CN104134711B - A kind of preparation method of perovskite solar cell - Google Patents

A kind of preparation method of perovskite solar cell Download PDF

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CN104134711B
CN104134711B CN201410342998.3A CN201410342998A CN104134711B CN 104134711 B CN104134711 B CN 104134711B CN 201410342998 A CN201410342998 A CN 201410342998A CN 104134711 B CN104134711 B CN 104134711B
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陆运章
刘文峰
杨晓生
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CETC 48 Research Institute
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/42Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for sensing infra-red radiation, light, electro-magnetic radiation of shorter wavelength or corpuscular radiation and adapted for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation using organic materials as the active part, or using a combination of organic materials with other material as the active part; Multistep processes for their manufacture
    • H01L51/4213Comprising organic semiconductor-inorganic semiconductor hetero-junctions
    • H01L51/422Majority carrier devices using sensitisation of widebandgap semiconductors, e.g. TiO2
    • H01L51/4226Majority carrier devices using sensitisation of widebandgap semiconductors, e.g. TiO2 the wideband gap semiconductor comprising titanium oxide, e.g. TiO2
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/0001Processes specially adapted for the manufacture or treatment of devices or of parts thereof
    • H01L51/0002Deposition of organic semiconductor materials on a substrate
    • H01L51/0003Deposition of organic semiconductor materials on a substrate using liquid deposition, e.g. spin coating
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
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    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/0032Selection of organic semiconducting materials, e.g. organic light sensitive or organic light emitting materials
    • H01L51/0077Coordination compounds, e.g. porphyrin
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/42Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for sensing infra-red radiation, light, electro-magnetic radiation of shorter wavelength or corpuscular radiation and adapted for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation using organic materials as the active part, or using a combination of organic materials with other material as the active part; Multistep processes for their manufacture
    • H01L51/4213Comprising organic semiconductor-inorganic semiconductor hetero-junctions
    • H01L51/422Majority carrier devices using sensitisation of widebandgap semiconductors, e.g. TiO2
    • H01L51/4233Majority carrier devices using sensitisation of widebandgap semiconductors, e.g. TiO2 the wideband gap semiconductor comprising zinc oxide, e.g. ZnO
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L2251/00Indexing scheme relating to organic semiconductor devices covered by group H01L51/00
    • H01L2251/30Materials
    • H01L2251/301Inorganic materials
    • H01L2251/303Oxides, e.g. metal oxides
    • 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
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    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/549Organic PV cells
    • 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
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    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses a kind of perovskite solar cell and solwution method preparation method thereof.This perovskite solar cell comprises the substrate, transparency electrode, electron transfer layer, light-absorption layer, hole transmission layer and the top electrode that stack gradually, wherein: described light-absorption layer is the photovoltaic material light-absorption layer with perovskite structure.Its electron transfer layer, perovskite material light-absorption layer and hole transmission layer all can realize solwution method preparation under the air ambient of low temperature (less than 200 DEG C); especially electron transfer layer does not need the nano particle that high temperature (more than 450 DEG C) processes or synthesizes; be conducive to simplification of flowsheet; reduce costs; improve the preparation efficiency of battery, accomplish scale production.

Description

A kind of preparation method of perovskite solar cell
Technical field
The invention belongs to technical field of solar batteries, particularly relate to a kind of perovskite solar cell and solwution method preparation method thereof.
Background technology
Solar cell is the device directly light energy conversion being become electric energy by photoelectric effect or Photochemical effects, is also called photovoltaic cell.Along with solar power generation obtains more and more extensive use as a kind of clean energy resource, index request more simple and fast is waited to the preparation technology of solar cell.The preparation technology of conventional solar cells is greatly mainly with monocrystalline silicon or the polysilicon crystal silicon solar energy battery as sunlight absorbing material.Because the type battery exists preparation technology's long flow path, easily there is the problem of cell piece production cycle long, the low output of high investment in the shortcomings such as the high and Preparation equipment costliness of preparation process energy consumption.
Perovskite solar cell is the emerging solar cell of a class, mainly utilizes similar ABX 3(A=CH 3nH 3 +deng; B=Pb 2+, Sn 2+deng; X=Cl -, Br -, I -deng) there is the photovoltaic material of perovskite structure to realize opto-electronic conversion, have that raw material sources is extensive, manufacture craft is simple, price is low, can be prepared into the advantages such as flexible battery.The basic structure of perovskite solar cell comprises substrate, transparency electrode, electron transport material, perovskite material light-absorption layer, hole mobile material and metal electrode.Transform light energy becomes electric energy can be divided into three main process by perovskite solar cell: the photon of (1) certain energy is absorbed by light-absorption layer and produces electron hole pair; (2) there is separation of charge when electron hole pair diffuses to the interface of light absorbent; (3) electronics enters external circuit along electron transport material through electrode, and hole enters external circuit along hole mobile material through electrode, completes the conversion of luminous energy to electric energy by load.
From 2009, document " Kojima; A., Teshima, K.; Shirai; Y. & Miyasaka, T.Organometalhalideperovskitesasvisible-lightsensitizers forphotovoltaiccells.J.Am.Chem.Soc.131,6050 – 6051 (2009). " first reported the light absorbent of perovskite material as solar cell, along with going deep into of research, the efficiency of perovskite solar cell promotes rapidly.2013, document " Burschka, J.etal.Sequentialdepositionasaroutetohigh-performanceper ovskite-sensitizedsolarcells.Nature499, 316 – 319 (2013). " and document " Liu, D., Kelly, T.L.Perovskitesolarcellswithaplanarheterojunctionstructu repreparedusingroom-temperaturesolutionprocessingtechniq ues.Naturephotonics342, (2013). " report efficient perovskite solar cell respectively, improve the photoelectric conversion efficiency of perovskite solar cell greatly.These perovskite solar cells are all the preparation technologies based on solwution method.This preparation technology is simple to operate, with low cost.But in above-mentioned preparation technology, existence need prepare mesoporous shape titanium oxide layer (TiO 2as electron transfer layer) or the problem such as synthesis of nano grain-like zinc-oxide (ZnO), mesoporous shape TiO 2layer need carry out high temperature (more than 450 DEG C) sintering processes link, and the Nanoparticulate ZnO solution of synthesis can not long-term storage.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, provides a kind of perovskite solar cell and solwution method preparation method thereof.
In order to achieve the above object, technical scheme provided by the invention is:
Described perovskite solar cell is followed successively by substrate, transparent electrode layer, electron transfer layer, light-absorption layer, hole transmission layer and top electrode layer from top to bottom.
Wherein, described backing material is glass or flexiplast; Described transparency electrode layer material is indium tin oxide (ITO, IndiumTinOxide) or fluorine tin-oxide (FTO, FluorineDopedTinOxide); Described electron transport layer materials is electron transport material; Described light-absorption layer material is perovskite structure photovoltaic material; Described hole transport layer material is hole mobile material; Described top electrode layer is metal electrode.
Preferably, described electron transport material is metal oxide; Described perovskite structure photovoltaic material is ABX 3the organic inorganic hybridization perovskite of type crystal structure; Described hole mobile material is organic material or inorganic material.
Described metal oxide is TiO 2or ZnO.
In described hole mobile material, organic material is Spiro-MeOTAD, and inorganic material is NiO x(x is 1 ~ 1.5), MoO x(x is 2 ~ 3) or V 2o 5in one or more.
Described electric transmission layer thickness is 30 ~ 60nm; Described light-absorption layer thickness is 300 ~ 400nm; Described thickness of hole transport layer is 100 ~ 200nm; Described top electrode layer thickness is 60 ~ 150nm.
The preparation method of above-mentioned solar cell comprises the following steps:
(1) coating electronic transport layer precursor solution on transparent electrode layer, electron transfer layer presoma is dissolved in less than 200 DEG C hydrolysis and forms dense film, and obtained thickness is the electron transfer layer of 30 ~ 60nm;
(2) employing is dissolved with PbI 2dimethyl formamide solution and be dissolved with CH 3nH 3the aqueous isopropanol of I deposits perovskite structure photovoltaic material on the electron transport layer, and obtained thickness is the light-absorption layer of 300 ~ 400nm;
(3) at light-absorption layer surface coating hole mobile material, forming thickness is the hole transmission layer of 100 ~ 200nm;
(4) on hole transmission layer, adopt vacuum thermal evaporation metal electrode method deposit thickness to be the top electrode layer of 60 ~ 150nm.
Below in conjunction with principle and beneficial effect, the invention will be further described:
The present invention is beneficial to industrialization in the future to improve the problems such as above-mentioned high-temperature process, provides a kind of solwution method preparation method of perovskite solar cell.Adopt the perovskite solar cell that the inventive method is prepared; its electron transfer layer, perovskite material light-absorption layer and hole transmission layer all can realize solwution method preparation under air ambient; and do not need the Nanoparticulate zinc oxide that high temperature (more than 450 DEG C) processes or synthesizes; be conducive to simplification of flowsheet; reduce costs; improve the preparation efficiency of battery, accomplish scale production.
The backing material being applicable to perovskite solar cell of the present invention has the transparent material such as glass, flexiplast (PEN, PET).The material of transparency electrode can be the transparent electrode material that indium tin oxide (ITO, IndiumTinOxide), fluorine tin-oxide (FTO, FluorineDopedTinOxide) etc. are conventional.The PEN plastic film of normal employing ITO electro-conductive glass, FTO electro-conductive glass or band ITO is as substrate and transparency electrode, and its square resistance is 10 ~ 50 Ω, and transmitance is 80 ~ 90%.
What in electron transfer layer, electron transport material used was common is metal oxide, as TiO 2, ZnO etc.Electron transfer layer is the film that aggregated metal oxide is formed on the transparent electrodes, is generally the compacted zone of thickness between 10nm ~ 100nm, plays the effect of transmission electronic, prevent electrode from directly contacting with light-absorption layer simultaneously.
Light-absorption layer adopts perovskite crystal preparation, and its effect absorbs incident light.The simple light-absorption layer of device of the present invention is made up of the crystal grain of perovskite material, and thickness is usually at 100 ~ 500nm.Common perovskite material mainly contains similar ABX 3(A=CH 3nH 3 +deng; B=Pb 2+, Sn 2+deng; X=Cl -, Br -, I -deng) the organic inorganic hybridization perovskite of type crystal structure.
Hole transmission layer mainly by hole transport to top electrode, thickness is generally 40 ~ 300nm.Hole mobile material is generally the material with higher hole mobility, and can be organic material and/or inorganic material, organic material be as Spiro-MeOTAD etc., and inorganic material is as NiO x, MoO x, V 2o 5deng.
Top electrode generally adopts the metal material such as gold, silver, copper, aluminium with higher work-functions, and thickness is generally 20 ~ 100nm.The manufacture methods such as vacuum coating, plasma spray coating, sputtering, inkjet printing and solution film forming can be adopted.
The preparation method of solar cell of the present invention is included in the step that clean ITO electro-conductive glass first deposits electron transfer layer, and then prepares one deck hydridization perovskite structure CH on the electron transport layer 3nH 3pbI 3step, then at hydridization perovskite structure CH 3nH 3pbI 3the step of deposition of hole transport layer on layer, the finally step of deposit metal electrodes layer on hole transmission layer; Electron transfer layer, light-absorption layer and hole transmission layer is prepared by solwution method deposition process.
On substrate and transparency electrode, adopt ZnO or TiO 2precursor solution carries out surperficial spin coating and prepares electron transfer layer, and then under the low temperature of 150 DEG C ~ 200 DEG C, hydrolysis forms fine and close ZnO or TiO 2film.It is characterized in that: in air ambient, ZnO or TiO 2precursor solution can form dense film, without the need to high temperature sintering by the low temperature hydrolysis below 200 DEG C.
On the electron transport layer, employing is dissolved with PbI 2dimethyl formamide (N, N-dimethylformamide) solution on above-mentioned substrate, carry out surperficial spin coating, then substrate be soaked in be dissolved with CH 3nH 3in isopropyl alcohol (2-propanol) solution of I, prepare light-absorption layer.It is characterized in that: in air ambient, light-absorption layer is prepared by solwution method deposition process.
On light-absorption layer, adopt chlorobenzene (chlorobenzene) solution being dissolved with Spiro-OMeTAD, or NiO xor MoO xprecursor solution on above-mentioned substrate, carry out surperficial spin coating, prepare hole transmission layer.It is characterized in that: in air ambient, hole transmission layer is prepared by solwution method deposition process.
Finally, by the mode of thermal evaporation or plasma spraying at the silver of above-mentioned deposited on substrates 100nm thickness or gold electrode.
In the preparation technology of current perovskite battery, usually adopt the mesoporous shape TiO needing high temperature (450 DEG C) sintering processes 2layer or need synthesis of nano graininess ZnO etc. as electron transfer layer; or more complicated plasma activated chemical vapour deposition method; and the present invention proposes solwution method preparation technology in the air ambient of low temperature just can complete; be conducive to simplification of flowsheet; reduce costs; improve the preparation efficiency of battery, accomplish scale production.
Accompanying drawing explanation
Fig. 1 is perovskite solar battery structure figure of the present invention; Wherein: 1-glass; 2-ITO; 3-electron transfer layer; 4-light-absorption layer; 5-hole transmission layer; 6-metal electrode.1, substrate, 2, transparent electrode layer, 3, electron transfer layer, 4, light-absorption layer, 5, hole transmission layer, 6, top electrode layer;
Fig. 2 is under AM1.5G illumination, the volt-ampere characteristic of the perovskite material solar cell of embodiment 2 and embodiment 3.Wherein: circle point curve is TiO 2as volt-ampere characteristic during electron transfer layer, closed square curve is that ZnO is as volt-ampere characteristic during electron transfer layer.
embodiment:
embodiment 1
See Fig. 1, described perovskite solar cell is followed successively by substrate 1, transparent electrode layer 2, electron transfer layer 3, light-absorption layer 4, hole transmission layer 5 and top electrode layer 6 from top to bottom.
Wherein, described substrate 1 material is glass or flexiplast; Described transparent electrode layer 2 material is indium tin oxide or fluorine tin-oxide; Described electron transfer layer 3 material is electron transport material; Described light-absorption layer 4 material is perovskite structure photovoltaic material; Described hole transmission layer 5 material is hole mobile material; Described top electrode layer 6 is metal electrode.Described electron transport material is metal oxide; Described perovskite structure photovoltaic material is ABX 3the organic inorganic hybridization perovskite of type crystal structure; Described hole mobile material is organic material or inorganic material.Described electric transmission layer thickness is 30 ~ 60nm; Described light-absorption layer thickness is 300 ~ 400nm; Described thickness of hole transport layer is 100 ~ 200nm; Described top electrode layer thickness is 60 ~ 150nm.
embodiment 2
The preparation method of solar cell described in embodiment 1, comprises the following steps:
Preparation PbI 2solution: PbI 2concentration be 1mol/L, solvent is dimethyl formamide.Preparation CH 3nH 3i solution: concentration 10mg/mL, is dissolved in isopropyl alcohol.Preparation TiO 2precursor solution: butyl titanate (tetra-n-butyltitanate) is dissolved in 2-methyl cellosolve solution after mixing with monoethanolamine by the mol ratio of 1:1.
(1) select sheet resistance 15 Ω/, thickness is 3mm, transmitance be 85% ito glass be backing material;
(2) method of solution spin coating is adopted to be coated with TiO on substrate 2precursor solution, on heating station, 150 DEG C ~ 200 DEG C K cryogenic treatment 30min, obtain the TiO that thickness is about 30-60nm 2film is as electron transfer layer;
(3) spin coating PbI on the substrate depositing electron transfer layer 2solution, after the upper oven dry of 70 DEG C, puts into CH 3nH 3soak about 40 seconds in I solution, substrate color becomes brownish black rapidly, is put in clean isopropyl alcohol after taking-up, washes away unnecessary CH 3nH 3i, the heating station being finally placed on 70 DEG C dries 10min, obtains the CH that thickness is 350nm 3nH 3pbI 3the light-absorption layer of perovskite material;
(4) be 0.17mol/L in the surperficial spin coating hole mobile material Spiro-MeOTAD(concentration of light-absorption layer, solvent is chlorobenzene), form the hole transmission layer that thickness is about 100-200nm;
(5) adopt the mode of vacuum thermal evaporation metal electrode on hole transmission layer, deposit the thick top electrode layer of 60-150nm.
Implementation result: the performance test finally carrying out battery, at AM1.5,100mW/cm 2under the irradiation of etalon optical power, the open circuit voltage 0.98V of solar cell sample, short-circuit current density 16.2mA/cm 2, fill factor, curve factor 0.68, conversion efficiency is 10.79%.
embodiment 3
The preparation method of solar cell described in embodiment 1, comprises the following steps:
Preparation PbI 2solution: PbI 2concentration be 1mol/L, solvent is dimethyl formamide.Preparation CH 3nH 3i solution: concentration 10mg/mL, is dissolved in isopropyl alcohol.Preparation ZnO precursor solution: zinc acetate (Zn (Ac) 22H 2o), after mixing with monoethanolamine by the mol ratio of 1:1, be dissolved in 2-methyl cellosolve solution.
4, the preparation of device function layer, see Fig. 1, mainly comprise each functional layer be laminated on glass substrate 1 and transparent ITO electrode 2: electron transfer layer 3, light-absorption layer 4, hole transmission layer 5, and metal electrode 6, preparation process is as follows:
(1) select sheet resistance 15 Ω/, thickness is 3mm, transmitance be 85% ito glass be backing material;
(2) method of solution spin coating is adopted to be coated with TiO on substrate 2precursor solution, on heating station, 150 DEG C ~ 200 DEG C K cryogenic treatment 30min, obtain the TiO that thickness is about 30-60nm 2film is as electron transfer layer;
(3) spin coating PbI on the substrate depositing electron transfer layer 2solution, after the upper oven dry of 70 DEG C, puts into CH 3nH 3soak about 40 seconds in I solution, substrate color becomes brownish black rapidly, is put in clean isopropyl alcohol after taking-up, washes away unnecessary CH 3nH 3i, the heating station being finally placed on 70 DEG C dries 10min, obtains the CH that thickness is 350nm 3nH 3pbI 3the light-absorption layer of perovskite material;
(4) be 0.17mol/L in the surperficial spin coating hole mobile material Spiro-MeOTAD(concentration of light-absorption layer, solvent is chlorobenzene), form the hole transmission layer that thickness is about 100-200nm;
(5) adopt the mode of vacuum thermal evaporation metal electrode on hole transmission layer, deposit the thick top electrode layer of 60-150nm.
Implementation result: the performance test finally carrying out battery, at AM1.5,100mW/cm 2under the irradiation of etalon optical power, the open circuit voltage 0.97V of solar cell sample, short-circuit current density 15.8mA/cm 2, fill factor, curve factor 0.66, conversion efficiency is 10.11%.

Claims (6)

1. a preparation method for perovskite solar cell, described battery is followed successively by substrate (1), transparent electrode layer (2), electron transfer layer (3), light-absorption layer (4), hole transmission layer (5) and top electrode layer (6) from top to bottom; Said method comprising the steps of:
(1) coating electronic transport layer precursor solution on transparent electrode layer, electron transfer layer presoma is dissolved in less than 200 DEG C hydrolysis and forms dense film, and obtained thickness is the electron transfer layer of 30 ~ 60nm;
(2) employing is dissolved with PbI 2dimethyl formamide solution and be dissolved with CH 3nH 3the aqueous isopropanol of I deposits perovskite structure photovoltaic material on the electron transport layer, and obtained thickness is the light-absorption layer of 300 ~ 400nm;
(3) at light-absorption layer surface coating hole mobile material, forming thickness is the hole transmission layer of 100 ~ 200nm;
(4) on hole transmission layer, adopt vacuum thermal evaporation metal electrode method deposit thickness to be the top electrode layer of 60 ~ 150nm.
2. the preparation method of solar cell as claimed in claim 1, it is characterized in that, described substrate (1) material is glass or flexiplast; Described transparent electrode layer (2) material is ITO or FTO; Described electron transfer layer (3) material is electron transport material; Described light-absorption layer (4) material is perovskite structure photovoltaic material; Described hole transmission layer (5) material is hole mobile material; Described top electrode layer (6) is metal electrode.
3. the preparation method of solar cell as claimed in claim 2, it is characterized in that, described electron transport material is metal oxide; Described perovskite structure photovoltaic material is ABX 3the organic inorganic hybridization perovskite of type crystal structure; Described hole mobile material is organic material or inorganic material.
4. the preparation method of solar cell as claimed in claim 3, it is characterized in that, described metal oxide is TiO 2or ZnO.
5. the preparation method of solar cell as claimed in claim 3, it is characterized in that, in described hole mobile material, organic material is Spiro-MeOTAD, and inorganic material is NiO x, MoO xor V 2o 5in one or more, described NiO xin x be 1 ~ 1.5, described MoO xin x be 2 ~ 3.
6. the preparation method of solar cell as claimed in claim 1, it is characterized in that, described electric transmission layer thickness is 30 ~ 60nm; Described light-absorption layer thickness is 300 ~ 400nm; Described thickness of hole transport layer is 100 ~ 200nm; Described top electrode layer thickness is 60 ~ 150nm.
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