CN110048000A - A kind of electron transfer layer being passivated calcium titanium ore bed surface defect is inverted perovskite structure and its preparation method and application - Google Patents
A kind of electron transfer layer being passivated calcium titanium ore bed surface defect is inverted perovskite structure and its preparation method and application Download PDFInfo
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- CN110048000A CN110048000A CN201910209515.5A CN201910209515A CN110048000A CN 110048000 A CN110048000 A CN 110048000A CN 201910209515 A CN201910209515 A CN 201910209515A CN 110048000 A CN110048000 A CN 110048000A
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- electron transfer
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- 230000027756 respiratory electron transport chain Effects 0.000 title claims abstract description 60
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 230000007547 defect Effects 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 18
- MCEWYIDBDVPMES-UHFFFAOYSA-N [60]pcbm Chemical group C123C(C4=C5C6=C7C8=C9C%10=C%11C%12=C%13C%14=C%15C%16=C%17C%18=C(C=%19C=%20C%18=C%18C%16=C%13C%13=C%11C9=C9C7=C(C=%20C9=C%13%18)C(C7=%19)=C96)C6=C%11C%17=C%15C%13=C%15C%14=C%12C%12=C%10C%10=C85)=C9C7=C6C2=C%11C%13=C2C%15=C%12C%10=C4C23C1(CCCC(=O)OC)C1=CC=CC=C1 MCEWYIDBDVPMES-UHFFFAOYSA-N 0.000 claims abstract description 10
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 5
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims description 21
- 238000000137 annealing Methods 0.000 claims description 20
- 239000011521 glass Substances 0.000 claims description 16
- 229910005855 NiOx Inorganic materials 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229920000144 PEDOT:PSS Polymers 0.000 claims description 2
- 229920001167 Poly(triaryl amine) Polymers 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 230000005525 hole transport Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 238000002161 passivation Methods 0.000 abstract description 7
- 230000006798 recombination Effects 0.000 abstract description 7
- 238000005215 recombination Methods 0.000 abstract description 7
- 238000001338 self-assembly Methods 0.000 abstract description 7
- 230000001737 promoting effect Effects 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 93
- 239000000243 solution Substances 0.000 description 56
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical group CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 32
- 238000004528 spin coating Methods 0.000 description 19
- 239000010408 film Substances 0.000 description 14
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 8
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 8
- 229910052726 zirconium Inorganic materials 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- GRPQBOKWXNIQMF-UHFFFAOYSA-N indium(3+) oxygen(2-) tin(4+) Chemical compound [Sn+4].[O-2].[In+3] GRPQBOKWXNIQMF-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 5
- MWVTWFVJZLCBMC-UHFFFAOYSA-N 4,4'-bipyridine Chemical group C1=NC=CC(C=2C=CN=CC=2)=C1 MWVTWFVJZLCBMC-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- MVPPADPHJFYWMZ-IDEBNGHGSA-N chlorobenzene Chemical group Cl[13C]1=[13CH][13CH]=[13CH][13CH]=[13CH]1 MVPPADPHJFYWMZ-IDEBNGHGSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
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- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
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- 238000011160 research Methods 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- RELMFMZEBKVZJC-UHFFFAOYSA-N 1,2,3-trichlorobenzene Chemical class ClC1=CC=CC(Cl)=C1Cl RELMFMZEBKVZJC-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000012296 anti-solvent Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010129 solution processing Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical group ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 description 1
- DHDHJYNTEFLIHY-UHFFFAOYSA-N 4,7-diphenyl-1,10-phenanthroline Chemical compound C1=CC=CC=C1C1=CC=NC2=C1C=CC1=C(C=3C=CC=CC=3)C=CN=C21 DHDHJYNTEFLIHY-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 150000004816 dichlorobenzenes Chemical class 0.000 description 1
- -1 during spin coating Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- WZAPMUSQALINQD-UHFFFAOYSA-M potassium;ethenyl sulfate Chemical compound [K+].[O-]S(=O)(=O)OC=C WZAPMUSQALINQD-UHFFFAOYSA-M 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
-
- 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
- H10K30/80—Constructional details
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- 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
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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
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- 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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- Engineering & Computer Science (AREA)
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- Electromagnetism (AREA)
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- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Photovoltaic Devices (AREA)
Abstract
The present invention relates to electron transfer layer, inversion perovskite structures and its preparation method and application that one kind can be passivated calcium titanium ore bed surface defect.The electron transfer layer is made of electron transport layer materials and passivator, and the passivator is distributed in electron transport layer materials；The electron transfer layer is PCBM, nano zine oxide or nano-cerium oxide；The passivator is one or more of 2,2 bipyridyls, 4,4 bipyridyls, phenanthroline or EDTA.Specific passivator is distributed in electron transfer layer provided by the invention, these passivator have the characteristics that self assembly, it can combine automatically on perovskite surface, effectively passivation perovskite surface defect, weaken charge recombination, when electron transfer layer being coated on calcium titanium ore bed, and then solar battery is made, solar battery efficiency can be effectively improved, for promoting the commercialization process of perovskite solar battery to be of great significance.
Description
Technical field
The invention belongs to technical field of solar batteries, and in particular to one kind can be passivated the electronics of calcium titanium ore bed surface defect
Transport layer, inversion perovskite structure and its preparation method and application.
Background technique
Hybrid inorganic-organic perovskite solar cell, have absorb that strong, mobility is high, carrier lifetime is long and can it is low at
The potential advantages such as this solution processing, become the new important research direction of field of solar energy utilization.Currently, its laboratory small area device
The energy conversion efficiency of part is improved from 3.8% (J.Am.Chem.Soc., 2009,131,6050-6051) of report in 2009
To 22.1% (NREL, Best Research-Cell Efficiencies, http://www.nrel.gov, accessed:
November 2016), the energy conversion efficiency of module device up to 8.7% (Energy Environ.Sci.2014,7,
2642), become most potential solar cell technology.Perovskite has very regular crystal structure.The excellent performance of perovskite
Also this structure is derived from, but many problems also occur from this aspect.That is the defect inside perovskite crystal with surface
It will be greatly reduced the performance of perovskite.However, there is many researchs to concentrate on these sides in the defect inside processing perovskite at present
Method has limitation for the impact of performance for improving perovskite.Really the defect processing inside perovskite and Morphological control have very heavy
The status wanted, but the defect processing on perovskite surface is also that cannot ignore.Charge is passed because perovskite surface is born
Defeated to next layer of challenge, this largely affects the efficiency of battery, and is surface-treated and does not interfere with generally
Structure and pattern inside perovskite will be helpful to further increase solar battery effect in combination with upper surface defect passivation
Rate.
Therefore, the technology that calcium titanium ore bed surface defect can be passivated by developing one kind has important research significance and using valence
Value.
Summary of the invention
It is an object of the invention to overcome to be improved mainly for the defect inside perovskite in the prior art, and improve
Effect has limited defect and deficiency, provides a kind of electron transfer layer that can be passivated calcium titanium ore bed surface defect.The present invention
Specific passivator is distributed in the electron transfer layer of offer, these passivator have the characteristics that self assembly, can combine automatically in calcium
Titanium ore surface is effectively passivated perovskite surface defect, weakens charge recombination, when being made into solar battery, can effectively improve
Solar battery efficiency.
Another object of the present invention is to provide the preparation methods of above-mentioned electron transfer layer.
Another object of the present invention is to provide a kind of inversion perovskite structures.
Another object of the present invention is to provide above-mentioned inversion perovskite structure preparation methods.
Another object of the present invention is to provide above-mentioned inversion perovskite structures to prepare the application in solar battery.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of electron transfer layer being passivated calcium titanium ore bed surface defect, is made of electron transport layer materials and passivator,
The passivator is distributed in electron transport layer materials；The electron transfer layer is PCBM, nano zine oxide or nano-cerium oxide；
The passivator is one or more of 2,2 bipyridyls, 4,4 bipyridyls, phenanthroline or EDTA.
Specific passivator is distributed in electron transfer layer provided by the invention, these passivator have the characteristics that self assembly,
It can combine automatically on perovskite surface, effectively be passivated perovskite surface defect, weaken charge recombination, electron transfer layer is coated in
On calcium titanium ore bed, and then when solar battery is made, solar battery efficiency can be effectively improved, for promoting perovskite solar energy
The commercialization process of battery is of great significance.
It such as to realize roll-to-roll industrialized production, following condition need to be met: the 1. requirement of solution processing；2. annealing temperature is low
(volume, flexible substrates cannot the bear high temperature) time is short；3. not needing individually to prepare passivation layer solution, saving of work and time, step is reduced,
Increase yields；4. self assembly acts on, dosage is few, reduces waste, economical and practical；5. solvent is cheap and easily-available, low toxicity).
Perovskite surface can be realized merely with the electron transfer layer that there is originally, without increasing additional layer in the present invention
The passivation of defect can meet the requirement of the roll-to-roll printing technology of the following high throughput.
The amount of passivator can according to actual needs and the quantity of perovskite surface defect etc. carries out selection optimization.
Passivator can be both uniformly distributed in electron transfer layer, can also be with uneven distribution.
Currently, uneven distribution is relatively easy to realize.
Preferably, the mass concentration that the passivator is distributed in electron transport layer materials is gradually increased by side to the other side
Add.
Preferably, the electron transfer layer is set on calcium titanium ore bed.
Under normal circumstances, when electron transfer layer is set on calcium titanium ore bed, the mass concentration of passivator is from top to bottom successively
Increase.
Preferably, the perovskite structure of the calcium titanium ore bed is ABX3, wherein one or both of A Pb, Sn, B are
One or more of MA, FA, Cs, X ClpBrqI3-p-q, the value range of p, q are 0~3.
It is further preferable that the perovskite structure of the calcium titanium ore bed is (FAPbI3)0.85(MAPbBr3)0.15、 CsPbI2Br
Or MAPbI3。
Most preferably, the perovskite structure of the calcium titanium ore bed is (FAPbI3)0.85(MAPbBr3)0.15Organic-inorganic is miscellaneous
Change structure.
Preferably, the mass ratio of the electron transport layer materials and passivator is 20~400:1.
It is further preferable that the mass ratio of the electron transport layer materials and passivator is 200:1.
The preparation method of above-mentioned electron transfer layer, includes the following steps:
S1: electron transport layer materials, passivator and solvent are mixed into obtain mixed solution；
S2: mixed solution is spin-coated on calcium titanium ore bed, is annealed up to the electron transfer layer.
Method provided by the invention can realize distribution of the passivator in electron transfer layer, during spin coating, solvent
It gradually volatilizees, so that distributed density of the passivator in electron transfer layer is sequentially increased from top to bottom.Passivator has certainly
Assembly features can combine automatically on perovskite surface, effectively be passivated perovskite surface defect, weaken charge recombination.
In addition, method provided by the invention is simple and easy, the dosage of passivator is small.
Annealing temperature and time can be determined that spin coating generally before the anneal terminates rear film base by thin-film material and solvent
This has been dried, and leather hard has formed, and annealing is to fix and dispel residual solvent to prevent next layer of solution
It destroys.
Preferably, the temperature of the annealing is 40~55 DEG C, and the time is 3~5min.
There can be one or more steps annealing according to different types of perovskite, it can be common that two steps, the first step keep solvent slow
Volatilization makes film densification initial crystallization, and second step high temperature promotes crystallization complete.
Preferably, the number of the spin coating and annealing is twice, alternately by spin coating, annealing, spin coating, annealing.
(spin coating obtains calcium titanium ore bed on ito glass, and then spin coating obtains electricity again for using ito glass as basal layer
Sub- transport layer), spin coating principle is to inhale ito glass on rotating basis with vacuum pump vacuum, it opens rotation redundant solution and gets rid of,
The solution that leaves forms one layer of uniform nano thin-film, and usually leather hard is annealed drying, but when can also extend rotation
Between obtain relatively dry film (adjust revolving speed it is thinner to control the faster film of film thickness, solution concentration is diluter, and film is thinner, and two o'clock is common
Effect obtains suitable film thickness.
Preferably, the concentration of electron transport layer materials is 10~30mg/mL in the mixed solution.
It is further preferable that the concentration of electron transport layer materials is 20mg/mL in the mixed solution.
Preferably, the concentration of passivator is 0.03~5mg/mL in the mixed solution.
It is further preferable that the concentration of passivator is 0.05mg/mL in the mixed solution.
Preferably, the solvent is one or more of chlorobenzene, dichloro-benzenes, trichloro-benzenes or chloroform.
Above-mentioned solvent, especially to the PCBM material of indissoluble, has preferable dissolubility to electron transport layer materials.
A kind of inversion perovskite structure, comprises the following structure from the bottom to top: transparency conducting layer, cathode interface layer, perovskite
Layer, the electron transfer layer and to electrode.
The present invention provides a kind of inversion perovskite structure, and wherein electron transfer layer selects specific electronics provided by the invention
Transport layer, remainder layer select the layer of this field routine.
Preferably, the transparency conducting layer is ITO electro-conductive glass piece, FIO glass or transparent nano silver wire electrode.
Preferably, the hole transmission layer is NiOx, PEDOT:PSS or PTAA.
Preferably, described is silver electrode, gold electrode or aluminium electrode to electrode.
Preferably, the electron transfer layer and to being additionally provided with cathode interface layer between electrode.
The setting of cathode interface layer can reduce the work function of metal electrode, so that the open-circuit voltage of battery improves, improve electricity
Pond performance.The cathode interface layer of this field routine is used equally in the present invention.
It is further preferable that the cathode interface layer is acetylacetone,2,4-pentanedione zirconium layer or BPhen.
Inversion perovskite structure provided by the invention can be prepared or be handled according to conventional methods in the art.
For example, transparency conducting layer can carry out 5~20min of oxygen plasma treatment, solution can be conducive to increase surface and existed
Transparency conducting layer infiltration.
Cathode interface layer, calcium titanium ore bed, electron transfer layer can be obtained by spin coating, annealing.
Electrode can be obtained by vapor deposition.
Above-mentioned inversion perovskite structure prepare in solar battery application it is also within the scope of the present invention.
Compared with prior art, the invention has the following beneficial effects:
Specific passivator is distributed in electron transfer layer provided by the invention, these passivator have the characteristics that self assembly,
It can combine automatically on perovskite surface, effectively be passivated perovskite surface defect, weaken charge recombination, be made into inversion perovskite
When structure and solar battery, solar battery efficiency can be effectively improved, for promoting the commercialization of perovskite solar battery
Process is of great significance.
Detailed description of the invention
Fig. 1 is the schematic diagram of upside-down mounting perovskite structure；(a) in contain cathode interface layer, (b) in be free of cathode interface layer；
Fig. 2 be the embodiment of the present invention 1 (sample 3, a), the calcium titanium ore bed fluorescent emission that provides of embodiment 2 (b) and comparative example 1
Spectrum test curve；
Fig. 3 is the test philosophy of XPS depth profiling test；
Fig. 4 is the self assembly schematic diagram of 4,4 bipyridyl of passivator in the embodiment of the present invention 1 (sample 3)；
The electric current for the perovskite solar battery that Fig. 5 is the embodiment of the present invention 1 (sample 1,2,3)~4 and comparative example 1 provides
Density-voltage curve.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.These embodiments are merely to illustrate the present invention rather than limitation
The scope of the present invention.Test method without specific conditions in lower example embodiment usually according to this field normal condition or is pressed
The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market
The raw materials and reagents that approach obtains.The variation for any unsubstantiality that those skilled in the art is done on the basis of the present invention
And replacement belongs to scope of the present invention.
Embodiment 1
The present embodiment provides a kind of perovskite device (being inverted perovskite structure), such as Fig. 1, specific structure ITO/NiOx/
Perovskite (PVSK, calcium titanium ore bed, (FAPbI3)0.85(MAPbBr3)0.15)/electron transfer layer/acetylacetone,2,4-pentanedione zirconium/Ag.Its
Preparation method is as follows.
(1) pre-treatment of transparency conducting layer
It is 15 Ω square by resistance–1Tin indium oxide (ITO) electro-conductive glass piece successively through deionized water, acetone, washing
Agent, deionized water and ethyl alcohol pass through ultrasonic cleaning, every each 20min of step.
(2) configuration of perovskite precursor liquid
The solution A of 1.5mol/L lead iodide and 1.376mol/L FAI is prepared, solvent for use is DMF:DMSO 4:1 (volume
Than).
The B solution of 1.5mol/L lead bromide and 1.376mol/L MABr is prepared, solvent for use is DMF:DMSO 4:1.
Prepare 1.5mol/L cesium iodide, solvent DMOS.
It takes solution A and B solution to mix (A:B 0.85:0.15, volume ratio) and obtains C solution, C liquor capacity is then added
5% 1.5mol/L cesium iodide solution, obtain perovskite solution.
(3) electron transfer layer solution is prepared
PCBM solution concentration is 20 milligrams every milliliter, and solvent is chlorobenzene, and 4,4 bipyridyls are added, and is configured to 0.05 milli respectively
Gram every milliliter (being denoted as sample 1), 0.1 milligram every milliliter (being denoted as sample 2), the 4 of 1 milligram every milliliter (being denoted as sample 3), 4 pyrroles
Pyridine solution is to get electron transfer layer Solutions Solution.
(4) preparation of cathode interface layer solution
2 milligrams every milliliter of acetylacetone,2,4-pentanedione zirconium, solvent is ethyl alcohol.
(5) preparation of perovskite device
After drying ito glass in an oven, handled 4 minutes using PLASMA (oxygen plasma).Then above-mentioned processed
Ito glass on piece, spin coating layer of Ni OxFilm, thickness are about 10nm, 120 DEG C of annealing 20min.In the glove box of nitrogen atmosphere
In perovskite precursor liquid is spin-coated on NiOxOn layer.Spincoating conditions, 1000 turns of first segment 10 seconds, 5000 turns of 15 seconds Shi Chong of second segment
Anti-solvent chlorobenzene turns 10 seconds again, stops to sol evenning machine, is placed on 100 DEG C of 40~60min of annealing of thermal station, electron transfer layer solution 2500
Turn 30 seconds, 50 DEG C of annealing 5min.4000 turns of spin coating acetylacetone,2,4-pentanedione zirconium 60 seconds.It is scraped using tweezers and other items and exposes ito anode.Most
Afterwards, it is put into mask plate, < 3 × 10-4Under the vacuum of Pa, 90nm metal Ag is deposited.The effective area of battery device is 0.16cm2。
Except NiOxThe preparation process of film is completed in atmospheric environment, remaining all link is complete in the glove box of nitrogen atmosphere
At.
Embodiment 2
The present embodiment provides a kind of perovskite device (being inverted perovskite structure), and structure is consistent in embodiment 1, system
In Preparation Method in addition to electron transfer layer solution prepares difference, remaining is consistent with embodiment 1.
Electron transfer layer solution is formulated as follows:
PCBM solution concentration is 20 milligrams every milliliter, and solvent is chlorobenzene, and 2,2 bipyridyls are added, are configured to 1 milligram of every milli
2,2 bipyridyl solutions risen are to get electron transfer layer Solutions Solution.
Embodiment 3
The present embodiment provides a kind of perovskite device (being inverted perovskite structure), and structure is consistent in embodiment 1, system
In Preparation Method in addition to electron transfer layer solution prepares difference, remaining is consistent with embodiment 1.
Electron transfer layer solution is formulated as follows:
PCBM solution concentration is 20 milligrams every milliliter, and solvent is dichloro-benzenes, and phenanthroline is added, is configured to 0.05 milligram
Every milliliter of phenanthroline solution is to get electron transfer layer Solutions Solution.
Embodiment 4
The present embodiment provides a kind of perovskite device (being inverted perovskite structure), and structure is consistent in embodiment 1, system
In Preparation Method in addition to electron transfer layer solution prepares difference, remaining is consistent with embodiment 1.
Electron transfer layer solution is formulated as follows:
PCBM solution concentration is 20 milligrams every milliliter, and solvent is trichloro-benzenes, and EDTA is added, is configured to 1 milligram every milliliter
EDTA solution is to get electron transfer layer Solutions Solution.
Embodiment 5
The present embodiment provides a kind of perovskite device (being inverted perovskite structure), specific structure CsPbI2Br, preparation
Method is as follows.
(1) pre-treatment of transparency conducting layer
It is 15 Ω square by resistance–1Tin indium oxide (ITO) electro-conductive glass piece successively through deionized water, acetone, washing
Agent, deionized water and ethyl alcohol pass through ultrasonic cleaning, every each 20min of step.
(2) configuration of perovskite precursor liquid
1.3284mol/L lead iodide, 1.302mol/L lead bromide, solvent for use DMSO are prepared respectively.
Above-mentioned lead iodide and lead bromide 1:1 are mixed, 1.2mol/L cesium iodide is prepared with the mixed solution, obtains perovskite
Solution.
(3) electron transfer layer solution is prepared
PCBM solution concentration is 20 milligrams every milliliter, and solvent is chlorobenzene, and 4,4 bipyridyls are added, are configured to 1 milligram of every milli
4,4 bipyridyl solutions risen are to get electron transfer layer Solutions Solution.
(4) preparation of cathode interface layer solution
2 milligrams every milliliter of acetylacetone,2,4-pentanedione zirconium, solvent is ethyl alcohol.
(5) preparation of perovskite device
After drying ito glass in an oven, handled 4 minutes using PLASMA (oxygen plasma).Then above-mentioned processed
Ito glass on piece, spin coating layer of Ni OxFilm, thickness are about 10nm, 120 DEG C of annealing 20min.In the glove box of nitrogen atmosphere
In perovskite precursor liquid is spin-coated on NiOxOn layer.Spincoating conditions, 500 turns of first segment 3 seconds, 2500 turns of second segment 30 seconds to spin coating
Machine stops, and is placed on 42 DEG C of annealing 4min of thermal station, later in 160 DEG C of thermal station annealing 10min.2500 turn 30 of electron transfer layer solution
Second, 50 DEG C of annealing 5min.4000 turns of spin coating acetylacetone,2,4-pentanedione zirconium 60 seconds.It is scraped using tweezers and other items and exposes ito anode.Finally,
It is put into mask plate, < 3 × 10-4Under the vacuum of Pa, 90nm metal Ag is deposited.The effective area of battery device is 0.16cm2.It removes
NiOxThe preparation process of film is completed in atmospheric environment, remaining all link is complete in the glove box of nitrogen atmosphere
At.
Embodiment 6
The present embodiment provides a kind of perovskite device (being inverted perovskite structure), specific structure MAPbI3, preparation side
Method is as follows.
(1) pre-treatment of transparency conducting layer
It is 15 Ω square by resistance–1Tin indium oxide (ITO) electro-conductive glass piece successively through deionized water, acetone, washing
Agent, deionized water and ethyl alcohol pass through ultrasonic cleaning, every each 20min of step.
(2) configuration of perovskite precursor liquid
1.06mol/L MAI is prepared, dissolves lead iodide with it, obtains 1mol/L lead iodide and 1.06mol/LMAI mixing
Solution, i.e. perovskite solution.
(3) electron transfer layer solution is prepared
PCBM solution concentration is 20 milligrams every milliliter, and solvent is chlorobenzene, and 4,4 bipyridyls are added, are configured to 1 milligram of every milli
4,4 bipyridyl solutions risen are to get electron transfer layer Solutions Solution.
(4) preparation of cathode interface layer solution
2 milligrams every milliliter of acetylacetone,2,4-pentanedione zirconium, solvent is ethyl alcohol.
(5) preparation of perovskite device
After drying ito glass in an oven, handled 4 minutes using PLASMA (oxygen plasma).Then above-mentioned processed
Ito glass on piece, spin coating layer of Ni OxFilm, thickness are about 10nm, 120 DEG C of annealing 20min.In the glove box of nitrogen atmosphere
In perovskite precursor liquid is spin-coated on NiOxOn layer.Spincoating conditions, 900 turns of first segment 50 seconds, 5000 turns of 20 seconds Shi Chong of second segment
Anti-solvent isopropanol (400 microlitres) turns 20 seconds again, stops to sol evenning machine, is placed on 100 DEG C of annealing 10min of thermal station, electron transfer layer
2500 turns of solution 30 seconds, 50 DEG C of annealing 5min.4000 turns of spin coating acetylacetone,2,4-pentanedione zirconium 60 seconds.It is scraped and is exposed using tweezers and other items
Ito anode.Finally, mask plate is put into, < 3 × 10-4Under the vacuum of Pa, 90nm metal Ag is deposited.The effective area of battery device
For 0.16cm2.Except NiOxThe preparation process of film is completed in atmospheric environment, remaining all link is in nitrogen atmosphere
It is completed in glove box.
Comparative example 1
This comparative example provides a kind of perovskite device (being inverted perovskite structure), is electronics with the difference of embodiment 1
Transport layer solution is not added with 4,4 bipyridyls when preparing, with step and structure consistent, the obtained electron-transport with embodiment 1
4,4 bipyridyl of passivator is not distributed in layer.
Fluorescence emission spectrum test is carried out to the calcium titanium ore bed that embodiment 1 (sample 3), embodiment 2 and comparative example 1 provide,
Test result such as Fig. 2.As seen from the figure, in embodiment 1 after the electron transfer layer of passivator is distributed in perovskite surface modification, calcium
Titanium ore film fluorescence is substantially better than the calcium titanium ore bed of modification ordinary electronic transport layer, and charge recombination weakens, and showing can after introducing B layers
Significant passivation defect reduces the probability of charge recombination.
The distribution of 4,4 bipyridyl of passivator in the electron transfer layer of embodiment 1 is measured (test of XPS depth profiling,
Test philosophy such as Fig. 3), result such as table 1, the object element can qualitatively find out the changes of contents of passivator.It can from table 1
Know, it is higher closer to calcium titanium ore bed passivation agent content, confirm self assembly, such as Fig. 4.
The distribution of 1 passivator of table, 4,4 bipyridyl
The perovskite device provided Examples 1 to 4 and comparative example 1 carries out photovoltaic property test, result such as 2 He of table
Fig. 5.Conventional electrical transport layer is selected, calcium titanium ore bed is not passivated, energy conversion efficiency 15.92%, current density
For 21.43mAcm-2, open-circuit voltage 1.01V, fill factor 72.95%.In contrast, one layer is prepared on perovskite surface
Electron transfer layer, performance significantly improve.For example, the perovskite device energy conversion efficiency that embodiment 2 provides is 17.00%, electricity
Current density is 22.19mAcm-2, open-circuit voltage 0.96V, fill factor 79.81%.In area of solar cell, a pass
The technical parameter of key is exactly fill factor, and fill factor shows the relative populations of defect in the device, from data it can be seen that
It uses the method for the invention to be passivated so that fill factor is promoted from 72% to the degree close to 80%, illustrates the present invention
Perovskite surface defect can be effectively passivated.Even we are it is to be understood that carry out the filling of the precision control device of atomic level
The factor is also extremely difficult to 85% or more (even promoting 1% is also to have technical difficulty), this is because the vibration of atom so that
Inevitably there are some defects in crystal, is not only surface defect there are also being more internal flaw, this can more illustrate this hair
The bright passivation effect to device surface defect it is obvious.Show to be passivated significantly perovskite surface using this method
Effect shows biggish application potential.
The photovoltaic property test result of 2 perovskite device of table
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. the electron transfer layer that one kind can be passivated calcium titanium ore bed surface defect, which is characterized in that by electron transport layer materials and blunt
Agent composition, the passivator are distributed in electron transport layer materials；The electron transfer layer is PCBM, nano zine oxide or receives
Rice cerium oxide；The passivator is one or more of 2,2 bipyridyls, 4,4 bipyridyls, phenanthroline or EDTA.
2. electron transfer layer according to claim 1, which is characterized in that the passivator is distributed in electron transport layer materials
Mass concentration gradually increased by side to the other side.
3. electron transfer layer according to claim 1, which is characterized in that the electron transfer layer is set on calcium titanium ore bed.
4. electron transfer layer according to claim 1, which is characterized in that the quality of the electron transport layer materials and passivator
Than for 20~400:1.
5. the preparation method of electron transfer layer described in Claims 1 to 4, which comprises the steps of:
S1: electron transport layer materials, passivator and solvent are mixed into obtain mixed solution；
S2: mixed solution is spin-coated on calcium titanium ore bed, is annealed up to the electron transfer layer.
6. electron transfer layer according to claim 5, which is characterized in that the temperature of the annealing is 40~55 DEG C, the time 3
~5min.
7. a kind of inversion perovskite structure, which is characterized in that comprise the following structure from the bottom to top: transparency conducting layer, hole transport
Any electron transfer layer of layer, calcium titanium ore bed, Claims 1 to 4 and to electrode.
8. being inverted perovskite structure according to claim 7, which is characterized in that the transparency conducting layer is ITO electro-conductive glass
Piece, FIO electro-conductive glass or transparent nano silver wire electrode；The hole transmission layer is NiOx, PEDOT:PSS or PTAA；It is described right
Electrode is silver electrode, gold electrode or aluminium electrode.
9. being inverted perovskite structure according to claim 7, which is characterized in that the electron transfer layer and between electrode also
It is provided with cathode interface layer.
10. any inversion perovskite structure of claim 7~9 is preparing the application in solar battery.
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