CN107464882A - A kind of organic inorganic hybridization perovskite solar cell and preparation method thereof - Google Patents
A kind of organic inorganic hybridization perovskite solar cell and preparation method thereof Download PDFInfo
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- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
- H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
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Abstract
The invention discloses a kind of organic inorganic hybridization perovskite solar cell and preparation method thereof.Preparation method of the present invention is to deposit layer of semiconductor compacted zone by spray pyrolysis in transparent conductive electrode;Then mixed-cation organic inorganic hybridization perovskite solution is sprayed on semiconductor compacted zone by hot substrate spraying process, forms one layer of mixed-cation organic inorganic hybridization perovskite thin film light-absorption layer;Again hole transmission layer is prepared in extinction layer surface;Finally using thermal evaporation evaporation gold electrode, organic inorganic hybridization perovskite solar cell is obtained.The present invention prepares organic inorganic hybridization perovskite solar cell using hot substrate spraying process, simplifies preparation technology, can quickly prepare large area perovskite thin film, be advantageous to scale application;And present invention optimizes the ratio between mixed-cation organic inorganic hybridization perovskite solution each component, gained solar cell crystallite dimension is more than 500nm, and stability is preferable.
Description
Technical field
The invention belongs to technical field of solar utilization technique, it is more particularly related to a kind of novel organic-inorganic hybrid
Perovskite solar cell and preparation method thereof.
Background technology
Hybrid inorganic-organic perovskite solar cell (hereinafter referred to as perovskite solar cell) is in numerous new sun electricity
Show one's talent in pond, attracted the concern of numerous researchers, gone back quilt《Science》Ten big sciences in 2013 are chosen as to break through
One of.The light absorbing material that this battery uses is organic-inorganic hybrid ABX3, wherein A is the organic cation of+l valencys, is selected
From methylamine ion (CH3NH3 +), ethamine ion (C2H5NH3 +) or methyl ether ion (NH2CH=NH2 +), B is the+metal ion of divalent,
Selected from Sn2+Or Pb2+, X is halide ion, selected from Cl-、Br-Or I-, it is typical perovskite crystal structure, therefore the battery quilt
Referred to as Ca-Ti ore type solar cell.Because it uses all solid state form, the problem of can both avoiding liquid electrolyte from bringing, again may be used
To obtain high conversion efficiency, its photoelectric transformation efficiency of a few years brings up to 22.1% in 2016 from 3.8% in 2009, this
Kind development speed is unprecedented, and perovskite solar cell has great potentiality and application prospect.
Single cation perovskite material, such as MAPbI3, because crystallinity is poor, cause its stability poor, and
Mixed-cation perovskite material system, such as FAMAPbI3, larger FA+Ionic radius and MA+Compared to showing crystallization power
Superiority on, MA+Incorporation can reduce crystal defect, improve crystallinity.Br mixed-cation perovskite system is mixed,
Such as (FAPbI3)x(MAPbBr3)(1-x), perovskite energy gap can be adjusted by adjusting Br content, further improve perovskite
The light conversion efficiency and its stability of material.
At present, the preparation method of mixed-cation type perovskite absorbed layer mainly has spin-coating method, flash method, is unfavorable for advising greatly
Mould application, and prepared perovskite grain size is no more than 300nm, stability is also poor.
The content of the invention
It is an object of the invention to:Overcome less stable existing for existing perovskite solar cell and crystal grain is no more than
A kind of the defects of 300nm, there is provided organic-nothing that can exceed 500nm with high stability, suitable large-scale production, grain particles
Machine hydridization perovskite solar cell and preparation method thereof.
In order to realize foregoing invention purpose, the invention provides a kind of hybrid inorganic-organic perovskite solar cell
Preparation method, it comprises the following steps:
(1) layer of semiconductor compacted zone is deposited by spray pyrolysis in transparent conductive electrode;
(2) mixed-cation hybrid inorganic-organic perovskite solution is sprayed at step (1) institute by hot substrate spraying process
State on semiconductor compacted zone, form one layer of mixed-cation hybrid inorganic-organic perovskite thin film light-absorption layer;
(3) hole is prepared in step (2) the mixed-cation hybrid inorganic-organic perovskite thin film extinction layer surface to pass
Defeated layer;
(4) using thermal evaporation evaporation gold electrode, hybrid inorganic-organic perovskite solar cell is obtained;
Wherein, the general structure of the hybrid inorganic-organic perovskite is (FAPbI3)x(MAPbBr3)(1-x), x be 0.7~
0.9。
As a kind of optimal technical scheme of the preparation method of hybrid inorganic-organic perovskite solar cell of the present invention,
In step (1), the transparent conductive electrode is fluorine doped tin oxide or Al-Doped ZnO.
As a kind of optimal technical scheme of the preparation method of hybrid inorganic-organic perovskite solar cell of the present invention,
The substrate is substrate of glass or plastic-substrates.
As a kind of optimal technical scheme of the preparation method of hybrid inorganic-organic perovskite solar cell of the present invention,
In step (1), the semiconductor compacted zone is with TiO2, ZnO or SnO2For raw material, deposit to obtain by spray pyrolysis.
As a kind of optimal technical scheme of the preparation method of hybrid inorganic-organic perovskite solar cell of the present invention,
In step (1), the thickness of the semiconductor compacted zone is 30~200nm.
As a kind of optimal technical scheme of the preparation method of hybrid inorganic-organic perovskite solar cell of the present invention,
The preparation method of the mixed-cation hybrid inorganic-organic perovskite solution is by FAI:PbI2:MABr:PbBr2According to mole
Than 0.7~0.9:0.7~0.9:0.1~0.3:0.1~0.3 is mixed to join DMF and dimethyl sulfoxide (DMSO)
In mixed solution, and the mass ratio of DMF and dimethyl sulfoxide (DMSO) is 7~9.5:1.
As a kind of optimal technical scheme of the preparation method of hybrid inorganic-organic perovskite solar cell of the present invention,
In step (2), the concentration of the mixed-cation hybrid inorganic-organic perovskite solution is 0.1~0.5mol/L.
As a kind of optimal technical scheme of the preparation method of hybrid inorganic-organic perovskite solar cell of the present invention,
In step (2), in the hot substrate spraying process, carrier gas is nitrogen, and nebulizer gas pressure is 2~4 atmospheric pressure, and hot substrate temperature is
110~150 DEG C, spray speed is 1~2g/min, and spray time is 10~15s, and annealing temperature is 100~150 DEG C, annealing time 8
~20min.
In order to realize foregoing invention purpose, present invention also offers a kind of hybrid inorganic-organic perovskite solar cell,
It is prepared by above-mentioned preparation method.
Relative to prior art, the present invention has the advantages that:
In the prior art, hybrid inorganic-organic perovskite thin film is to use spin-coating method film forming under an inert atmosphere mostly, difficult
To prepare large area film, and crystallite dimension is mostly in 300nm or so, less stable.The present invention passes through hot substrate spraying process
Hybrid inorganic-organic perovskite thin film is prepared, be can be achieved in atmospheric environment, do not required harsh gaseous environment, reduce
Preparation condition;Obtained hybrid inorganic-organic perovskite thin film is fine and close, and crystallite dimension can exceed 500nm, obtained organic-nothing
Machine hydridization perovskite solar cell photoelectric conversion efficiency is more than 12%, and after preserving 80 days, photoelectric transformation efficiency, which reduces, not to be surpassed
5% is crossed, excellent in stability.
Brief description of the drawings
With reference to the accompanying drawings and detailed description, to hybrid inorganic-organic perovskite solar cell of the present invention and its
Preparation method and beneficial effect are described in detail.
Fig. 1 is the hybrid inorganic-organic perovskite solar battery structure of the present invention, wherein, 1 is transparent conductive electrode
(FTO), 2 be semiconductor compacted zone, and 3 be perovskite light-absorption layer, and 4 be hole transmission layer, and 5 be metal electrode.
Fig. 2 is the (FAPbI of the embodiment of the present invention 23)0.85(MAPbBr3)0.15Organic inorganic hybridization perovskite thin film SEM schemes.
Fig. 3 is the (FAPbI of the embodiment of the present invention 23)0.85(MAPbBr3)0.15Organic inorganic hybridization perovskite solar cell
Preserve the J-V curves of 0 day and 80 days.
Embodiment
In order that the purpose of the present invention, technical scheme and advantageous effects become apparent from, with reference to embodiments, to this
Invention is further elaborated.It should be appreciated that the embodiment described in this specification is just for the sake of this hair of explanation
Bright, being not intended to limit the present invention, the parameter of embodiment, ratio etc. can suit measures to local conditions to make a choice and have no substance to result
Influence.
Embodiment 1
(1) the depositing Ti O in transparent conductive electrode2Compacted zone:By 1g tetraisopropyl titanates be added to 1g acetylacetone,2,4-pentanediones and
TiO is prepared in 3g ethanol solutions2Presoma, under the conditions of 450 DEG C, the thick TiO of 50nm are deposited by spray pyrolysis2Compacted zone.
(2) mixed-cation organic inorganic hybridization perovskite solution is prepared:By mol ratio FAI:PbI2:MABr:PbBr2=
0.70:070:0.30:0.30 mixture is added in DMSO and DMF mixed solution, and DMF and DMSO mass ratio are 9:1, institute
It is 0.3mol/L to obtain mixed-cation organic inorganic hybridization perovskite solution concentration.
(3) in TiO2Perovskite thin film is deposited on compacted zone:Under atmospheric environment, calcium titanium is prepared by hot substrate spraying process
Ore deposit film, wherein carrier gas are N2, spray gun air pressure is 3 atmospheric pressure, and hot substrate temperature is 130 DEG C, controls spray time, film layer thickness
Spend for 200nm, then anneal 15min at 100 DEG C.
(4) by hole transport layer material (Spiro-OMeTAD) under 4000rpm rotating speeds spin-coating film, wherein hole transport
Layer compound method be:72.3mg Spiro-OMeTAD are added in 1ml chlorobenzenes, are stirred to clarify, are then added 28.8ul's
TBP and 17.5ul Li-TFSI solution stirring 1min.
(5) finally using thermal evaporation evaporation 50nm gold electrodes.
Prepared perovskite thin film crystallite dimension is 400nm, and hybrid inorganic-organic perovskite solar cell light is changed
Efficiency is 10.60%, and after 80 days, the photoelectric transformation efficiency of test is 9.57%.
Embodiment 2
(1) the depositing Ti O in transparent conductive electrode2Compacted zone:By 1g tetraisopropyl titanates be added to 1g acetylacetone,2,4-pentanediones and
TiO is prepared in 3g ethanol solutions2Presoma, under the conditions of 450 DEG C, the thick TiO of 50nm are deposited by spray pyrolysis2Compacted zone.
(2) mixed-cation organic inorganic hybridization perovskite solution is prepared:By mol ratio FAI:PbI2:MABr:PbBr2=
0.85:0.85:0.15:0.15 mixture is added in DMSO and DMF mixed solution, and DMF and DMSO mass ratio are 9:1,
Gained mixed-cation organic inorganic hybridization perovskite solution concentration is 0.3mol/L.
(3) in TiO2Perovskite thin film is deposited on compacted zone:Under atmospheric environment, calcium titanium is prepared by hot substrate spraying process
Ore deposit film, wherein carrier gas are N2, spray gun air pressure is 3 atmospheric pressure, and hot substrate temperature is 130 DEG C, controls spray time, film layer thickness
Spend for 200nm, then anneal 15min at 100 DEG C.
(4) by hole transport layer material (Spiro-OMeTAD) under 4000rpm rotating speeds spin-coating film, wherein hole transport
Layer compound method be:72.3mg Spiro-OMeTAD are added in 1ml chlorobenzenes, are stirred to clarify, are then added 28.8ul's
TBP and 17.5ul Li-TFSI solution stirring 1min.
(5) finally using thermal evaporation evaporation 50nm gold electrodes.
Prepared perovskite thin film crystallite dimension is 500nm, and hybrid inorganic-organic perovskite solar cell light is changed
Efficiency is 12.08%, and after 80 days, the photoelectric transformation efficiency of test is 12.36%.
Embodiment 3
(1) the depositing Ti O in transparent conductive electrode2Compacted zone:By 1g tetraisopropyl titanates be added to 1g acetylacetone,2,4-pentanediones and
TiO is prepared in 3g ethanol solutions2Presoma, under the conditions of 450 DEG C, the thick TiO of 50nm are deposited by spray pyrolysis2Compacted zone.
(2) mixed-cation organic inorganic hybridization perovskite solution is prepared:By mol ratio FAI:PbI2:MABr:PbBr2=
0.90:0.90:0.10:0.10 mixture is added in DMSO and DMF mixed solution, and DMF and DMSO mass ratio are 9:1,
Gained mixed-cation organic inorganic hybridization perovskite solution concentration is 0.3mol/L.
(3) in TiO2Perovskite thin film is deposited on compacted zone:Under atmospheric environment, calcium titanium is prepared by hot substrate spraying process
Ore deposit film, wherein carrier gas are N2, spray gun air pressure is 3 atmospheric pressure, and hot substrate temperature is 130 DEG C, controls spray time, film layer thickness
Spend for 200nm, then anneal 15min at 100 DEG C.
(4) by hole transport layer material (Spiro-OMeTAD) under 4000rpm rotating speeds spin-coating film, wherein hole transport
Layer compound method be:72.3mg Spiro-OMeTAD are added in 1ml chlorobenzenes, are stirred to clarify, are then added 28.8ul's
TBP and 17.5ul Li-TFSI solution stirring 1min.
(5) finally using thermal evaporation evaporation 50nm gold electrodes.
Prepared perovskite thin film crystallite dimension is 450nm, and hybrid inorganic-organic perovskite solar cell light is changed
Efficiency is 11.24%, and after 80 days, the photoelectric transformation efficiency of test is 10.75%.
Embodiment 4
Hot substrate temperature is 110 DEG C as different from Example 2, and prepared perovskite thin film crystallite dimension is 300nm,
Hybrid inorganic-organic perovskite solar cell light conversion efficiency is 10.20%, after 80 days, the photoelectric transformation efficiency of test
For 9.32%.
Embodiment 5
Hot substrate temperature is 120 DEG C as different from Example 2, and prepared perovskite thin film crystallite dimension is 350nm,
Hybrid inorganic-organic perovskite solar cell light conversion efficiency is 11.00%, after 80 days, the photoelectric transformation efficiency of test
For 10.37%.
Embodiment 6
Hot substrate temperature is 140 DEG C as different from Example 2, and prepared perovskite thin film crystallite dimension is 500nm,
Hybrid inorganic-organic perovskite solar cell light conversion efficiency is 11.70%, after 80 days, the photoelectric transformation efficiency of test
For 11.22%.
Embodiment 7
Hot substrate temperature is 150 DEG C as different from Example 2, and prepared perovskite thin film crystallite dimension is 450nm,
Hybrid inorganic-organic perovskite solar cell light conversion efficiency is 11.55%, after 80 days, the photoelectric transformation efficiency of test
For 10.48%.
Embodiment 8
Annealing time is 8min as different from Example 2, and prepared perovskite thin film crystallite dimension is 300nm, is had
Machine-inorganic hybridization perovskite solar cell light conversion efficiency is 9.25%, and after 80 days, the photoelectric transformation efficiency of test is
8.18%.
Embodiment 9
Annealing time is 10min as different from Example 2, and prepared perovskite thin film crystallite dimension is 350nm, is had
Machine-inorganic hybridization perovskite solar cell light conversion efficiency is 10.45%, and after 80 days, the photoelectric transformation efficiency of test is
9.37%.
Embodiment 10
Annealing time is 12min as different from Example 2, and prepared perovskite thin film crystallite dimension is 400nm, is had
Machine-inorganic hybridization perovskite solar cell light conversion efficiency is 11.20%, and after 80 days, the photoelectric transformation efficiency of test is
10.91%.
Embodiment 11
Annealing time is 18min as different from Example 2, and prepared perovskite thin film crystallite dimension is 450nm, is had
Machine-inorganic hybridization perovskite solar cell light conversion efficiency is 11.82%, and after 80 days, the photoelectric transformation efficiency of test is
11.21%.
Embodiment 12
Annealing time is 20min as different from Example 2, and prepared perovskite thin film crystallite dimension is 450nm, is had
Machine-inorganic hybridization perovskite solar cell light conversion efficiency is 11.49%, and after 80 days, the photoelectric transformation efficiency of test is
10.85%.
Embodiment 13
DMF as different from Example 2:DMSO=7:1, prepared perovskite thin film crystallite dimension is 300nm, is had
Machine-inorganic hybridization perovskite solar cell light conversion efficiency is 10.47%, and after 80 days, the photoelectric transformation efficiency of test is
9.75%.
Embodiment 14
DMF as different from Example 2:DMSO=8:1, prepared perovskite thin film crystallite dimension is 400nm, is had
Machine-inorganic hybridization perovskite solar cell light conversion efficiency is 10.83%, and after 80 days, the photoelectric transformation efficiency of test is
10.25%.
Embodiment 15
DMF as different from Example 2:DMSO=9.5:1, prepared perovskite thin film crystallite dimension is 500nm, is had
Machine-inorganic hybridization perovskite solar cell light conversion efficiency is 11.53%, and after 80 days, the photoelectric transformation efficiency of test is
11.05%.
Comparative example 1
(1) the depositing Ti O in transparent conductive electrode2Compacted zone:By 1g tetraisopropyl titanates be added to 1g acetylacetone,2,4-pentanediones and
TiO is prepared in 3g ethanol solutions2Presoma, under the conditions of 450 DEG C, the thick TiO of 50nm are deposited by spray pyrolysis2Compacted zone.
(2) mixed-cation organic inorganic hybridization perovskite solution is prepared:By mol ratio FAI:PbI2:MAI=0.85:1:
0.15 mixture is added in DMSO and DMF mixed solution, and DMF and DMSO mass ratio are 9:1, gained mixed-cation has
Machine inorganic hybridization perovskite solution concentration is 0.3mol/L.
(3) in TiO2Perovskite thin film is deposited on compacted zone:Under atmospheric environment, calcium titanium is prepared by hot substrate spraying process
Ore deposit film, wherein carrier gas are N2, spray gun air pressure is 3 atmospheric pressure, and hot substrate temperature is 130 DEG C, controls spray time, film layer thickness
Spend for 200nm, then anneal 15min at 100 DEG C.
(4) by hole transport layer material (Spiro-OMeTAD) under 4000rpm rotating speeds spin-coating film, wherein hole transport
Layer compound method be:72.3mg Spiro-OMeTAD are added in 1ml chlorobenzenes, are stirred to clarify, are then added 28.8ul's
TBP and 17.5ul Li-TFSI solution stirring 1min.
(5) finally using thermal evaporation evaporation 50nm gold electrodes.
Prepared perovskite thin film crystallite dimension is 400nm, and hybrid inorganic-organic perovskite solar cell light is changed
Efficiency is 11.28%, and after 80 days, the photoelectric transformation efficiency of test is 7.36%.
Comparative example 2
(1) the depositing Ti O in transparent conductive electrode2Compacted zone:By 1g tetraisopropyl titanates be added to 1g acetylacetone,2,4-pentanediones and
TiO is prepared in 3g ethanol solutions2Presoma, under the conditions of 450 DEG C, the thick TiO of 50nm are deposited by spray pyrolysis2Compacted zone.
(2) mixed-cation organic inorganic hybridization perovskite solution is prepared:By mol ratio FAI:PbI2:MABr:PbBr2=
0.85:0.85:0.15:0.15 mixture is added in DMSO and DMF mixed solution, and DMF and DMSO mass ratio are 9:1,
Gained mixed-cation organic inorganic hybridization perovskite solution concentration is 0.3mol/L.
(3) in TiO2Perovskite thin film is deposited on compacted zone:In glove box, perovskite thin film is prepared by spin-coating method,
Spin coating rotating speed is 4000r/min, and spin coating perovskite amount of solution is 40ul, spin-coating time 30s, and ether is added dropwise in spin coating process and goes
Except solvent, then anneal 15min at 100 DEG C.
(4) by hole transport layer material (Spiro-OMeTAD) under 4000rpm rotating speeds spin-coating film, wherein hole transport
Layer compound method be:72.3mg Spiro-OMeTAD are added in 1ml chlorobenzenes, are stirred to clarify, are then added 28.8ul's
TBP and 17.5ul Li-TFSI solution stirring 1min.
(5) finally using thermal evaporation evaporation 50nm gold electrodes.
Prepared perovskite thin film crystallite dimension is 300nm, and hybrid inorganic-organic perovskite solar cell light is changed
Efficiency is 10.42%, and after 80 days, the photoelectric transformation efficiency of test is 6.26%.
The solar cell performance parameter of 1 embodiment of table 2
Voc(V) | Jsc(mA/cm2) | FF | PCE | |
0day | 1.08 | 17.83 | 62.7% | 12.08% |
80day | 1.08 | 17.63 | 64.9% | 12.36% |
Note:VocFor open-circuit voltage, JscFor short circuit current, FF is fill factor, curve factor, and PCE is cell photoelectric conversion efficiency.
Each embodiment perovskite solar battery efficiency statistics of table 2
The perovskite solar battery efficiency of 3 comparative example of table 1
The perovskite solar battery efficiency of 4 comparative example of table 2
The announcement and teaching of book according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula carries out appropriate change and modification.Therefore, the invention is not limited in embodiment disclosed and described above, to this
Some modifications and changes of invention should also be as falling into the scope of the claims of the present invention.In addition, although this specification
In used some specific terms, but these terms are merely for convenience of description, do not form any restrictions to the present invention.
Claims (9)
1. a kind of preparation method of hybrid inorganic-organic perovskite solar cell, it is characterised in that comprise the following steps:
(1) layer of semiconductor compacted zone is deposited by spray pyrolysis in transparent conductive electrode;
(2) mixed-cation hybrid inorganic-organic perovskite solution is sprayed at step (1) described half by hot substrate spraying process
On conductor compacted zone, one layer of mixed-cation hybrid inorganic-organic perovskite thin film light-absorption layer is formed;
(3) hole transport is prepared in step (2) the mixed-cation hybrid inorganic-organic perovskite thin film extinction layer surface
Layer;
(4) using thermal evaporation evaporation gold electrode, hybrid inorganic-organic perovskite solar cell is obtained;
Wherein, the general structure of the hybrid inorganic-organic perovskite is (FAPbI3)x(MAPbBr3)(1-x), x is 0.7~0.9.
2. the preparation method of hybrid inorganic-organic perovskite solar cell according to claim 1, it is characterised in that
In step (1), the transparent conductive electrode is fluorine doped tin oxide or Al-Doped ZnO.
3. the preparation method of hybrid inorganic-organic perovskite solar cell according to claim 1, it is characterised in that
The substrate is substrate of glass or plastic-substrates.
4. the preparation method of hybrid inorganic-organic perovskite solar cell according to claim 1, it is characterised in that
In step (1), the semiconductor compacted zone is with TiO2, ZnO or SnO2For raw material, deposit to obtain by spray pyrolysis.
5. the preparation method of hybrid inorganic-organic perovskite solar cell according to claim 4, it is characterised in that
In step (1), the thickness of the semiconductor compacted zone is 30~200nm.
6. the preparation method of hybrid inorganic-organic perovskite solar cell according to claim 1, it is characterised in that
The preparation method of the mixed-cation hybrid inorganic-organic perovskite solution is by FAI:PbI2:MABr:PbBr2According to mole
Than 0.7~0.9:0.7~0.9:0.1~0.3:0.1~0.3 is mixed to join DMF and dimethyl sulfoxide (DMSO)
In mixed solution, and the mass ratio of DMF and dimethyl sulfoxide (DMSO) is 7~9.5:1.
7. the preparation method of hybrid inorganic-organic perovskite solar cell according to claim 6, it is characterised in that
In step (2), the concentration of the mixed-cation hybrid inorganic-organic perovskite solution is 0.1~0.5mol/L.
8. the preparation method of hybrid inorganic-organic perovskite solar cell according to claim 1, it is characterised in that
In step (2), in the hot substrate spraying process, carrier gas is nitrogen, and nebulizer gas pressure is 2~4 atmospheric pressure, and hot substrate temperature is
110~150 DEG C, spray speed is 1~2g/min, and spray time is 10~15s, and annealing temperature is 100~150 DEG C, annealing time 8
~20min.
9. the preparation side of hybrid inorganic-organic perovskite solar cell described in any one claim in claim 1~8
The hybrid inorganic-organic perovskite solar cell that method is prepared.
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