CN103872248A - Perovskite thin-film photovoltaic cell and manufacturing method thereof - Google Patents

Perovskite thin-film photovoltaic cell and manufacturing method thereof Download PDF

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CN103872248A
CN103872248A CN201410118541.4A CN201410118541A CN103872248A CN 103872248 A CN103872248 A CN 103872248A CN 201410118541 A CN201410118541 A CN 201410118541A CN 103872248 A CN103872248 A CN 103872248A
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perovskite
layer
cell
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hole transmission
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CN103872248B (en
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方国家
柯维俊
王静
雷红伟
陶洪
刘琴
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Wuhan University WHU
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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
    • H01L51/0032Selection of organic semiconducting materials, e.g. organic light sensitive or organic light emitting materials
    • H01L51/0077Coordination compounds, e.g. porphyrin
    • H01L51/0084Transition metal complexes, e.g. Ru(II)polypyridine complexes
    • 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
    • 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
    • H01L51/44Details of devices
    • H01L51/441Electrodes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/549Organic PV cells
    • 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
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention relates to a perovskite thin-film photovoltaic cell and a manufacturing method of the perovskite thin-film photovoltaic cell. The perovskite thin-film photovoltaic cell is composed of a conducting transparent substrate, a perovskite light-absorbing layer, a hole transfer layer and a metal electrode. The perovskite thin-film photovoltaic cell has the advantages that the structure is quite simple, a traditional electron transfer layer which needs high-temperature sintering is omitted due to the fact that a perovskite material serves as the light-absorbing layer and achieves the electron transfer function, and a porous layer is not needed either; the perovskite material is high in light-absorbing performance, the whole cell is manufactured at a low temperature, the complicated processes such as high-temperature sintering are not needed, and therefore the manufacturing cost of the cell is effectively reduced; the great promotion function is achieved on the flexibility of the cell and the large-sized reel-to-reel printing manufacturing of the cell; the whole manufacturing technology of the cell is simple, the popularization of the technology is facilitated, high photoelectric converting efficiency (approximate to 14 percent) and good device stability are obtained particularly, and therefore the industrial application prospect is achieved.

Description

A kind of perovskite thin film photovoltaic cell and preparation method thereof
Technical field
The present invention relates to a kind of film photovoltaic cell of perovskite structure light absorbent and preparation method thereof, belong to photoelectron material and devices field.
Background technology
Consumption and increasingly serious environmental problem with conventional fossil fuel, the demand of clean energy resource become more and more urgent.Solar energy has very big application value as clean energy resource, and the solar cell for developing a kind of electricity conversion height, simple technique, low cost and high stability has great strategic importance.From traditional silicon solar cell again to rapid development is obtained for by the third generation solar cell of representative of dyestuff sensitized solar battery and organic battery at present, some applications have also been obtained.Comparatively cost is too high for traditional silion cell, and dye-sensitized cell has many limitations in technology of preparing, although and the simple stability of organic battery battery structure also in the presence of it is very big the problem of, so also there are many problems in industrialization in them.
Perovskite solar cell is closely being quickly grown in two years, and a research boom has been started in the world.Perovskite structural material main effect for doing light-absorption layer inside battery.Perovskite light absorbent have high carrier mobility, band gap it is adjustable, can solution method prepare and the features such as with high absorption coefficient.So can obtain very high electricity conversion as the solar cell of light-absorption layer using perovskite material, the highest transformation efficiency of document report alreadys exceed 15% in the world at present.Perovskite solar cell one layer of porous layer support the need for initially finally can directly make hull cell again, also have very big application prospect in industrialized production.
The making of perovskite is general can just to be completed in the annealing of 100 degrees centigrades, but either loose structure or the perovskite battery of planar structure are required for one layer of electron transfer layer, are also functioned to during this layer of electron transfer layer transmission electron synchrotron and stop that hole suppresses compound effect.Most electron transfer layers of tradition are TiO2Film, can reach very high photoelectric transformation efficiency (Kim, H. S.; Lee, C. R.; Im, J. H.; Lee, K. B.; Moehl, T.; Marchioro, A.; Moon, S. J.; Humphry-Baker, R.; Yum, J. H.; Moser, J. E.; Gratzel, M.; Park, N. G., Lead iodide perovskite sensitized all-solid-state submicron thin film mesoscopic solar cell with efficiency exceeding 9%. Scientific reports  2012, 2, 591.), and TiO here2Be typically necessary four, 500 degree of high temperature sintering.If using low temperature preparation TiO2, cause the problems such as due to crystallinity the transformation efficiency of solar cell relative far short of what is expected.And have document report TiO2It is more sensitive to ultraviolet portion, the unstable mainly TiO of perovskite solar cell under ultraviolet light2(Leijtens, the T. caused; Eperon, G. E.; Pathak, S.; Abate, A.; Lee, M. M.; Snaith, H. J., Overcoming ultraviolet light instability of sensitized TiO2 with meso-superstructured organometal tri-halide perovskite solar cells. Nature communications  2013, 4), the TiO of high temperature sintering is more importantly needed2Film is done almost cannot on flexible substrates.There is one layer of TiO simultaneously2Film can also absorb a part of light, can influence the absorptivity of the light of perovskite light-absorption layer.On the other hand also there is research to make perovskite electron transfer layer of ZnO film, can also obtain good efficiency (Liu, D.; Kelly, T. L., Perovskite solar cells with a planar heterojunction structure prepared using room-temperature solution processing techniques. Nature Photonics  2013, 8 (2), 133-138.).Although can do on flexible substrates, ZnO electron transfer layers not acid and alkali-resistance, if be really used in the long-time stability of battery in industrialized production there is also problem, or even be also possible to sometimes can and perovskite reaction.The perovskite battery being had been reported that at present is required for one layer of electron transfer layer, if substantially inefficent without electron transfer layer battery, and electron-hole recombinations are very serious so causing efficiency very low.
The content of the invention
Problem to be solved by this invention is to provide a kind of low cost and does not need perovskite thin film battery of efficient stable of electron transfer layer and preparation method thereof.
Technical scheme:
A kind of perovskite thin film photovoltaic cell, including transparent conductive substrate, perovskite light-absorption layer, hole transmission layer and the metal electrode being sequentially overlapped.
The transparent conductive substrate is FTO or ITO electro-conductive glass.
The calcium titanium ore bed light-absorption layer is CH3NH3PbI3-xClx(0<x<3, x be real number)Or CH3NH3PbI3Film.
Described hole transmission layer is 68 mM 2,2', the fluorenes of 7,7'- tetra- [N, N- bis- (4- methoxyphenyls) amino] -9,9'- spiral shells two(spiro-OMeTAD), the mixed solution of the sub- acid amides lithium of 26 mM bis trifluoromethyl sulfonic acid and 55 mM 4- tert .-butylpyridines.Solvent for use is that volume ratio is 10:Stupid and acetonitrile the mixture of 1 chlorine.
Described electrode is gold electrode or silver electrode.
The preparation method of the above-mentioned perovskite thin film photovoltaic cell of the present invention, comprises the following steps:
(1)First FTO or ITO electro-conductive glass is cleaned using semiconductor technology, is dried up with nitrogen, is used as transparent conductive substrate;
(2)By the CH synthesized in advance3NH3I and PbCl2In molar ratio 3:1 or by CH3NH3I and PbI2In molar ratio 1:1 is dissolved in dimethylformamide, at room temperature stir 24 hours it is stand-by;The solution configured is spin-coated on(1)In the transparent conductive substrate prepared, perovskite light-absorption layer 0.5 to 2 microns thick is formed, is then annealed under 100 degrees Celsius;
(3)In the sample surfaces covered with perovskite light-absorption layer, spin-coating method one layer of hole transmission layer of formation is passed through with the hole transmission layer solution prepared in advance;
(4)Evaporation on the sample of the good hole transmission layer of spin coating is prepared Au or Ag and is used as electrode.
The hole transmission layer solution is the 2,2' containing 68 mM, the fluorenes of 7,7'- tetra- [N, N- bis- (4- methoxyphenyls) amino] -9,9'- spiral shells two(spiro-OMeTAD), the mixed solution of the sub- acid amides lithium of 26 mM bis trifluoromethyl sulfonic acid and 55 mM 4- tert .-butylpyridines, solvent for use is that volume ratio is 10:Stupid and acetonitrile the mixture of 1 chlorine
The CH used in above-mentioned steps 23NH3I synthetic method, comprises the following steps:
(1)Methylamine and HI are 1 in molar ratio:1 reacts two hours under zero degrees celsius;
(2)50 degrees Celsius of lower rotary evaporations 1 ~ 2 hour;
(3)Diethyl ether recrystallization;
(4)60 degrees Celsius of dryings 24 hours in baking oven, form dry white powder.
The perovskite thin film photovoltaic cell device structure of the present invention is extremely simple, eliminates the electron transfer layer of high temperature sintering the need for tradition, it is not required that porous layer, perovskite material had both done light-absorption layer or played electronics transmitting effect in itself, so not needing electron transfer layer.Here perovskite material has very strong absorption to light, and whole battery is also low temperature preparation, it is not necessary to which the complex process such as high temperature sintering, This effectively reduces the cost of manufacture of battery.Prepared by the printing of flexibility and large area volume to volume to battery have very big impetus.The whole manufacture craft of battery is simple, beneficial to the popularization of technology, very high electricity conversion and good device stability is particularly have also obtained, with prospects for commercial application.
Brief description of the drawings
Fig. 1 is the device junction composition of perovskite thin film solar cell, wherein 1- transparent conductive substrates, 2-perovskite light-absorption layer, 3- hole transmission layers, 4- metal electrodes.
Fig. 2 is the current density voltage curve figure that perovskite thin film solar cell is made in embodiment 1.
Fig. 3 is the current density voltage curve figure that perovskite thin film solar cell is made in embodiment 2.
Fig. 4 is the current density voltage curve figure that perovskite thin film solar cell is made in embodiment 3.
Fig. 5 is the current density voltage curve figure that perovskite thin film solar cell is made in embodiment 4.
Fig. 6 is the current density voltage curve figure that perovskite thin film solar cell is made in embodiment 5.
Fig. 7 is the current density voltage curve figure that perovskite thin film solar cell is made in embodiment 6.
Embodiment
Embodiment 1:
1)Cleaning.First FTO Conducting Glass is cleaned, be dried up in experiment.Electro-conductive glass is cut into required size with glass cutter first, first cleaned up with cleaning agent after cutting, then use deionized water rinsing.It is then placed in ultrasonic cleaner to spend successively in acetone, ethanol, ionized water and is cleaned by ultrasonic, finally being dried up again with nitrogen can obtains testing the clean substrate in the surface needed.
2)Perovskite solution allocation.By CH3NH3I and PbCl2In molar ratio 3:1 is dissolved in dimethylformamide, at room temperature stir 24 hours it is stand-by;
3)It is prepared by perovskite light-absorption layer.With one layer of 2 microns of thick CH of control photoresist spinner rotating speed spin coating on FTO3NH3PbI3-xClxPerovskite light-absorption layer, then anneals 45 minutes under 100 degrees Celsius.
4)It is prepared by hole transmission layer.The hole transmission layer solution prepared in advance with one layer of photoresist spinner spin coating on film covered with perovskite light-absorption layer on FTO(The mixed solution of the fluorenes of 68 mM 2,2', 7,7'- tetra- [N, N- bis- (4- methoxyphenyls) amino] -9,9'- spiral shells two, the 26 mM sub- acid amides lithium of bis trifluoromethyl sulfonic acid and 55 mM 4- tert .-butylpyridines.Solvent for use is that volume ratio is 10:Stupid and acetonitrile the mixture of 1 chlorine).
5)It is prepared by electrode.The sample of the good hole transmission layer of spin coating is placed in vacuum evaporation apparatus one layer of gold electrode is done by the method for tungsten filament thermal evaporation.
6)Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.The photoelectric transformation efficiency parameter of acquisition is, the V of open-circuit voltage 0.91, the mA/cm of short-circuit current density 19.962, fill factor, curve factor 0.50, the % of conversion efficiency 9.09.
Embodiment 2:
1)Cleaning.Be the same as Example 1.
2)Perovskite solution allocation.Be the same as Example 1.
3)It is prepared by perovskite light-absorption layer.With the perovskite light-absorption layer that photoresist spinner spin coating one layer is 1.5 microns thick on FTO, then annealed 45 minutes under 100 degrees Celsius.
4)It is prepared by hole transmission layer.Be the same as Example 1.
5)It is prepared by electrode.Be the same as Example 1.
6)Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.The photoelectric transformation efficiency parameter of acquisition is, the V of open-circuit voltage 0.99, the mA/cm of short-circuit current density 21.332, fill factor, curve factor 0.55, conversion efficiency 11.55%.
Embodiment 3:
1)Cleaning.Be the same as Example 1.
2)Perovskite solution allocation.Be the same as Example 1.
3)It is prepared by perovskite light-absorption layer.With the perovskite light-absorption layer that photoresist spinner spin coating one layer is 1 micron thick on FTO, then annealed 45 minutes under 100 degrees Celsius.
4)It is prepared by hole transmission layer.Be the same as Example 1.
5)It is prepared by electrode.Be the same as Example 1.
6)Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.The photoelectric transformation efficiency parameter of acquisition is, the V of open-circuit voltage 1.04, the mA/cm of short-circuit current density 21.352, fill factor, curve factor 0.61, conversion efficiency 13.44%.
Embodiment 4:
1)Cleaning.Be the same as Example 1.
2)Perovskite solution allocation.Be the same as Example 1.
3)It is prepared by perovskite light-absorption layer.With the perovskite light-absorption layer that photoresist spinner spin coating one layer is 0.5 micron thick on FTO, then annealed 45 minutes under 100 degrees Celsius.
4)It is prepared by hole transmission layer.Be the same as Example 1.
5)It is prepared by electrode.Be the same as Example 1.
6)Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.The photoelectric transformation efficiency parameter of acquisition is, the V of open-circuit voltage 1.01, the mA/cm of short-circuit current density 18.102, fill factor, curve factor 0.53, conversion efficiency 9.71%.
Embodiment 5:
1)Cleaning.First ITO Conducting Glass is cleaned, be dried up in experiment.Electro-conductive glass is cut into required size with glass cutter first, first cleaned up with cleaning agent after cutting, then use deionized water rinsing.It is then placed in ultrasonic cleaner to spend successively in acetone, ethanol, ionized water and is cleaned by ultrasonic, finally being dried up again with nitrogen can obtains testing the clean substrate in the surface needed.
2)Perovskite solution allocation.Be the same as Example 1.
3)It is prepared by perovskite light-absorption layer.With the perovskite light-absorption layer that photoresist spinner spin coating one layer is 1 micron thick on ITO, then annealed 45 minutes under 100 degrees Celsius.
4)It is prepared by hole transmission layer.Be the same as Example 1.
5)It is prepared by Ag electrodes.Method be the same as Example 1.
6)Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.The photoelectric transformation efficiency parameter of acquisition is, the V of open-circuit voltage 0.67, the mA/cm of short-circuit current density 17.142, fill factor, curve factor 0.57, conversion efficiency 6.60%.
Embodiment 6:
1)Cleaning.Be the same as Example 1.
2)Perovskite solution allocation.By CH3NH3I and PbI2In molar ratio 1:1 is dissolved in dimethylformamide, at room temperature stir 24 hours it is stand-by;
3)It is prepared by perovskite light-absorption layer.1 micron of thick CH of photoresist spinner spin coating one layer is used on ITO3NH3PbI3Perovskite light-absorption layer, then anneals 15 minutes under 100 degrees Celsius.
4)It is prepared by hole transmission layer.Be the same as Example 1.
5)It is prepared by electrode.Be the same as Example 1.
6)Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.The photoelectric transformation efficiency parameter of acquisition is, the V of open-circuit voltage 0.39, the mA/cm of short-circuit current density 9.552, fill factor, curve factor 0.27, conversion efficiency 1.01%.
The perovskite thin film battery made on FTO substrates in the present invention is more much higher than the perovskite thin film cell photoelectric transformation of ownership efficiency made on ITO substrates, and the same perovskite CH made on FTO substrates3NH3PbI3-xClxFilm is than perovskite CH3NH3PbI3The solar cell photoelectric transformation efficiency that film does light-absorption layer is higher by a lot, the perovskite CH of the optimization performance of acquisition3NH3PbI3-xClxThe thickness of film is 1 micron, obtain very high solar cell photoelectric conversion efficiency, except the annealing process needed when making perovskite light-absorption layer in whole process, whole device all makes at room temperature, the preparation process of high temperature is not needed, the solar cell that technique is simple and repeatability is high and makes is stored in air at room temperature still can keep good performance stability, the potential application with huge production capacity.The solar cell so made has excellent performance.This has absolutely proved the feasibility that this perovskite thin film photovoltaic cell is applied in the industrialized productions such as large area, flexible and printing. 

Claims (8)

1. a kind of perovskite thin film photovoltaic cell, including transparent conductive substrate, perovskite light-absorption layer, hole transmission layer and the metal electrode being sequentially overlapped.
2. perovskite solar cell according to claim 1, it is characterised in that the transparent conductive substrate is FTO or ITO conductive substrates.
3. perovskite solar cell according to claim 1 or claim 2, it is characterised in that the calcium titanium ore bed light-absorption layer is CH3NH3PbI3-xClxOr CH3NH3PbI3Film.
4. perovskite solar cell according to claim 1 or claim 2, it is characterized in that, described hole transmission layer is the 2 of 68 mM, 2', 7,7'- tetra- [N, N- bis- (4- methoxyphenyls) amino] -9, the mixed solution of the fluorenes of 9'- spiral shells two, the 26 mM sub- acid amides lithium of bis trifluoromethyl sulfonic acid and 55 mM 4- tert .-butylpyridines, solvent for use is that volume ratio is 10:1 chlorobenzene and the mixture of acetonitrile.
5. perovskite solar cell according to claim 1 or claim 2, it is characterised in that described metal electrode is gold electrode or silver electrode.
6. the preparation method of the perovskite thin film photovoltaic cell described in claim 1, it is characterised in that comprise the following steps:
(1)First FTO or ITO electro-conductive glass is cleaned using semiconductor technology, is dried up with nitrogen, is used as transparent conductive substrate;
(2)By the CH synthesized in advance3NH3I and PbCl2In molar ratio 3:1 or by CH3NH3I and PbI2In molar ratio 1:1 is dissolved in dimethylformamide, at room temperature stir 24 hours it is stand-by;The solution configured is spin-coated on(1)In the transparent conductive substrate prepared, perovskite light-absorption layer 0.5 to 2 microns thick is formed, is then annealed under 100 degrees Celsius;
(3)In the sample surfaces covered with perovskite light-absorption layer, spin-coating method one layer of hole transmission layer of formation is passed through with the hole transmission layer solution prepared in advance;
(4)Evaporation on the sample of the good hole transmission layer of spin coating is prepared Au or Ag and is used as electrode.
7. preparation method according to claim 6, it is characterized in that, the hole transmission layer solution is 2 containing 68 mM, 2', 7,7'- tetra- [N, N- bis- (4- methoxyphenyls) amino] -9, the mixed solution of the fluorenes of 9'- spiral shells two, the 26 mM sub- acid amides lithium of bis trifluoromethyl sulfonic acid and 55 mM 4- tert .-butylpyridines, solvent for use is that volume ratio is 10:Stupid and acetonitrile the mixture of 1 chlorine.
8. the preparation method according to claim 6 or 7, it is characterised in that step(2)Described in CH3NH3I synthetic method, comprises the following steps:
(1)Methylamine and HI are 1 in molar ratio:1 reacts two hours under zero degrees celsius;
(2)50 degrees Celsius lower rotary evaporation 1-2 hours;
(3)Diethyl ether recrystallization;
(4)60 degrees Celsius of dryings 24 hours in baking oven, form dry white powder.
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