CN113517404B - Perovskite solar cell based on multilayer gradient energy charge transport layer and preparation method thereof - Google Patents
Perovskite solar cell based on multilayer gradient energy charge transport layer and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 122
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 118
- 230000005525 hole transport Effects 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 239000010410 layer Substances 0.000 claims description 133
- 239000008367 deionised water Substances 0.000 claims description 40
- 229910021641 deionized water Inorganic materials 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 229910001432 tin ion Inorganic materials 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 31
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 claims description 28
- 238000004528 spin coating Methods 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 22
- 229940046892 lead acetate Drugs 0.000 claims description 13
- 239000002243 precursor Substances 0.000 claims description 13
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 11
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 7
- 238000010345 tape casting Methods 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 239000002344 surface layer Substances 0.000 claims description 6
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- JKSIBASBWOCEBD-UHFFFAOYSA-N N,N-bis(4-methoxyphenyl)-9,9'-spirobi[fluorene]-1-amine Chemical compound COc1ccc(cc1)N(c1ccc(OC)cc1)c1cccc2-c3ccccc3C3(c4ccccc4-c4ccccc34)c12 JKSIBASBWOCEBD-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- KQNKJJBFUFKYFX-UHFFFAOYSA-N acetic acid;trihydrate Chemical compound O.O.O.CC(O)=O KQNKJJBFUFKYFX-UHFFFAOYSA-N 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 238000007639 printing Methods 0.000 claims description 3
- 238000007761 roller coating Methods 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 229920002457 flexible plastic Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002159 nanocrystal Substances 0.000 claims description 2
- 229920000123 polythiophene Polymers 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 27
- 238000012827 research and development Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 description 17
- 238000005303 weighing Methods 0.000 description 16
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 9
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- FWPIDFUJEMBDLS-UHFFFAOYSA-L tin(II) chloride dihydrate Chemical group O.O.Cl[Sn]Cl FWPIDFUJEMBDLS-UHFFFAOYSA-L 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- UUIMDJFBHNDZOW-UHFFFAOYSA-N 2-tert-butylpyridine Chemical compound CC(C)(C)C1=CC=CC=N1 UUIMDJFBHNDZOW-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
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- 238000005215 recombination Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- -1 trifluoromethanesulfonyl imide Chemical class 0.000 description 1
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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
-
- 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
- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
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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
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
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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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Abstract
The invention discloses a perovskite solar cell based on a plurality of gradient energy charge transport layers and a preparation method thereof. The perovskite solar cell consists of a substrate, a transparent conducting layer, an electron transport layer, an organic-inorganic perovskite structure photoactive layer, a hole transport layer and a back electrode from bottom to top, wherein the electron transport layer is a lead-doped tin oxide multilayer gradient energy level electron transport layer. The lead-doped tin oxide multilayer gradient energy level electron transport layer can greatly reduce leakage current, greatly improve the photoelectric conversion efficiency of the solar cell in a weak light environment, and has positive significance for research and development of perovskite solar cells which can be worn in future movement.
Description
Technical Field
The invention relates to the technical field of perovskite solar cells, in particular to a perovskite solar cell based on a plurality of gradient energy charge transport layers and a preparation method thereof.
Background
The organic-inorganic hybrid perovskite solar cell has the advantages of simple process, low production cost, capability of preparing flexible and portable devices, high photoelectric conversion efficiency and the like, is widely focused by global researchers, and in addition, a plurality of companies begin to research and prepare the organic-inorganic hybrid perovskite solar cell in China, so that the organic-inorganic hybrid perovskite solar cell becomes an important direction of development in the photovoltaic field. Silicon solar cells have been an absolute advantage in the photovoltaic field, and perovskite solar cells are difficult to replace comprehensively, but can be partially replaced according to the disadvantages of silicon solar cells. For example, silicon solar cells are heavy and it is difficult to produce flexible portable photovoltaic devices. Flexible organic-inorganic hybrid perovskite solar cells would be an important development direction. The use of portable photovoltaic devices, which are mobile, faces a problem, requiring use in different lighting environments. Therefore, research on organic-inorganic hybrid perovskite solar cells which still have excellent photoelectric conversion performance in low-light illumination environments is of great significance to the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a perovskite solar cell based on a multi-layer gradient energy electron transport layer and a preparation method thereof, wherein lead is doped in tin oxide to enable a conduction band of the tin oxide to move downwards, the band gap is narrowed, and a plurality of layers of tin oxide with different doping amounts can be sequentially prepared to obtain a gradient energy level electron transport layer, and the interface electron recombination and leakage current are reduced by the multi-layer gradient energy level electron transport layer; and in the low-light environment, the photoelectric performance is better.
The invention aims to provide a perovskite solar cell based on a multi-layer gradient energy charge transport layer, which sequentially comprises a substrate, a transparent conducting layer, an electron transport layer, an organic-inorganic perovskite structure photoactive layer, a hole transport layer and a back electrode from bottom to top, wherein the electron transport layer is a lead-doped tin oxide multi-layer gradient energy electron transport layer.
Preferably, the lead-doped tin oxide multilayer gradient energy level electron transport layer is prepared by spin coating, knife coating, spray coating, printing or roller coating. The invention adopts the doctor-blading, or spraying, roller coating, roll-to-roll, printing technology or spin coating method to deposit tin oxide with different doping concentrations for a plurality of times to obtain the ultrathin multilayer gradient energy level electron transport layer.
Preferably, the deposition layer number of the lead-doped tin oxide multilayer gradient energy level electron transport layer is 2-3, and the lead doping concentration gradient in the electron transport layer is reduced from the bottom layer to the surface layer.
Preferably, the lead doping concentration is 0.1-10mol%.
Further preferably, the deposition layer number of the lead-doped tin oxide multilayer gradient energy level electron transport layer is 2, the lead doping concentration of the bottom layer is 0.1-1mol%, and the lead doping concentration of the surface layer is 3-10mol%.
Preferably, the thickness of each electron transport layer is 15nm, the thickness of the organic-inorganic perovskite structure photoactive layer is 400nm, the thickness of the hole transport layer is 100nm, and the thickness of the back electrode is 60nm.
Preferably, the substrate is glass or flexible plastic, the transparent conductive layer is made of fluorine doped tin oxide (FTO) or indium doped tin oxide (ITO), and the perovskite structure photoactive layer is made of one of MAPbI 3、FAPbI3、MAPbBr3、FAPbBr3 or Cs (1-x-y):FAxMAyPbI(3-z)Brz、CsPbI3、CsPbBr3 and CsPbI (3-y)Bry; the hole transport layer is made of one or two selected from polythiophene, 2', 7' -tetra [ N, N-di (4-methoxyphenyl) amino ] -9,9' -spirobifluorene, cuSCN, WO 3 and MoO 3; the material of the back electrode is silver, aluminum, gold, copper or alloy material of silver, aluminum, gold and copper.
The invention also provides a preparation method of the perovskite solar cell, which comprises the following steps:
(1) Carrying out ultraviolet ozone treatment on the pretreated transparent conductive layer;
(2) Preparing a lead-doped tin oxide nanocrystalline film on the surface of the transparent conductive layer, carrying out ultraviolet ozone treatment on the tin oxide nanocrystalline film, and repeating the steps for a plurality of times to obtain a lead-doped tin oxide multilayer gradient energy level electron transport layer;
(3) Preparing a perovskite structure photoactive layer on the lead-doped tin oxide multilayer gradient energy level electron transport layer through a knife coating process;
(4) Preparing a hole transport material layer on the perovskite structure photoactive layer through a spin coating process;
(5) Depositing a back electrode on the hole transport material layer by adopting a thermal evaporation method;
the lead-doped tin oxide nanocrystalline film is prepared by the following steps:
a. Preparing a lead ion solution: dissolving a lead ion precursor in deionized water to obtain a lead ion solution with the concentration of 0.0003-0.009 mol/L;
b. preparing tin ion solution: dissolving a tin ion precursor in deionized water to obtain a tin ion solution with the concentration of 0.1-0.3 mol/L;
c. Preparing a lead-doped tin oxide nano solution: slowly dripping the lead ion solution into the tin ion solution at the temperature of 0-5 ℃ and stirring, heating the solution to the temperature of 70-90 ℃ after uniformly stirring, and introducing air into the solution for 1-2 hours to obtain the lead-doped tin oxide nano solution;
d. Preparing a lead-doped tin oxide nanocrystalline film: and (3) the obtained lead-doped tin oxide nano solution is subjected to a blade coating, spraying or spin coating method to obtain the lead-doped tin oxide nano crystal film.
The pretreatment steps of the transparent conductive layer specifically comprise: ultrasonic cleaning is respectively carried out for 30 minutes by deionized water, absolute ethyl alcohol and isopropanol, and then drying is carried out by high-purity nitrogen.
Preferably, the specific steps of step d are: preparing a lead-doped tin oxide nanocrystalline film by adopting a spin coating method, wherein the spin coating rate is 3000-5000rpm, and the heat treatment is carried out for 30 minutes at 100-150 ℃.
Preferably, the lead ion precursor is anhydrous lead acetate or lead acetate trihydrate, and the tin ion precursor is selected from one of anhydrous tin tetrachloride, anhydrous stannous chloride and anhydrous stannous chloride.
Compared with the prior art, the invention has the beneficial effects that:
1. The lead element is used for doping, so that the conduction band of the tin oxide moves downwards, the band gap is narrowed, and the multilayer gradient energy level electron transport layer can be obtained.
2. The lead-doped tin oxide multi-layer gradient energy level electron transport layer is used, so that the photoelectric conversion efficiency of the perovskite solar cell can be improved, the weak light performance of the perovskite solar cell can be greatly improved, and the lead-doped tin oxide multi-layer gradient energy level electron transport layer has positive significance for research and development of the perovskite solar cell which can be worn in future movement.
Drawings
Fig. 1 is a schematic structural view of a solar cell prepared in example 1 of the present invention;
FIG. 2 is a graph of the relationship (. Alpha.hν) 2 -hν for doping concentrations of 1-3mol% tin oxide and pure tin oxide;
FIG. 3 is a J-V curve of the solar cell prepared in example 1 and comparative example 1 of the present invention under the condition that the light source is a solar simulator (standard light source) and the illumination intensity is 100mW/cm 2, wherein J is the photocurrent density and V is the photovoltage;
FIG. 4 is a J-V curve of the solar cell prepared in example 1 and comparative example 1 of the present invention at an energy density of 0.1mW/cm 2, where J is a photocurrent density and V is a photovoltage;
The attached sign indicates: 1. a substrate; 2. a transparent conductive layer; 3. 3% lead doped tin oxide three-layer gradient energy level electron transport layer; 4. 2% lead doped tin oxide three-layer gradient energy level electron transport layer; 5. 1% lead doped tin oxide three-layer gradient energy level electron transport layer; 6. an organic-inorganic perovskite structure photoactive layer; 7. a hole transport layer; 8. and a back electrode.
Detailed Description
The following examples are further illustrative of the invention and are not intended to be limiting thereof. The equipment and reagents used in the present invention are conventional commercially available products in the art, unless specifically indicated. In the following examples, it is preferable that the thickness of each of the electron transport layers is 15nm, the thickness of the organic-inorganic perovskite structure photoactive layer is 400nm, the thickness of the hole transport layer is 100nm, and the thickness of the back electrode is 60nm. Unless otherwise specified in the following examples, the photoelectric conversion efficiency of the perovskite solar cell refers to the photoelectric conversion efficiency under the condition of a standard light source (illumination intensity of 100mW/cm 2).
Example 1
As shown in fig. 1, the perovskite solar cell prepared by the implementation has a structure comprising a substrate 1, an FTO transparent conductive layer 2, a lead-doped tin oxide three-layer gradient energy level electron transport layer 3-5 (comprising 3% lead-doped tin oxide, 2% lead-doped tin oxide and 1% lead-doped tin oxide from bottom to top), a perovskite light absorption layer 6, a hole transport layer 7 and a back electrode 8.
The preparation of the perovskite solar cell comprises the following steps:
(1) Respectively carrying out ultrasonic cleaning on FTO glass for 30 minutes by deionized water, absolute ethyl alcohol and isopropanol, and then drying by high-purity nitrogen;
(2) Carrying out ultraviolet ozone treatment on the cleaned FTO glass sheet, improving the wettability of the FTO surface and increasing the work function of the transparent conductive film;
(3) Spin-coating a tin oxide nanocrystalline film doped with 3% lead on the surface of the FTO as an electron transmission layer, wherein the spin-coating rotating speed is 4000rpm, and performing heat treatment at 150 ℃ for 30 minutes;
(4) Carrying out ultraviolet ozone treatment on the tin oxide nanocrystalline film doped with 3% lead, improving the wettability of the surface of the FTO, and increasing the work function of the transparent conductive film;
(5) Spin-coating a layer of tin oxide nanocrystalline film with 2% lead on the tin oxide nanocrystalline film doped with 3% lead, wherein the spin-coating rotating speed is 4000rpm, and performing heat treatment at 150 ℃ for 30 minutes;
(6) Carrying out ultraviolet ozone treatment on the tin oxide nanocrystalline film doped with 2% lead, improving the wettability of the surface of the FTO, and increasing the work function of the transparent conductive film;
(7) Spin-coating a layer of tin oxide nanocrystalline film with 1% lead on the tin oxide nanocrystalline film doped with 2% lead, wherein the spin-coating rotating speed is 4000rpm, and performing heat treatment at 150 ℃ for 30 minutes;
(8) Carrying out ultraviolet ozone treatment on the tin oxide nanocrystalline film doped with 1% lead, improving the wettability of the surface of the FTO, and increasing the work function of the transparent conductive film;
(9) A layer of MAPbI 3 film is coated on the tin oxide nanocrystalline film doped with 1% of lead in a scraping way, the scraping speed is 100mm/min, the heating temperature of a base is 150 ℃, and the gap between a scraper and the surface of a substrate is 100 mu m;
(10) A layer of 2,2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9 '-spirobifluorene was spin-coated on the MAPbI 3 film as a hole transport layer material at 4000rpm, wherein the hole transport layer material solution was an acetonitrile solution containing 72.3mg of 2,2',7 '-tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene, 28.8. Mu.L of tert-butylpyridine, 17.5. Mu.L of lithium bis (trifluoromethanesulfonyl imide) in 1mL of chlorobenzene.
(11) And depositing a gold counter electrode by adopting a thermal evaporation method, wherein the thickness of the gold counter electrode is 60nm.
The synthesis of the 1% lead-doped tin oxide nanocrystalline film in this embodiment includes the following steps:
a. Weighing 4.8mg of anhydrous lead acetate by taking deionized water as a solvent, and adding 5mL of deionized water, wherein the concentration of a lead ion solution is 0.003mol/L;
b. Taking deionized water as a solvent, weighing 389.5mg of stannic chloride, adding 5mL of deionized water, and enabling the concentration of a tin ion solution to be 0.3mol/L;
c. Slowly dripping the lead ion solution into the tin ion solution at 0 ℃ and stirring, heating the solution to 90 ℃ after stirring uniformly, and introducing 10mL/min of air into the solution to obtain semitransparent milky tin oxide nano solution doped with 1% lead after 2 hours;
d. The lead-doped tin oxide nanocrystalline film is prepared by adopting a spin coating method, the rotating speed is 4000rpm, and the heat treatment is carried out for 30 minutes at 120 ℃.
The synthesis of the 1% lead-doped tin oxide nanocrystalline film in this embodiment includes the following steps:
a. 9.6mg of anhydrous lead acetate is weighed by taking deionized water as a solvent, 5mL of deionized water is added, and the concentration of a lead ion solution is 0.006mol/L;
b. Taking deionized water as a solvent, weighing 389.5mg of stannic chloride, adding 5mL of deionized water, and enabling the concentration of a tin ion solution to be 0.3mol/L;
c. slowly dripping the lead ion solution into the tin ion solution at 0 ℃ and stirring, heating the solution to 90 ℃ after stirring uniformly, and introducing 10mL/min of air into the solution to obtain semitransparent milky tin oxide nano solution doped with 2% lead after 2 hours;
d. The lead-doped tin oxide nanocrystalline film is prepared by adopting a spin coating method, the rotating speed is 4000rpm, and the heat treatment is carried out for 30 minutes at 120 ℃.
The synthesis of the 3% lead-doped tin oxide nanocrystalline film comprises the following steps:
(1) Weighing 14.4mg of anhydrous lead acetate by taking deionized water as a solvent, adding 5mL of deionized water, and enabling the concentration of a lead ion solution to be 0.009mol/L;
(2) Taking deionized water as a solvent, weighing 389.5mg of stannic chloride, adding 5mL of deionized water, and enabling the concentration of a tin ion solution to be 0.3mol/L;
(3) Slowly dripping the lead ion solution into the tin ion solution at 0 ℃ and stirring, heating the solution to 90 ℃ after stirring uniformly, and introducing 10mL/min of air into the solution to obtain semitransparent milky tin oxide nano solution doped with 3% lead after 2 hours;
d. The lead-doped tin oxide nanocrystalline film is prepared by adopting a spin coating method, the rotating speed is 4000rpm, and the heat treatment is carried out for 30 minutes at 120 ℃.
Finally, the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer has the photoelectric conversion efficiency of 19.3%.
Comparative example 1
The same as in example 1, except that:
the synthesis of the tin oxide nanocrystalline film in this comparative example comprises the following steps:
a. Taking deionized water as a solvent, weighing 389.5mg of stannic chloride, adding 5mL of deionized water, and enabling the concentration of a tin ion solution to be 0.3mol/L;
b. slowly dripping the lead ion solution into the tin ion solution at 0 ℃ and stirring, heating the solution to 90 ℃ after uniformly stirring, and introducing 10mL/min of air into the solution for 2 hours to obtain semitransparent milky tin oxide nano solution;
c. The tin oxide nanocrystalline film was prepared by spin coating at 4000rpm and heat-treated at 120℃for 30 minutes.
Finally, the obtained perovskite solar cell with a tin oxide electron transport layer had a photoelectric conversion efficiency of 16.6%.
Fig. 3 and 4 show the J-V curves of the solar cells of example 1 and comparative example 1, respectively, under a solar simulator (illumination intensity 100mW/cm 2) and under a white LED (illumination intensity 0.1mW/cm 2), where J is the photocurrent density and V is the photovoltage. The lead-doped tin oxide multilayer gradient energy level electron transport layer can be used for improving the photoelectric conversion efficiency in 1 solar (100 mW/cm 2) and the indoor-like light environment (0.1 mW/cm 2) to a small extent. The photoelectric conversion efficiency of the solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer under the indoor-like light environment (0.1 mW/cm 2) is improved by 4.27 times compared with that of the solar cell with the single-layer SnO 2 transport layer. The photoelectric conversion efficiency of the solar cell in fig. 4 was 7.2% and 30.8%, respectively.
Therefore, the lead-doped tin oxide multilayer gradient energy level electron transport layer can greatly improve the photoelectric conversion performance in a weak light environment.
Comparative example 2
The same as in example 1, except that:
the synthesis of the 1% lead-doped tin oxide nanoparticle in this comparative example comprises the following steps:
a. Weighing 4.8mg of anhydrous lead acetate by taking deionized water as a solvent, and adding 5mL of deionized water, wherein the concentration of a lead ion solution is 0.003mol/L;
b. Taking deionized water as a solvent, weighing 389.5mg of stannic chloride, adding 5mL of deionized water, and enabling the concentration of a tin ion solution to be 0.3mol/L;
c. Slowly dripping the lead ion solution into the tin ion solution at 0 ℃ and stirring, heating the solution to 90 ℃ after stirring uniformly, and introducing 10mL/min of air into the solution to obtain semitransparent milky tin oxide nano solution doped with 1% lead after 2 hours;
d. The lead-doped tin oxide nanocrystalline film is prepared by adopting a spin coating method, the rotating speed is 4000rpm, and the heat treatment is carried out for 30 minutes at 120 ℃.
Finally, the obtained perovskite solar cell with the lead-tin oxide electron transport layer doped with 1mol% has a photoelectric conversion efficiency of 17.1%.
Example 2
The same as in example 1, except that:
The preparation method of the lead-doped tin oxide multilayer gradient energy level electron transport layer is changed into a knife coating method, the knife coating speed is 120mm/min, the heating temperature of a substrate is 50 ℃, the gap between a scraper and the surface of the substrate is 50 mu m, and then the heat treatment is carried out for 30 minutes at 150 ℃.
The photoelectric conversion efficiency of the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer reaches 17.5%.
Example 3
The same as in example 1, except that:
the preparation method of the lead-doped tin oxide multilayer gradient energy level electron transport layer is changed into a spraying method, the spraying time is 3s, the heating temperature of the substrate is 80 ℃, the distance between the nozzle and the surface of the substrate is 10cm, and then the heat treatment is carried out for 30 minutes at 150 ℃.
The photoelectric conversion efficiency of the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer reaches 17.2%.
FIG. 2 is a schematic representation of the forbidden band width calculated from the absorption edge for lead-doped tin oxide of varying lead concentrations. Lead doping can be seen to effectively reduce the forbidden bandwidth of tin oxide.
Example 4
The same as in example 1, except that:
the preparation method of the lead-doped tin oxide multilayer gradient energy level electron transport layer is an ink-jet printing method.
The photoelectric conversion efficiency of the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer is 16.2%.
Example 5
The same as in example 1, except that:
The preparation method of the lead-doped tin oxide multilayer gradient energy level electron transport layer is a roll coating method.
The photoelectric conversion efficiency of the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer is 17.5%.
Example 6
The same as in example 1, except that:
The preparation method of the lead-doped tin oxide multilayer gradient energy level electron transport layer is spin coating, the rotating speed is 3000rpm, and the heat treatment is carried out for 30 minutes at 120 ℃.
The photoelectric conversion efficiency of the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer was 17.9%.
Example 7
The same as in example 1, except that:
The preparation method of the lead-doped tin oxide multilayer gradient energy level electron transport layer is spin coating, the rotating speed is 5000rpm, and the heat treatment is carried out for 30 minutes at the temperature of 120 ℃.
The photoelectric conversion efficiency of the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer is 17.5%.
Example 8
The same as in example 1, except that:
Except that lead acetate trihydrate is used as a lead ion precursor.
The obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer has the photoelectric conversion efficiency of 17.8%.
Example 9
The same as in example 1, except that:
A double-layer lead-doped tin oxide electron transport layer is used. Respectively a tin oxide nanocrystalline film doped with 3% lead and a tin oxide nanocrystalline film doped with 1% lead.
The obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer has the photoelectric conversion efficiency of 20.3 percent.
Example 10
The same as in example 9, except that:
Lead concentration of lead-doped tin oxide varies.
In this example, the synthesis of 1% doped lead tin oxide nanoparticles comprises the following steps:
a. Weighing 4.8mg of anhydrous lead acetate by taking deionized water as a solvent, and adding 5mL of deionized water, wherein the concentration of a lead ion solution is 0.003mol/L;
b. Taking deionized water as a solvent, weighing 389.5mg of stannic chloride, adding 5mL of deionized water, and enabling the concentration of a tin ion solution to be 0.3mol/L;
c. Slowly dripping the lead ion solution into the tin ion solution at 0 ℃ and stirring, heating the solution to 90 ℃ after stirring uniformly, and introducing 10mL/min of air into the solution to obtain semitransparent milky tin oxide nano solution doped with 1% lead after 2 hours;
d. The lead-doped tin oxide nanocrystalline film is prepared by adopting a spin coating method, the rotating speed is 4000rpm, and the heat treatment is carried out for 30 minutes at 120 ℃.
The synthesis of the 10% lead-doped tin oxide nanoparticle comprises the following steps:
a. Weighing 48.0mg of anhydrous lead acetate by taking deionized water as a solvent, and adding 5mL of deionized water, wherein the concentration of a lead ion solution is 0.03mol/L;
b. weighing 259.6mg of stannic chloride by taking deionized water as a solvent, and adding 5mL of deionized water, wherein the concentration of a tin ion solution is 0.3mol/L;
c. Slowly dripping the lead ion solution into the tin ion solution at 0 ℃ and stirring, heating the solution to 90 ℃ after stirring uniformly, and introducing 10mL/min of air into the solution to obtain semitransparent milky 10% lead-doped tin oxide nano solution after 2 hours;
d. The lead-doped tin oxide nanocrystalline film is prepared by adopting a spin coating method, the rotating speed is 4000rpm, and the heat treatment is carried out for 30 minutes at 120 ℃.
Finally, the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer has the photoelectric conversion efficiency of 16.1 percent.
Example 11
The same as in example 9, except that:
Lead concentration of lead-doped tin oxide varies.
In this example, the synthesis of the doped 0.1% lead tin oxide nanoparticle comprises the following steps:
a. weighing 0.48mg of anhydrous lead acetate by taking deionized water as a solvent, adding 5mL of deionized water, and enabling the concentration of a lead ion solution to be 0.0003mol/L;
b. Taking deionized water as a solvent, weighing 389.5mg of stannic chloride, adding 5mL of deionized water, and enabling the concentration of a tin ion solution to be 0.3mol/L;
c. Slowly dripping the lead ion solution into the tin ion solution at 0 ℃ and stirring, heating the solution to 90 ℃ after stirring uniformly, and introducing 10mL/min of air into the solution to obtain semitransparent milky tin oxide nano solution doped with 0.1% lead after 2 hours;
d. The lead-doped tin oxide nanocrystalline film is prepared by adopting a spin coating method, the rotating speed is 4000rpm, and the heat treatment is carried out for 30 minutes at 120 ℃.
In this example, the synthesis of 10% doped lead tin oxide nanoparticles comprises the following steps:
a. Weighing 38.0mg of anhydrous lead acetate by taking deionized water as a solvent, and adding 5mL of deionized water, wherein the concentration of a lead ion solution is 0.03mol/L;
b. Taking deionized water as a solvent, weighing 389.5mg of stannic chloride, adding 5mL of deionized water, and enabling the concentration of a tin ion solution to be 0.3mol/L;
c. Slowly dripping the lead ion solution into the tin ion solution at 0 ℃ and stirring, heating the solution to 90 ℃ after stirring uniformly, and introducing 10mL/min of air into the solution to obtain semitransparent milky 10% lead-doped tin oxide nano solution after 2 hours;
d. The lead-doped tin oxide nanocrystalline film is prepared by adopting a spin coating method, the rotating speed is 4000rpm, and the heat treatment is carried out for 30 minutes at 120 ℃.
Finally, the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer has the photoelectric conversion efficiency of 18.2%.
Example 12
The same as in example 9, except that:
The concentration of the tin ion solution was different, and the concentration of the tin ion solution was 0.2mol/L.
Finally, the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer has the photoelectric conversion efficiency of 17.3%.
Example 13
The same as in example 9, except that:
the concentration of the tin ion solution was varied, and the concentration of the tin ion solution was 0.1mol/L.
Finally, the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer has the photoelectric conversion efficiency of 15.2%.
Example 14
The same as in example 9, except that:
The tin ion solution is different in precursor, and the tin ion precursor is anhydrous stannous chloride.
Finally, the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer has the photoelectric conversion efficiency of 18.2%.
Example 15
The same as in example 9, except that:
The tin ion solution is different in precursor, and the tin ion precursor is stannous chloride dihydrate.
Finally, the obtained perovskite solar cell with the lead-doped tin oxide multilayer gradient energy level electron transport layer has the photoelectric conversion efficiency of 18.3%.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (5)
1. The preparation method of the perovskite solar cell based on the multilayer gradient energy electron transport layer is characterized in that the perovskite solar cell sequentially comprises a substrate, a transparent conductive layer, an electron transport layer, an organic-inorganic perovskite structure photoactive layer, a hole transport layer and a back electrode from bottom to top, wherein the electron transport layer is a lead-doped tin oxide multilayer gradient energy electron transport layer; the lead-doped tin oxide multilayer gradient energy level electron transport layer is prepared by spin coating, knife coating, spray coating, printing or roller coating; the lead doping concentration gradient from the bottom layer to the surface layer in the electron transport layer is reduced, the deposition layer number of the lead-doped tin oxide multilayer gradient energy level electron transport layer is 2, the lead doping concentration of the surface layer is 0.1-1 mol%, and the lead doping concentration of the bottom layer is 3-10 mol%;
The preparation method of the perovskite solar cell based on the multilayer gradient energy electron transport layer comprises the following steps:
(1) Carrying out ultraviolet ozone treatment on the pretreated transparent conductive layer;
(2) Preparing a bottom layer of lead-doped tin oxide nanocrystalline film on the surface of the transparent conductive layer, carrying out ultraviolet ozone treatment on the bottom layer of tin oxide nanocrystalline film, preparing a surface layer of lead-doped tin oxide nanocrystalline film, and carrying out ultraviolet ozone treatment on the surface layer of tin oxide nanocrystalline film to obtain a lead-doped tin oxide multilayer gradient energy level electron transport layer;
(3) Preparing a perovskite structure photoactive layer on the lead-doped tin oxide multilayer gradient energy level electron transport layer through a knife coating process;
(4) Preparing a hole transport material layer on the perovskite structure photoactive layer through a spin coating process;
(5) Depositing a back electrode on the hole transport material layer by adopting a thermal evaporation method;
the lead-doped tin oxide nanocrystalline film is prepared by the following steps:
a. Preparing a lead ion solution: dissolving a lead ion precursor in deionized water to obtain a lead ion solution with the concentration of 0.0003-0.009 mol/L;
b. preparing tin ion solution: dissolving a tin ion precursor in deionized water to obtain a tin ion solution with the concentration of 0.1-0.3 mol/L;
c. Preparing a lead-doped tin oxide nano solution: slowly dripping the lead ion solution into the tin ion solution at the temperature of 0-5 ℃ and stirring, heating the solution to the temperature of 70-90 ℃ after uniformly stirring, and introducing air into the solution for 1-2 hours to obtain the lead-doped tin oxide nano solution;
d. Preparing a lead-doped tin oxide nanocrystalline film: and (3) the obtained lead-doped tin oxide nano solution is subjected to a blade coating, spraying or spin coating method to obtain the lead-doped tin oxide nano crystal film.
2. The method for manufacturing a perovskite solar cell based on a multi-layered gradient energy electron transport layer according to claim 1, wherein the thickness of each electron transport layer is 15 nm, the thickness of the organic-inorganic perovskite photoactive layer is 400 nm, the thickness of the hole transport layer is 100 nm, and the thickness of the back electrode is 60 nm.
3. The method for preparing the perovskite solar cell based on the multilayer gradient energy electron transport layer according to claim 1, wherein the substrate is glass or flexible plastic, the transparent conductive layer is made of fluorine-doped tin oxide or indium-doped tin oxide, and the perovskite structure photoactive layer is made of one of MAPbI 3、FAPbI3、MAPbBr3、FAPbBr3、CsPbI3 and CsPbBr 3; the hole transport layer is made of one or two selected from polythiophene, 2', 7' -tetra [ N, N-di (4-methoxyphenyl) amino ] -9,9' -spirobifluorene, cuSCN, WO 3 and MoO 3; the material of the back electrode is silver, aluminum, gold, copper or alloy material of silver, aluminum, gold and copper.
4. The method for preparing a perovskite solar cell based on a multi-layered gradient energy electron transport layer according to claim 1, wherein the specific steps of step d are: preparing a lead-doped tin oxide nanocrystalline film by adopting a spin coating method, wherein the spin coating rate is 3000-5000 rpm, and the heat treatment is carried out for 30 minutes at 100-150 ℃.
5. The method for preparing the perovskite solar cell based on the multilayer gradient energy electron transport layer according to claim 1, wherein the lead ion precursor is anhydrous lead acetate or lead acetate trihydrate, and the tin ion precursor is one of anhydrous tin tetrachloride, anhydrous stannous chloride and anhydrous stannous chloride.
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