CN105449104A - Perovskite solar cell with stable performance in air environment and preparation method of perovskite solar cell - Google Patents

Perovskite solar cell with stable performance in air environment and preparation method of perovskite solar cell Download PDF

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Publication number
CN105449104A
CN105449104A CN201510916410.5A CN201510916410A CN105449104A CN 105449104 A CN105449104 A CN 105449104A CN 201510916410 A CN201510916410 A CN 201510916410A CN 105449104 A CN105449104 A CN 105449104A
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layer
solar cell
perovskite
perovskite solar
stable performance
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张青红
熊浩
芮一川
王宏志
李耀刚
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Donghua University
National Dong Hwa University
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    • 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
    • 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
    • H10K85/40—Organosilicon compounds, e.g. TIPS pentacene
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2102/00—Constructional details relating to the organic devices covered by this subclass
    • 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
    • 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
    • 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

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  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Photovoltaic Devices (AREA)

Abstract

The invention relates to a perovskite solar cell with stable performance in an air environment and a preparation method of the perovskite solar cell. The solar cell sequentially comprises a conductive base, an electron blocking layer, an electron transport layer, a perovskite sensitization layer, a hydrophobic interface layer, a hole transport layer and a metal layer from bottom to top. The preparation method comprises the following steps: depositing the electron blocking layer and the electron transport layer on the conductive base; depositing the perovskite sensitization layer; depositing the hydrophobic interface layer; depositing the hole transport layer; and depositing the metal layer. According to the perovskite solar cell provided by the invention, the stability of the perovskite cell in air is obviously improved.

Description

Perovskite solar cell of a kind of stable performance in air ambient and preparation method thereof
Technical field
The invention belongs to perovskite solar cell and preparation field thereof, perovskite solar cell of particularly a kind of stable performance in air ambient and preparation method thereof.
Background technology
Perovskite solar cell due to the photoelectric effect of its excellence rapid in the development of recent years, its photoelectric conversion efficiency is more than 20%, and sensitizing layer is as thin as less than 1 micron, and noble metal dosage is few, causes and pays close attention to widely.But this battery, due to more responsive to the moisture light irradiation in environment, easily decomposes; The stability of a lot of research groups to this perovskite-like has done some researchs at present, one deck alumina flake is modified after adopting the modes such as ald, although the method can improve the hydrophobicity of perovskite preferably, this method depends on expensive equipment.Other groups side chain of one deck silane that utilized the hydrophobic performance of silane at perovskite surface graft, change the hydrophily on perovskite surface, but effect is not also given prominence to.
Summary of the invention
Technical problem to be solved by this invention is to provide perovskite solar cell of a kind of stable performance in air ambient and preparation method thereof, and this perovskite solar cell property stable in the air is good; This preparation method adopts super-hydrophobic silicon fluoride to cover perovskite surface, forms one deck hydrophobic interfaces layer, thus protects calcium titanium ore bed to greatest extent from all directions, obtain the perovskite solar cell of stable performance on perovskite sensitizing layer surface and side.
The perovskite solar cell of a kind of stable performance in air ambient of the present invention, comprises: conductive substrates, electronic barrier layer, electron transfer layer, perovskite sensitizing layer, hydrophobic interfaces layer, hole transmission layer and metal level from the bottom to top successively.
Described conductive substrates is FTO electro-conductive glass or ITO-PET; Electronic barrier layer is TiO 2compacted zone, thickness is 60-100nm; Electron transfer layer is TiO 2mesoporous layer, thickness is 300-500n.
Described perovskite sensitizing layer is CH 3nH 3pbX 3, thickness is 300-500nm; Hydrophobic interfaces layer is silicon fluoride, and thickness is 10nm-20nm; Hole transmission layer is Spiro-OMeTAD, and thickness is 60-120nm; Metal level is Au electrode, and thickness is 60-120nm; Wherein, X is at least one in I and Br.
Described silicon fluoride is ten trifluoro octyl group trimethoxy silanes, at least one in ten trifluoro octyltri-ethoxysilane or 17 fluorine decyl trimethoxy silanes.
The preparation method of the perovskite solar cell of a kind of stable performance in atmosphere of the present invention, comprising: conductive substrates deposits electronic barrier layer and electron transfer layer, deposition perovskite sensitizing layer, depositing hydrophobic boundary layer, deposition of hole transport layer and depositing metal layers.
Described electro-conductive glass deposits electronic barrier layer and electron transfer layer, deposition perovskite sensitizing layer, deposition of hole transport layer adopt is spin-coating method, what depositing metal layers adopted is thermal evaporation coating method.
Described depositing hydrophobic boundary layer comprises:
(1) prepare the silicon fluoride/aqueous isopropanol of 0.5-2wt%, prehydrolysis 30-90 minute at 60-80 DEG C, obtains the silicon fluoride aqueous isopropanol that alkoxyl changes silicone hydroxyl into;
(2) in glove box, by the molten painting of silicon fluoride isopropyl alcohol in step (1) or dip-coating on perovskite sensitizing layer.
In described step (2), spin coating speed is 5000-7000rpm, and the time is 30-60s.
The technical solution adopted in the present invention is as follows:
One, the preparation of electronic barrier layer and electron transfer layer
In the tin oxide glass (FTO) of mixing fluorine, the TiO of spin coating one deck 60-100nm 2barrier layer, and then at TiO 2spin coating one deck TiO on barrier layer 2mesoporous layer, finally sinters 30-60min at 450-500 DEG C.Its thickness is 300-500nm;
Two, solwution method prepares organic inorganic hybridization calcium titanium ore bed
In glove box, by the perovskite precursor solution spin coating that configures on the electron transport layer, then annealing in process on hot plate.
Three, solwution method prepares hydrophobic interfaces layer
(1) prehydrolysis of hydrophobic interfaces layer
Getting silicon fluoride is dissolved in isopropyl alcohol, and the silicon fluoride aqueous isopropanol of preparation 0.5-2wt%, prehydrolysis 30-90 minute at 60-80 DEG C, obtains the silicon fluoride aqueous isopropanol that alkoxyl changes silicone hydroxyl into.
(2) preparation of hydrophobic interfaces layer
In glove box, by the silicon fluoride aqueous isopropanol spin coating that configures or dip-coating on perovskite sensitizing layer, spin coating speed is 5000-7000rpm, 30-60s.In glove box, by silicon fluoride aqueous isopropanol spin coating good for configured in advance or dip-coating on sensitizing layer.
Four, the preparation of hole transmission layer
In glove box, the Spiro-OMeTAD solution configured is spun on hydrophobic interfaces layer, placement of then spending the night in atmospheric environment;
Five, the preparation of metal level
Mask is put in the substrate prepared, and then put into vacuum vapor plating instrument, vacuum degree is less than 3 × 10 -3, the metal electrodes such as evaporation one deck Ag, Au.
In order to improve the aerial stability of perovskite system material; for the restriction of background technology Instrumental equipment and the defect of other decorative materials; the present invention adopts super-hydrophobic silicon fluoride to cover perovskite surface; one deck hydrophobic interfaces layer is formed on perovskite sensitizing layer surface and side; thus protect calcium titanium ore bed to greatest extent from all directions, provide a kind of preparation method of perovskite solar cell of stable performance.
For the sensitiveness of perovskite system material to moisture, the present invention starts with from the decomposition principle of perovskite, proposes a kind of new thinking to change the structure of perovskite solar cell, introduces hydrophobic interfaces layer between sensitizing layer and hole transmission layer.The introducing of hydrophobic interfaces layer to battery just sweep and anti-hysteresis effect of sweeping has obvious inhibitory action, it is more stable that the perovskite solar cell containing this layer shows in the environment of high humility.
Due to perovskite CH 3nH 3pbX 3(X=I; Br) be easily subject to the impact of moisture in atmosphere and decompose, after adding silicon fluoride hydrophobic interfaces layer, significantly enhance the aerial stability of perovskite battery, and just sweeping of perovskite battery also obviously disappearing with anti-hysteresis effect of sweeping.
beneficial effect
Silicon fluoride hydrophobic in the present invention covers calcium titanium ore bed surface, forms one deck super-hydrophobic layer, thus protect calcium titanium ore bed to greatest extent from all directions on perovskite surface and side.The silicon fluoride layer of insulation can not only stop electronics in calcium titanium ore bed and Spiro-OMeTAD hole-recombination, also due to the super-hydrophobicity of its strand, the effect of isolation moisture can be played, in conjunction with this properties of materials, effectively improve organic inorganic hybridization perovskite battery stability in the environment and photoelectric characteristic; And meet the labile characteristic of water for perovskite material, when preparing silicon fluoride hydrophobic interfaces layer, specialized designs adopts isopropyl alcohol as solvent and catalyst, instead of the mixed liquor of the water usually adopted and ethanol is as solvent and reactant, the method also considers quantum tunneling effect, reduce silicon fluoride thickness as far as possible, while raising stability test, ensure that the efficiency of battery remains efficient.
Accompanying drawing explanation
Fig. 1 is the structural representation of the perovskite solar cell of stable performance in atmosphere in the present invention;
Fig. 2 exposes lower battery efficiency to scheme over time in atmosphere in embodiment 1;
Fig. 3 exposes lower battery efficiency to scheme over time in atmosphere in embodiment 2;
Fig. 4 exposes lower battery efficiency to scheme over time in atmosphere in embodiment 3.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
1, select FTO glass as substrate, use cleaning agent, acetone, ethanol purge successively, then dry.
2, electronic barrier layer and electron transfer layer
Butyl titanate and ethylenediamine is water-soluble, in ethanol, be prepared into TiO 2 sol, be spin-coated in FTO substrate, rotating speed is 4000r.p.m, time is 30s, then 80 DEG C of dry 5min in thermal station, titania slurry dilution in ethanol, is spin-coated in the FTO substrate containing TiO 2 sol, rotating speed is 4000r.p.m, time is 30s, then 120 DEG C of annealing 5min, and the electron transfer layer then prepared sinters 30min at 500 DEG C.
3, CH 3nH 3pbI 3the preparation of calcium titanium ore bed
(1) CH is synthesized 3nH 3i
The round-bottomed flask filling 30ml methylamine alcohol solution is placed in the frozen water of 0 DEG C, the dropping limit, hydroiodic acid limit of 33ml is stirred in flask, is added dropwise to complete rear continuation and reacts 2h in ice-water bath, form water white CH 3nH 3i solution; Solution Rotary Evaporators evaporate to dryness at 80 DEG C obtains white crystal, then uses washed with diethylether, obtains lily CH 3nH 3i crystal.
(2) preparation of sensitizing layer
Be the PbI of 1:3 by the ratio of molal quantity 2powder and CH 3nH 3i crystal mixed dissolution in the DMF (DMF) of 1ml, and stirs 12 hours at 70 DEG C, obtains the CH of 40wt% 3nH 3pbI 3precursor solution, then filters, in glove box, by perovskite precursor solution CH with filtering head 3mH 3pbI 3on the electron transport layer, rotating speed is 3000r.p.m in spin coating, and the time is 30s, then at 100 DEG C, heats 10min.
4, the preparation of hydrophobic interfaces layer
Getting ten trifluoro octyltri-ethoxysilane is dissolved in isopropyl alcohol, then at 80 DEG C, 30min is heated, obtain the silicon fluoride aqueous isopropanol of the alcoholysis of 0.5wt%, in glove box, the silicon fluoride aqueous isopropanol of alcoholysis is spin-coated on perovskite sensitizing layer, rotating speed is 6000r.p.m, and the time is 30s.
5, the preparation of hole transmission layer
In glove box, get 80mgSpiro-OMeTAD (2,2 ', 7,7 '-four [N, N-bis-(4-methoxyphenyl) be amino]-9,9 '-spiral shell two fluorenes), 15 μ lLi-TESI acetonitrile solutions (500mg/mLLi-TFSI (two (trimethyl fluoride sulfonyl) lithium) is dissolved in acetonitrile), 28.8 μ l4-tert .-butylpyridine are dissolved in the chlorobenzene solution of 1ml, obtain hole transmission layer solution.Be spun on hydrophobic interfaces layer by the hole transmission layer solution prepared, rotating speed is 3000r.p.m, 30s, and the sample prepared is placed in atmospheric environment the 6-8h that spends the night.
6, the preparation of metal level
Vacuum chamber vacuum degree reaches 3 × 10 -3after Pa, the layer gold that hot evaporation 80nm is thick on above-mentioned sample, the effective area of battery is 0.4cm × 0.4cm.
Implementation result: the performance test finally carrying out battery, at AM1.5,100mW/cm 2test under etalon optical power, then perovskite battery storage (humidity is 50%) in atmospheric environment, over time as shown in Figure 2, as can be seen from the figure the efficiency of perovskite solar cell maintained 8% more than 200 hours to perovskite solar cell sample.
Embodiment 2
1, select FTO glass as substrate, use cleaning agent, acetone, ethanol purge successively, then dry.
2, the preparation of electronic barrier layer and electron transfer layer
With step 2 in embodiment 1
3, CH 3nH 3pbI 3the preparation of calcium titanium ore bed
With step 3 in embodiment 1
4, the preparation of hydrophobic interfaces layer
Getting ten trifluoro octyltri-ethoxysilane is dissolved in isopropyl alcohol, then at 80 DEG C, heats 30min, obtains the silicon fluoride solution of the alcoholysis of 1wt%, in glove box, be spin-coated on calcium titanium ore bed by the silicon fluoride solution of alcoholysis, rotating speed is 6000r.p.m, and the time is 30s.
5, the preparation of hole transmission layer
With step 5 in embodiment 1.
6, the preparation of metal level
With step 6 in embodiment 1.
Implementation result: the performance test finally carrying out battery, at AM1.5,100mW/cm 2test under etalon optical power, then perovskite battery storage (humidity is 50%) in atmospheric environment, over time as shown in Figure 3, as can be seen from the figure the efficiency of perovskite solar cell maintained 10% more than 300 hours to perovskite solar cell sample.
Embodiment 3
1, select FTO glass as substrate, use cleaning agent, acetone, ethanol purge successively, then dry.
2, the preparation of electronic barrier layer and electron transfer layer
With step 2 in embodiment 1
3, CH 3nH 3pbI 3the preparation of calcium titanium ore bed
With step 3 in embodiment 1
4, the preparation of hydrophobic interfaces layer
Getting ten trifluoro octyltri-ethoxysilane is dissolved in isopropyl alcohol, then at 80 DEG C, heats 30min, obtains the silicon fluoride solution of the alcoholysis of 2wt%, in glove box, be spin-coated on calcium titanium ore bed by the silicon fluoride solution of alcoholysis, rotating speed is 6000r.p.m, and the time is 30s.
5, the preparation of hole transmission layer
With step 5 in embodiment 1.
6, the preparation of metal level
With step 6 in embodiment 1.
Implementation result: the performance test finally carrying out battery, at AM1.5,100mW/cm 2test under etalon optical power, then perovskite battery storage (humidity is 50%) in atmospheric environment, over time as shown in Figure 4, as can be seen from the figure the efficiency of perovskite solar cell maintained 10% more than 400 hours to perovskite solar cell sample.

Claims (7)

1. a perovskite solar cell for stable performance in air ambient, is characterized in that, comprise successively from the bottom to top: conductive substrates, electronic barrier layer, electron transfer layer, perovskite sensitizing layer, hydrophobic interfaces layer, hole transmission layer and metal level.
2. the perovskite solar cell of a kind of stable performance in air ambient according to claim 1, it is characterized in that, described conductive substrates is FTO electro-conductive glass or ITO-PET; Electronic barrier layer is TiO 2compacted zone, thickness is 60-100nm; Electron transfer layer is TiO 2mesoporous layer, thickness is 300-500n.
3. the perovskite solar cell of a kind of stable performance in air ambient according to claim 1, it is characterized in that, described perovskite sensitizing layer is CH 3nH 3pbX 3, thickness is 300-500nm; Hydrophobic interfaces layer is silicon fluoride, and thickness is 10nm-20nm; Hole transmission layer is Spiro-OMeTAD, and thickness is 60-120nm; Metal level is Au electrode or Ag electrode, and thickness is 60-120nm; Wherein, X is at least one in I and Br.
4. the perovskite solar cell of a kind of stable performance in air ambient according to claim 3, it is characterized in that, described silicon fluoride is ten trifluoro octyl group trimethoxy silanes, at least one in ten trifluoro octyltri-ethoxysilane, 17 fluorine decyl trimethoxy silanes.
5. a preparation method for the perovskite solar cell of stable performance in atmosphere, comprising: conductive substrates deposits electronic barrier layer and electron transfer layer, deposition perovskite sensitizing layer, depositing hydrophobic boundary layer, deposition of hole transport layer and depositing metal layers.
6. the preparation method of the perovskite solar cell of a kind of stable performance in atmosphere according to claim 5, is characterized in that, described depositing hydrophobic boundary layer comprises:
(1) silicon fluoride is dissolved in isopropyl alcohol, is mixed with the silicon fluoride aqueous isopropanol of 0.5-2wt%, prehydrolysis 30-90 minute at 60-80 DEG C, obtain the silicon fluoride aqueous isopropanol that alkoxyl changes silicone hydroxyl into;
(2) in glove box, by silicon fluoride aqueous isopropanol spin coating in step (1) or dip-coating on perovskite sensitizing layer.
7. the preparation method of the perovskite solar cell of a kind of stable performance in atmosphere according to claim 6, is characterized in that, in described step (2), spin coating speed is 5000-7000rpm, and the time is 30-60s.
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CN106058061A (en) * 2016-07-18 2016-10-26 武汉大学 Hydrophobic perovskite solar cell and preparation method and application thereof
CN106340590A (en) * 2016-09-30 2017-01-18 中国科学院上海硅酸盐研究所 Perovskite solar battery and preparation method thereof
CN106410046A (en) * 2016-12-12 2017-02-15 吉林大学 Perovskite solar cell containing hydrophilic electrode modification layer and preparation method
CN106981574A (en) * 2017-04-18 2017-07-25 陈胜红 A kind of long-life perovskite photovoltaic cell and preparation method thereof
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KR101890595B1 (en) * 2017-06-21 2018-08-22 울산과학기술원 A solar cell having enhanced endurance and method for preparing the same
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CN110785473A (en) * 2017-06-23 2020-02-11 住友化学株式会社 Composition, film, laminated structure, light-emitting device, and display
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Application publication date: 20160330