratio 1:1 PbI2(668.5mg) and CH3NH3The cyanacrylate of I (230.5mg) and 3mg is molten
It is 4 that 1mL, which is solved, in volume ratio:1 n,N-Dimethylformamide and dimethyl sulfoxide in the mixed solvent, it is molten to obtain perovskite presoma
Liquid.Wherein, PbI2And CH3NH3The concentration of I is 1.45mmol/mL, and the concentration of cyanacrylate is 3mg/mL.
Then perovskite precursor solution being spin-coated on ito glass substrate with sol evenning machine, revolving speed is 4800 revs/min, when
Between be 20 seconds.
It is made annealing treatment 5 minutes at 100 DEG C again, forms perovskite thin film.Perovskite thin film formed after by solar irradiation
Processing polymerize cyanacrylate therein, and light application time is 30 minutes.
Obtained perovskite thin film includes CH3NH3PbI3With the polymer of cyanacrylate, wherein cyanoacrylate
The mass percent of the polymer of acetoacetic ester is 0.3%.
Embodiment 3：
By molar ratio 1:0.8 PbI2(668.5mg) and CH3NH3The cyanacrylate of I (184.4mg) and 10mg
Being dissolved in 1mL volume ratio is 3:1 n,N-Dimethylformamide and dimethyl sulfoxide in the mixed solvent, obtains perovskite presoma
Solution.Wherein, PbI2And CH3NH3The concentration of I is 1.45mmol/mL, and the concentration of cyanacrylate is 10mg/mL.
Then perovskite precursor solution being spin-coated on ito glass substrate with sol evenning machine, revolving speed is 4800 revs/min, when
Between be 20 seconds.
It is made annealing treatment 8 minutes at 80 DEG C again, forms perovskite thin film.Perovskite thin film formed after by ultraviolet light irradiation
Processing polymerize cyanacrylate therein, and light application time is 5 minutes.
Obtained perovskite thin film includes CH3NH3PbI3With the polymer of cyanacrylate, wherein cyanoacrylate
The mass percent of the polymer of acetoacetic ester is 1%.
Embodiment 4：
By molar ratio 1:1.2 PbI2(668.5mg) and CH3NH3The cyanacrylate of I (276.6mg) and 20mg
Dissolving 1mL in volume ratio is 5:1 n,N-Dimethylformamide and dimethyl sulfoxide in the mixed solvent, obtains perovskite presoma
Solution.Wherein, PbI2And CH3NH3The concentration of I is 1.45mmol/mL, and the concentration of cyanacrylate is 20mg/mL.
Then perovskite precursor solution being spin-coated on ito glass substrate with sol evenning machine, revolving speed is 4800 revs/min, when
Between be 20 seconds.
It is made annealing treatment 10 minutes at 90 DEG C again, forms perovskite thin film.Perovskite thin film formed after through infrared light irradiation
Processing polymerize cyanacrylate therein, and light application time is 20 minutes.
Obtained perovskite thin film includes CH3NH3PbI3With the polymer of cyanacrylate, wherein cyanoacrylate
The mass percent of the polymer of acetoacetic ester is 2%.
Embodiment 5：
By molar ratio 1:1 PbI2(668.5mg) and CH3NH3The methyl methacrylate of I (230.5mg) and 5mg is molten
It is 4 that 1mL, which is solved, in volume ratio:1 n,N-Dimethylformamide and dimethyl sulfoxide in the mixed solvent, it is molten to obtain perovskite presoma
Liquid.Wherein, PbI2And CH3NH3The concentration of I is 1.45mmol/mL, and the concentration of methyl methacrylate is 5mg/mL.
Then perovskite precursor solution being spin-coated on ito glass substrate with sol evenning machine, revolving speed is 4800 revs/min, when
Between be 20 seconds.
It is made annealing treatment 5 minutes at 80 DEG C again, forms perovskite thin film.Perovskite thin film formed after by UV illumination
Processing polymerize methyl methacrylate therein, and light application time is 20 minutes.
Obtained perovskite thin film includes CH3NH3PbI3With the polymer of methyl methacrylate, wherein metering system
The mass percent of the polymer of sour methyl esters is 0.5%.
Embodiment 6
By molar ratio 1:1 PbI2(668.5mg) and CH3NH3The ethyl methacrylate of I (230.5mg) and 5mg is molten
It is 4 that 1mL, which is solved, in volume ratio:1 n,N-Dimethylformamide and dimethyl sulfoxide in the mixed solvent, it is molten to obtain perovskite presoma
Liquid.Wherein, PbI2And CH3NH3The concentration of I is 1.45mmol/mL, and the concentration of ethyl methacrylate is 5mg/mL.
Then perovskite precursor solution being spin-coated on ito glass substrate with sol evenning machine, revolving speed is 4800 revs/min, when
Between be 20 seconds.
It is made annealing treatment 5 minutes at 80 DEG C again, forms perovskite thin film.Perovskite thin film formed after by UV illumination
Processing polymerize ethyl methacrylate therein, and light application time is 20 minutes.
Obtained perovskite thin film includes CH3NH3PbI3With the polymer of ethyl methacrylate, wherein metering system
The mass percent of the polymer of acetoacetic ester is 0.5%.
Embodiment 7：
As shown in fig. 6, perovskite solar battery includes substrate 1, the hole transmission layer 2, perovskite of successively lamination setting
Film 3, electron transfer layer 4 and electrode 5, preparation method is as follows：
It using ITO electro-conductive glass as substrate 1, is first washed with ITO cleaning agent and deionized water, removes grease and organic matter,
Then deionized water, acetone, isopropanol supersound washing are successively used, is dried with nitrogen, is further processed using oxygen plasma.
Hole transmission layer 2 is made using spin-coating method on ITO electro-conductive glass after treatment.Hole transmission layer 2 is P3CT-N
Material layer uses concentration to be formed for the methanol solution spin coating of the P3CT-N of 2mg/mL, and the revolving speed of sol evenning machine is 3500 revs/min,
Time is 45 seconds, with a thickness of 10nm.
Perovskite thin film 3 is made using the preparation method of embodiment 1 on hole transmission layer 2, with a thickness of 450nm.
Electron transfer layer 4 is made on perovskite thin film 3, and concentration is first used to revolve for the chlorobenzene solution of the PCBM of 10mg/mL
It applies and forms a PCBM layers, the revolving speed of sol evenning machine is 2000 revs/min, and the time is 60 seconds, with a thickness of 20nm.Then on PCBM layer
It is formed using the method for vacuum thermal evaporation with a thickness of the C60 layer of 40nm and is formed using the method for vacuum thermal evaporation on C60 layer
With a thickness of the BCP layer of 8nm.
One layer of copper is deposited as electrode 5, with a thickness of 300nm using the method for vacuum thermal evaporation on electron transfer layer 4.
Embodiment 8：
As shown in fig. 6, perovskite solar battery includes substrate 1, the hole transmission layer 2, perovskite of successively lamination setting
Film 3, electron transfer layer 4 and electrode 5, preparation method is as follows：
It using ITO electro-conductive glass as substrate 1, is first washed with ITO cleaning agent and deionized water, removes grease and organic matter,
Then deionized water, acetone, isopropanol supersound washing are successively used, is dried with nitrogen, is further processed using oxygen plasma.
Hole transmission layer 2 is made using spin-coating method on ITO electro-conductive glass after treatment.Hole transmission layer 2 is P3CT-N
Material layer uses concentration to be formed for the methanol solution spin coating of the P3CT-N of 1mg/mL, and the revolving speed of sol evenning machine is 3000 revs/min
Rev/min, the time is 45 seconds, with a thickness of 5nm.
Perovskite thin film 3 is made using the preparation method of embodiment 1 on hole transmission layer 2, with a thickness of 400nm.
Electron transfer layer 4 is made on perovskite thin film 3, and concentration is first used to revolve for the chlorobenzene solution of the PCBM of 15mg/mL
It applies and forms a PCBM layers, the revolving speed of sol evenning machine is 1500 revs/min, and the time is 80 seconds, with a thickness of 30nm.Then on PCBM layer
It is formed using the method for vacuum thermal evaporation with a thickness of the C60 layer of 20nm and is formed using the method for vacuum thermal evaporation on C60 layer
With a thickness of the BCP layer of 10nm.
One layer of copper is deposited as electrode 5, with a thickness of 100nm using the method for vacuum thermal evaporation on electron transfer layer 4.
Embodiment 9：
As shown in fig. 6, perovskite solar battery includes substrate 1, the hole transmission layer 2, perovskite of successively lamination setting
Film 3, electron transfer layer 4 and electrode 5, preparation method is as follows：
It using ITO electro-conductive glass as substrate 1, is first washed with ITO cleaning agent and deionized water, removes grease and organic matter,
Then deionized water, acetone, isopropanol supersound washing are successively used, is dried with nitrogen, is further processed using oxygen plasma.
Hole transmission layer 2 is made using spin-coating method on ITO electro-conductive glass after treatment.Hole transmission layer 2 is P3CT-N
Material layer uses concentration to be formed for the methanol solution spin coating of the P3CT-N of 3mg/mL, and the revolving speed of sol evenning machine is 3600 revs/min,
Time is 60 seconds, with a thickness of 15nm.
Perovskite thin film 3 is made using the preparation method of embodiment 1 on hole transmission layer 2, with a thickness of 460nm.
Electron transfer layer 4 is made on perovskite thin film 3, and concentration is first used to revolve for the chlorobenzene solution of the PCBM of 18mg/mL
It applies and forms a PCBM layers, the revolving speed of sol evenning machine is 1800 revs/min, and the time is 70 seconds, with a thickness of 40nm.Then on PCBM layer
It is formed using the method for vacuum thermal evaporation with a thickness of the C60 layer of 30nm and is formed using the method for vacuum thermal evaporation on C60 layer
With a thickness of the BCP layer of 9nm.
One layer of copper is deposited as electrode 5, with a thickness of 200nm using the method for vacuum thermal evaporation on electron transfer layer 4.
Embodiment 10：
As shown in fig. 6, perovskite solar battery includes substrate 1, the hole transmission layer 2, perovskite of successively lamination setting
Film 3, electron transfer layer 4 and electrode 5, preparation method is as follows：
It using ITO electro-conductive glass as substrate 1, is first washed with ITO cleaning agent and deionized water, removes grease and organic matter,
Then deionized water, acetone, isopropanol supersound washing are successively used, is dried with nitrogen, is further processed using oxygen plasma.
Hole transmission layer 2 is made using spin-coating method on ITO electro-conductive glass after treatment.Hole transmission layer 2 is P3CT-N
Material layer uses concentration to be formed for the methanol solution spin coating of the P3CT-N of 5mg/mL, and the revolving speed of sol evenning machine is 4000 revs/min,
Time is 60 seconds, with a thickness of 20nm.
Perovskite thin film 3 is made using the preparation method of embodiment 1 on hole transmission layer 2, with a thickness of 500nm.
Electron transfer layer 4 is made on perovskite thin film 3, and concentration is first used to revolve for the chlorobenzene solution of the PCBM of 25mg/mL
It applies and forms a PCBM layers, the revolving speed of sol evenning machine is 2500 revs/min, and the time is 80 seconds, with a thickness of 50nm.Then on PCBM layer
It is formed using the method for vacuum thermal evaporation with a thickness of the C60 layer of 40nm and is formed using the method for vacuum thermal evaporation on C60 layer
With a thickness of the BCP layer of 10nm.
One layer of copper is deposited as electrode 5, with a thickness of 150nm using the method for vacuum thermal evaporation on electron transfer layer 4.
Comparative example 1：
Comparative example 1 is identical as 1 condition of embodiment, and difference is only that, cyanogen is free of in the perovskite precursor solution of comparative example 1
Base ethyl acrylate, obtained perovskite thin film are free of the polymer of cyanacrylate.
Fig. 2 is the scanning electron microscope (SEM) photograph of the perovskite thin film of the embodiment of the present invention 1 and comparative example 1, as can be seen from Figure 2, cyano third
The addition of olefin(e) acid ethyl ester can effectively cause the homoepitaxial of perovskite, form fine and close uniform perovskite thin film.Embodiment 1
The perovskite thin film crystalline size arrived is uniform, and film dense uniform, without obvious cavity or crackle；And comparative example 1 obtains
Perovskite thin film crystalline size it is not of uniform size, and have apparent cavity.
Fig. 3 is the steady-state fluorescence spectrogram of the perovskite thin film of the embodiment of the present invention 1 and comparative example 1.As can be seen from Figure 3, cyanogen
The addition of base ethyl acrylate can make the fluorescence spectrum of perovskite thin film that blue shift occur, and show that the defect inside perovskite obtains
Effectively inhibit.
Fig. 4 is the time resolution fluorescence spectral figure of the perovskite thin film of the embodiment of the present invention 1 and comparative example 1.Time resolution
Fluorescence spectrum shows that the addition of cyanacrylate can effectively improve service life of the carrier in perovskite thin film, and then calcium
Battery efficiency can be improved when being applied in perovskite solar battery in titanium ore film.
Fig. 5 is X-ray diffraction (XRD) map comparison diagram of the perovskite thin film of the embodiment of the present invention 1 and comparative example 1.From
Fig. 5 shows it is found that the diffraction maximum of the perovskite thin film containing cyanacrylate does not occur any displacement：Cyano third
The addition of olefin(e) acid ethyl ester can't enter inside the crystal structure of perovskite, and be merely present between its crystal and crystal
Near crystal boundary.
Comparative example 2：
Comparative example 2 is identical as 7 condition of embodiment, and difference is only that, the perovskite thin film of comparative example 2 uses 1 institute of comparative example
Obtained perovskite thin film is free of the polymer of cyanacrylate in perovskite thin film.
The perovskite solar cell device efficiency comparative of embodiment 7 and comparative example 2 is as shown in table 1.
Table 1
Fig. 7 is the aerial stability contrast figure of perovskite solar battery of the embodiment of the present invention 7 and comparative example 2,
Air humidity is：40%~60%.As can be seen from Figure 7, the stability of perovskite solar battery of the invention is obviously improved.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of perovskite thin film, which is characterized in that the perovskite thin film includes Ca-Ti ore type ABX3Hybrid inorganic-organic material
Material and polymer, the polymer are polymerize to obtain by acrylate monomer.
2. perovskite thin film according to claim 1, which is characterized in that the acrylate monomer is methyl methacrylate
One of ester, ethyl methacrylate, cyanacrylate are a variety of.
3. perovskite thin film according to claim 1, which is characterized in that the matter of polymer described in the perovskite thin film
Measuring percentage is 0.3%~2%.
4. perovskite thin film according to claim 1, which is characterized in that the Ca-Ti ore type ABX3Hybrid inorganic-organic material
A is organic amine cation, B Pb in material2+、Sn2+、Ge2+In any one, X be halide anion or SCN-。
5. a kind of preparation method of perovskite thin film, which is characterized in that the preparation method comprises the following steps：
By acrylate monomer, AX and BX2It is dissolved in solvent, obtains perovskite precursor solution；
The perovskite precursor solution is formed in a substrate；
Annealing and lighting process are successively carried out to the substrate with perovskite precursor solution, obtain perovskite thin film；Its
In, the acrylate carries out polymerization reaction during lighting process.
6. the preparation method of perovskite thin film according to claim 5, which is characterized in that the A in the AX is organic amine
Cation, X are halide anion or SCN-；The BX2In B be Pb2+、Sn2+、Ge2+In any one.
7. the preparation method of perovskite thin film according to claim 5, which is characterized in that the temperature of the annealing is
80 DEG C~100 DEG C, the time is 5min~10min.
8. the preparation method of perovskite thin film according to claim 5, which is characterized in that the lighting process is using purple
Outside, the irradiation of infrared or sunlight, time are 5min~30min.
9. a kind of perovskite solar battery, hole transmission layer, perovskite thin film and electron transfer layer including lamination setting,
It is characterized in that, the perovskite thin film includes Ca-Ti ore type ABX3Hybrid inorganic-organic materials and polymer, the polymer by
Acrylate monomer polymerize to obtain.
10. a kind of preparation method of perovskite solar battery, which is characterized in that the preparation method comprises the following steps：
One substrate is provided；
Hole transmission layer is formed over the substrate；And
Perovskite thin film is formed using any preparation method of claim 5~8 on the hole transport layer；And
Electron transfer layer is formed on the perovskite thin film；And
Electrode is formed on the electron transport layer.
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