CN103872248B - 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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CN103872248B
CN103872248B CN201410118541.4A CN201410118541A CN103872248B CN 103872248 B CN103872248 B CN 103872248B CN 201410118541 A CN201410118541 A CN 201410118541A CN 103872248 B CN103872248 B CN 103872248B
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CN103872248A (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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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/30—Coordination compounds
    • H10K85/341—Transition metal complexes, e.g. Ru(II)polypyridine complexes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing 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 with conventional fossil fuel and increasingly serious environmental problem, the demand of clean energy resource becomes increasingly Urgently.Solar energy has very big using value as clean energy resource, and develop a kind of electricity conversion height, process is simple, The solar cell of low cost and high stability has great strategic importance.From traditional silicon solar cell more up till now with Dyestuff sensitized solar battery and the third generation solar cell that organic battery is representative are obtained for rapid development, also obtain Some applications.Traditional silion cell comparatively high cost, dye-sensitized cell has a lot of restrictions in technology of preparing, and has Although the simple still stability of machine battery battery structure also there is a problem of very big, so they also exist a lot in industrialization Problem.
Perovskite solar cell is closely quickly growing in two years, has started a research boom in the world.Perovskite Structural material mainly does the effect of light-absorption layer inside battery.Perovskite light absorbent has high carrier mobility, band gap Adjustable, can solution method preparation and the features such as there is high absorption coefficient.So the solar energy with perovskite material as light-absorption layer Battery can obtain very high electricity conversion, and the highest transformation efficiency of document report alreadys exceed 15% in the world at present.Calcium titanium Ore deposit solar cell finally can directly make hull cell again from initial one layer of porous layer support of needs, in industrial metaplasia Very big application prospect is also had on product.
The making of perovskite typically just can complete in 100 degrees centigrade annealing, but either loose structure is still The perovskite battery of planar structure is required for one layer of electron transfer layer, also functions to stop during this layer of electron transfer layer transmission electron synchrotron The compound effect of hole suppression.Most electron transfer layer of tradition is TiO2Film, can reach very high opto-electronic conversion effect Rate (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 reports2012,2, 591.), and TiO here2It is typically necessary four, 500 degree of high temperature sintering.If using low temperature preparation TiO2, due to crystallization Property the problems such as lead to solar cell transformation efficiency relatively far short of what is expected.And have document report TiO2To ultraviolet portion ratio More sensitive, perovskite solar cell unstable mainly TiO under ultraviolet light2(Leijtens, the T. causing; 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 communications2013,4.), more importantly need the TiO of high temperature sintering2Film does almost cannot on flexible substrates.There is one layer of TiO simultaneously2 Film also can absorb a part of light, can affect the absorptivity of the light of perovskite light-absorption layer.On the other hand also there is research ZnO film Do perovskite electron transfer layer, also can obtain good efficiency (Liu, D.; Kelly, T. L., Perovskite solar cells with a planar heterojunction structure prepared using room- temperature solution processing techniques.Nature Photonics2013, 8 , 133- 138.).Although can do on flexible substrates, ZnO electron transfer layer not acid and alkali-resistance, if be really used in industrialized production The long-time stability of middle battery there is also problem, or even is sometimes also possible to react with perovskite.The calcium titanium being had been reported that at present Ore deposit battery is required for one layer of electron transfer layer, and substantially inefficent without electron transfer layer battery, electron-hole recombinations are very Seriously so leading to efficiency very low.
Content of the invention
Problem to be solved by this invention is to provide a kind of low cost and does not need the efficient stable of electron transfer layer Perovskite thin film battery and preparation method thereof.
Technical scheme：
A kind of perovskite thin film photovoltaic cell, passes including the transparent conductive substrate being sequentially overlapped, perovskite light-absorption layer, hole Defeated layer and metal electrode.
Described transparent conductive substrate is FTO or ITO electro-conductive glass.
Described calcium titanium ore bed light-absorption layer is CH3NH3PbI3-xClx（0<x<3, x is real number）Or CH3NH3PbI3Film.
Described hole transmission layer is the 2,2' of 68 mM, 7,7'- tetra- [N, N- bis- (4- methoxyphenyl) amino] -9,9'- Spiral shell two fluorenes（spiro-OMeTAD）, the bis trifluoromethyl sulfonic acid Asia acid amides lithium of 26 mM and the 4- tert .-butylpyridine of 55 mM mixed Close solution.Solvent for use is volume ratio is 10：1 chlorobenzene and the mixture of acetonitrile.
Described electrode is gold electrode or silver electrode.
The preparation method of the present invention above-mentioned perovskite thin film photovoltaic cell, comprises the steps：
（1）First FTO or ITO electro-conductive glass is adopted semiconductor technology to clean, dried up with nitrogen, as electrically conducting transparent lining Bottom；
（2）CH by prior synthesis3NH3I and PbCl2In molar ratio 3：1 or by CH3NH3I and PbI2In molar ratio 1：1 Be dissolved in dimethylformamide, under room temperature stirring 24 hours stand-by；The solution having configured is spin-coated on（1）Prepared is transparent In conductive substrates, form 0.5 to 2 microns of thick perovskite light-absorption layers, then anneal under 100 degrees Celsius；
（3）In the sample surfaces being coated with perovskite light-absorption layer, pass through spin coating with the hole transmission layer solution preparing in advance Method forms one layer of hole transmission layer；
（4）Using evaporation preparation Au or Ag on the sample of good for spin coating hole transmission layer as electrode.
Described hole transmission layer solution is the 2,2' containing 68 mM, 7,7'- tetra- [N, N- bis- (4- methoxyphenyl) ammonia Base] -9,9'- spiral shell two fluorenes（spiro-OMeTAD）, 26 mM bis trifluoromethyl sulfonic acid Asia acid amides lithium and 55 mM the tertiary fourth of 4- The mixed solution of yl pyridines, solvent for use is volume ratio is 10：1 chlorobenzene and the mixture of acetonitrile
The CH using in above-mentioned steps 23NH3The synthetic method of I, comprises the 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 traditional high temperature sintering that needs It is not required that porous layer, perovskite material itself had both done light-absorption layer and had played electronics transmitting effect electron transfer layer, 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 height The complex processes such as temperature sintering, This effectively reduces the cost of manufacture of battery.Flexibility to battery and large area volume to volume Printing preparation have very big impetus.The whole manufacture craft of battery is simple, beneficial to the popularization of technology, particularly also obtains Very high electricity conversion and good device stability, have prospects for commercial application.
Brief description
Fig. 1 is the device junction composition of perovskite thin film solar cell, wherein 1- transparent conductive substrate, and 2 perovskites are inhaled Photosphere, 3- hole transmission layer, 4- metal electrode.
Fig. 2 is the current density voltage curve figure that embodiment 1 is obtained perovskite thin film solar cell.
Fig. 3 is the current density voltage curve figure that embodiment 2 is obtained perovskite thin film solar cell.
Fig. 4 is the current density voltage curve figure that embodiment 3 is obtained perovskite thin film solar cell.
Fig. 5 is the current density voltage curve figure that embodiment 4 is obtained perovskite thin film solar cell.
Fig. 6 is the current density voltage curve figure that embodiment 5 is obtained perovskite thin film solar cell.
Fig. 7 is the current density voltage curve figure that embodiment 6 is obtained perovskite thin film solar cell.
Specific embodiment
Embodiment 1：
1）Cleaning.First FTO Conducting Glass to be carried out, dries up in test.First by electro-conductive glass glass Knife is cut into required size, is first cleaned up with cleaning agent after cutting, then deionized water is rinsed.It is then placed on surpassing Use in acetone, ethanol, deionized water successively in sound wave washer and be cleaned by ultrasonic, finally being dried up with nitrogen can obtain testing needs The clean substrate in the surface wanted.
2）Perovskite solution allocation.By CH3NH3I and PbCl2In molar ratio 3：1 is dissolved in dimethylformamide, room temperature Lower stirring 24 hours stand-by；
3）Prepared by perovskite light-absorption layer.With controlling one layer of 2 microns of thick CH of photoresist spinner rotating speed spin coating on FTO3NH3PbI3- xClxPerovskite light-absorption layer, then anneals 45 minutes under 100 degrees Celsius.
4）Prepared by hole transmission layer.FTO is coated with the film of perovskite light-absorption layer and uses one layer of thing of photoresist spinner spin coating The hole transmission layer solution first preparing（The 2,2' of 68 mM, 7,7'- tetra- [N, N- bis- (4- methoxyphenyl) amino] -9,9'- spiral shell Two fluorenes, the mixed solution of the bis trifluoromethyl sulfonic acid Asia acid amides lithium of 26 mM and the 4- tert .-butylpyridine of 55 mM.Solvent for use Be volume ratio be 10：1 chlorobenzene and the mixture of acetonitrile）.
5）Prepared by electrode.The sample of good for spin coating hole transmission layer is placed in vacuum evaporation apparatus and passes through tungsten filament thermal evaporation Method does one layer of gold electrode.
6）Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.Obtain Photoelectric transformation efficiency parameter is, open-circuit voltage 0.91 V, short-circuit current density 19.96 mA/cm2, fill factor, curve factor 0.50, conversion Efficiency 9.09 %.
Embodiment 2：
1）Cleaning.With embodiment 1.
2）Perovskite solution allocation.With embodiment 1.
3）Prepared by perovskite light-absorption layer.One layer 1.5 microns thick perovskite light-absorption layers of photoresist spinner spin coating are used on FTO, so Anneal 45 minutes under 100 degrees Celsius afterwards.
4）Prepared by hole transmission layer.With embodiment 1.
5）Prepared by electrode.With embodiment 1.
6）Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.Obtain Photoelectric transformation efficiency parameter is, open-circuit voltage 0.99 V, short-circuit current density 21.33 mA/cm2, fill factor, curve factor 0.55, conversion Efficiency 11.55%.
Embodiment 3：
1）Cleaning.With embodiment 1.
2）Perovskite solution allocation.With embodiment 1.
3）Prepared by perovskite light-absorption layer.One layer 1 micron thick perovskite light-absorption layer of photoresist spinner spin coating is used on FTO, then Anneal 45 minutes under 100 degrees Celsius.
4）Prepared by hole transmission layer.With embodiment 1.
5）Prepared by electrode.With embodiment 1.
6）Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.Obtain Photoelectric transformation efficiency parameter is, open-circuit voltage 1.04 V, short-circuit current density 21.35 mA/cm2, fill factor, curve factor 0.61, conversion Efficiency 13.44%.
Embodiment 4：
1）Cleaning.With embodiment 1.
2）Perovskite solution allocation.With embodiment 1.
3）Prepared by perovskite light-absorption layer.One layer 0.5 micron thick perovskite light-absorption layer of photoresist spinner spin coating is used on FTO, so Anneal 45 minutes under 100 degrees Celsius afterwards.
4）Prepared by hole transmission layer.With embodiment 1.
5）Prepared by electrode.With embodiment 1.
6）Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.Obtain Photoelectric transformation efficiency parameter is, open-circuit voltage 1.01 V, short-circuit current density 18.10 mA/cm2, fill factor, curve factor 0.53, conversion Efficiency 9.71%.
Embodiment 5：
1）Cleaning.First ITO Conducting Glass to be carried out, dries up in test.First by electro-conductive glass glass Knife is cut into required size, is first cleaned up with cleaning agent after cutting, then deionized water is rinsed.It is then placed on surpassing Use in acetone, ethanol, deionized water successively in sound wave washer and be cleaned by ultrasonic, finally being dried up with nitrogen can obtain testing needs The clean substrate in the surface wanted.
2）Perovskite solution allocation.With embodiment 1.
3）Prepared by perovskite light-absorption layer.One layer 1 micron thick perovskite light-absorption layer of photoresist spinner spin coating is used on ITO, then Anneal 45 minutes under 100 degrees Celsius.
4）Prepared by hole transmission layer.With embodiment 1.
5）Prepared by Ag electrode.Method is with embodiment 1.
6）Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.Obtain Photoelectric transformation efficiency parameter is, open-circuit voltage 0.67 V, short-circuit current density 17.14 mA/cm2, fill factor, curve factor 0.57, conversion Efficiency 6.60%.
Embodiment 6：
1）Cleaning.With embodiment 1.
2）Perovskite solution allocation.By CH3NH3I and PbI2In molar ratio 1：1 is dissolved in dimethylformamide, under room temperature Stirring 24 hours stand-by；
3）Prepared by perovskite light-absorption layer.One layer of 1 micron of thick CH of photoresist spinner spin coating is used on ITO3NH3PbI3Perovskite is inhaled Photosphere, then anneals 15 minutes under 100 degrees Celsius.
4）Prepared by hole transmission layer.With embodiment 1.
5）Prepared by electrode.With embodiment 1.
6）Test.In AM1.5, active layer effective area is 0.09 cm2Under conditions of battery is tested.Obtain Photoelectric transformation efficiency parameter is, open-circuit voltage 0.39 V, short-circuit current density 9.55 mA/cm2, fill factor, curve factor 0.27, conversion effect Rate 1.01%.
The perovskite thin film battery making on FTO substrate in the present invention is than the perovskite making on ITO substrate Hull cell photoelectricity transformation of ownership efficiency is much higher, and the same perovskite CH making on FTO substrate3NH3PbI3-xClxFilm will Ratio perovskite CH3NH3PbI3The solar cell photoelectric transformation efficiency that film does light-absorption layer exceeds a lot, the optimization of acquisition The perovskite CH of energy3NH3PbI3-xClxThe thickness of film is 1 micron, obtains very high solar cell photoelectric conversion efficiency, whole Except the annealing process that needs when making perovskite light-absorption layer during individual, whole device all make at room temperature it is not necessary to The preparation process of high temperature, in the air stores still at room temperature for process is simple and the repeatable high and solar cell that makes Good performance stability so can be kept, there is the potential application of huge production capacity.The solar cell so made has Excellent performance.This has absolutely proved this perovskite thin film photovoltaic cell in industrialized production such as large area, flexibility and printings The feasibility of middle application.

Claims (7)

1. a kind of perovskite thin film photovoltaic cell not needing electron transfer layer, including the transparent conductive substrate being sequentially overlapped, calcium Titanium ore light-absorption layer, hole transmission layer and metal electrode, described hole transmission layer is the 2,2' of 68 mM, 7,7'- tetra- [N, N- bis- (4- methoxyphenyl) amino] -9,9'- spiral shell two fluorenes, the bis trifluoromethyl sulfonic acid Asia acid amides lithium of 26 mM and the tertiary fourth of 4- of 55 mM The mixed solution of yl pyridines.
2. perovskite thin film photovoltaic cell according to claim 1 is it is characterised in that described transparent conductive substrate is FTO Or ITO conductive substrates.
3. perovskite thin film photovoltaic cell according to claim 1 and 2 is it is characterised in that described perovskite light-absorption layer is CH3NH3PbI3-xClxOr CH3NH3PbI3Film, wherein 0<x<3, x is real number.
4. perovskite thin film photovoltaic cell according to claim 1 and 2 is it is characterised in that described hole transmission layer institute With solvent be volume ratio be 10：1 chlorobenzene and the mixture of acetonitrile.
5. perovskite thin film photovoltaic cell according to claim 1 and 2 is 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 not needing electron transfer layer described in claim 1, its feature exists In comprising the steps：
(1) first FTO or ITO electro-conductive glass is adopted semiconductor technology to clean, dried up with nitrogen, as transparent conductive substrate；
（2）CH by prior synthesis3NH3I and PbCl2In molar ratio 3：1 or by CH3NH3I and PbI2In molar ratio 1：1 dissolving In dimethylformamide, under room temperature stirring 24 hours stand-by；The solution having configured is spin-coated on step（1）Prepared is transparent In conductive substrates, form 0.5 to 2 microns of thick perovskite light-absorption layers, then anneal under 100 degrees Celsius；
（3）In the sample surfaces being coated with perovskite light-absorption layer, pass through spin-coating method shape with the hole transmission layer solution preparing in advance Become one layer of hole transmission layer, described hole transmission layer solution is 2,2', 7,7'- tetra- [N, N- bis- (the 4- methoxyl groups containing 68 mM Phenyl) amino] -9,9'- spiral shell two fluorenes, the bis trifluoromethyl sulfonic acid Asia acid amides lithium of 26 mM and the 4- tert .-butylpyridine of 55 mM Mixed solution, solvent for use is volume ratio is 10：1 chlorobenzene and the mixture of acetonitrile；
（4）On the sample of the good hole transmission layer of spin coating, evaporation preparation Au or Ag is as electrode.
7. preparation method according to claim 6 is it is characterised in that step（2）Described in CH3NH3The synthetic method of I, Comprise the 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 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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