CN112186109B - Perovskite thin film preparation method, perovskite thin film and perovskite solar cell - Google Patents
Perovskite thin film preparation method, perovskite thin film and perovskite solar cell Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000004528 spin coating Methods 0.000 claims abstract description 26
- 239000010408 film Substances 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 239000004065 semiconductor Substances 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 37
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 239000003570 air Substances 0.000 claims description 4
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims description 2
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000000630 rising effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000005424 photoluminescence Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 239000012046 mixed solvent Substances 0.000 description 5
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000012296 anti-solvent Substances 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
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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
- H10K30/30—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains
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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
- H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
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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 preparation method of a perovskite film, which comprises the following steps: 1) Spin-coating a perovskite solution onto a semiconductor layer of a substrate with the semiconductor layer, wherein the perovskite solution is one or more of DMF, DMSO and gamma-GBL; 2) Dropping an inverse solvent before spin coating is finished; 3) And after spin coating, annealing the substrate in a gas environment with the pressure of 0.1-10Mpa at 80-120 ℃ for 5-60 minutes to prepare the perovskite film. The perovskite thin film prepared by the method has good stability and improved photoelectric performance, and is suitable for being used as a material of a perovskite solar cell.
Description
Technical Field
The invention relates to the technical field of solar cells, in particular to a preparation method of a perovskite thin film, the prepared perovskite thin film and a perovskite solar cell.
Background
At present, a method for preparing a dense perovskite film is generally that a perovskite solution is firstly prepared, then dripped on a substrate for spin coating, and an anti-solvent (anti-solvent) such as toluene, isopropanol, diethyl ether and the like is dripped in the rotating process to induce the perovskite to be rapidly crystallized, so that the dense perovskite film is prepared.
Although this method can produce dense perovskite thin films, it also has the following problems: (1) The film has poor stability, is easy to decompose under the action of water and oxygen in the atmosphere, and is easy to decompose at high temperature even under the packaging condition; (2) The grain size of the film is smaller, the defect density is larger, and the improvement of photoelectric conversion efficiency is not facilitated. The above two factors limit the rapid induction of perovskite crystallization film formation techniques by inversion solvents to produce large grain perovskite films, and therefore, the above techniques have yet to be improved and developed.
Disclosure of Invention
In order to solve the problems that the perovskite thin film prepared by the prior art is poor in stability, small in crystal grain and large in defect density, and is unfavorable for improving the photoelectric conversion efficiency, the invention provides a preparation method of the perovskite thin film, the perovskite thin film and a perovskite solar cell.
The preparation method of the perovskite film comprises the following steps:
1) Spin-coating a perovskite solution onto a semiconductor layer of a substrate with the semiconductor layer, wherein the solvent of the perovskite solution is one or more of Dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and gamma-butyrolactone (gamma-GBL);
2) Dropping an inverse solvent before spin coating is finished;
3) And after spin coating, annealing the substrate in a gas environment with the pressure of 0.1-10Mpa at 80-120 ℃ for 5-60 minutes to prepare the perovskite film.
Annealing is carried out in the high-pressure gas environment, so that the grain size of the film is effectively increased, the defect density is effectively reduced, and the photoelectric performance of the film is improved; in addition, the stability of the annealed film in the high-pressure gas environment is also improved.
In step 1), the concentration of the perovskite solution is 1-1.5mol/L.
In the step 1), the substrate is an FTO or ITO transparent electrode, and the semiconductor layer is TiO 2 、SnO 2 ZnO, PEDOT: the thickness of the semiconductor layer is 30-50nm, which is one of PSS and NiO.
In the step 2), the inversion solvent is one or more of isopropanol, diethyl ether, toluene and chloroform, and the dripping of the inversion solvent is performed 5-15 seconds before the spin coating is finished.
In the step 3), the gas is one or more of nitrogen, argon, helium and air.
In the step 3), the heating rate of the annealing is 5-15 ℃/min.
The invention provides a perovskite thin film, which is prepared by using the preparation method of the perovskite thin film.
The invention provides a perovskite solar cell, which comprises the perovskite thin film.
The beneficial effects are that: in the process of preparing the perovskite film by using the perovskite solution, the high-pressure gas is used as a pressurizing medium, and the film is annealed in a high-pressure environment, so that the grain size can be effectively increased, the defect density is reduced, the quality of the perovskite film is improved, and the stability of the film is improved; the photoelectric property of the film is also improved, namely the efficiency of the perovskite solar cell is improved, wherein the filling factor and the short-circuit current in the performance parameters of the device are obviously improved.
Drawings
FIG. 1 is an atomic force microscope image of a perovskite thin film of the present invention;
FIG. 2 is a graph of the photoluminescence intensity and average grain size of a perovskite thin film of the invention;
FIG. 3 is a j-v plot of a perovskite thin film of the invention;
FIG. 4 is a graph of various parameters of a battery device using the perovskite thin film of the present invention;
FIG. 5 is an x-ray diffraction pattern of a perovskite thin film of the invention.
Detailed Description
The technical scheme of the present invention is described in detail by examples below, but the scope of the present invention is not limited to the examples.
Example 1
1) First, perovskite (CH 3 NH 3 PbI 3 ) TiO with thickness of 40nm spin-coated on FTO conductive glass 2 A semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, a mixed solvent of DMF and DMSO is used as the solvent, and the volume ratio of DMF to DMSO is 5:1, a step of;
2) Then, isopropanol and diethyl ether as inversion solvents were added dropwise 10 seconds before spin coating was stopped, the volume fraction of isopropanol being 0.1%;
3) After spin coating was completed, the substrate was placed in a high-pressure tube furnace (OTF-1200X-HP-55, hefei Kogyo materials technology Co., ltd., hereinafter the same), then argon was introduced to bring the gas pressure to 2MPa, and then heated to 100℃at a heating rate of 10℃per minute and maintained for 30 minutes to prepare perovskite thin film 1.
The perovskite solar cell 1 was manufactured in a conventional manner using the perovskite thin film 1.
Example 2
1) First spin-coating perovskite solution onto FTO conductive glass to obtain TiO with thickness of 40nm 2 A semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, a mixed solvent of DMF and DMSO is used as the solvent, and the volume ratio of DMF to DMSO is 5:1, a step of;
2) Then, isopropanol and diethyl ether as inversion solvents were added dropwise 10 seconds before spin coating was stopped, the volume fraction of isopropanol being 0.1%;
3) After spin coating, the substrate was placed in a high-pressure tube furnace, then argon was introduced to a gas pressure of 4MPa, and then heated to 100 ℃ at a heating rate of 10 ℃/min and maintained for 30 minutes to prepare a perovskite thin film 2.
Perovskite solar cell 2 was fabricated in a conventional manner using perovskite thin film 2.
Example 3
1) First spin-coating perovskite solution onto FTO conductive glass to obtain TiO with thickness of 40nm 2 A semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, a mixed solvent of DMF and DMSO is used as the solvent, and the volume ratio of DMF to DMSO is 5:1, a step of;
2) Then, isopropanol and diethyl ether as inversion solvents were added dropwise 10 seconds before spin coating was stopped, the volume fraction of isopropanol being 0.1%;
3) After spin coating, the substrate was placed in a high-pressure tube furnace, then argon was introduced to a gas pressure of 6MPa, and then heated to 100 ℃ at a heating rate of 10 ℃/min and maintained for 30 minutes to prepare a perovskite thin film 3.
The perovskite solar cell 3 is manufactured in a conventional manner using the perovskite thin film 3.
Example 4
1) First spin-coating perovskite solution onto FTO conductive glass to obtain TiO with thickness of 40nm 2 A semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, a mixed solvent of DMF and DMSO is used as the solvent, and the volume ratio of DMF to DMSO is 5:1, a step of;
2) Then, isopropanol and diethyl ether as inversion solvents were added dropwise 10 seconds before spin coating was stopped, the volume fraction of isopropanol being 0.1%;
3) After spin coating, the substrate was placed in a high-pressure tube furnace, then argon was introduced to a gas pressure of 8MPa, and then heated to 100 ℃ at a heating rate of 10 ℃/min and maintained for 30 minutes to prepare a perovskite thin film 4.
The perovskite solar cell 4 is manufactured in a conventional manner using the perovskite thin film 4.
Example 5
1) First spin-coating perovskite solution onto FTO conductive glass to obtain TiO with thickness of 40nm 2 A semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, a mixed solvent of DMF and DMSO is used as the solvent, and the volume ratio of DMF to DMSO is 5:1, a step of;
2) Then, isopropanol and diethyl ether as inversion solvents were added dropwise 10 seconds before spin coating was stopped, the volume fraction of isopropanol being 0.1%;
3) After spin coating, the substrate was placed in a high-pressure tube furnace, then argon was introduced to a gas pressure of 10MPa, and then heated to 100 ℃ at a heating rate of 10 ℃/min, and maintained for 30 minutes, to prepare a perovskite thin film 5.
The perovskite solar cell 5 is manufactured in a conventional manner using the perovskite thin film 5.
The perovskite thin films and perovskite solar cells prepared in examples 1, 2, 3, 4 and 5 above were subjected to performance tests, respectively.
Test conditions: the surface morphology of the films was photographed with a 3NTEGRA (NT-MDT) atomic force microscope, the photoluminescence spectra were tested with a LabRAM HR Evolution (Horiba) spectrometer, and the in situ XRD test was performed with a Bruker (D8 ADVANCE) x-ray diffractometer. Newport Oriel Solar (3A Class AAA, 94023A) solar simulator simulates the illumination conditions of AM 1.5G,1000 mW/cm 2 The j-v curve was measured using a Keithly 2400 model digital master, and all tests were performed in an air environment. The results are shown in Table 1, FIGS. 1-5.
TABLE 1
| Annealing air pressure | Average grain size (nm) | PL luminous intensity (a.u.) | Phase transition temperature (. Degree. C.) | |
| Example 1 | 2MPa | 833 | 8000 | 40 |
| Example 2 | 4MPa | 1083 | 22500 | 45 |
| Example 3 | 6MPa | 1182 | 25000 | 55 |
| Example 4 | 8MPa | 825 | 16000 | 55 |
| Example 5 | 10MPa | 706 | 5000 | 60 |
FIG. 1 is an atomic force microscope image of a perovskite thin film of the present invention. It can be seen that the surface grain size of the film annealed under the pressure environment is significantly larger than that of the conventional pressure (0.1 MPa), which is advantageous for the improvement of the efficiency of the battery device.
FIG. 2 is a graph of Photoluminescence (PL) intensity and average grain size of a perovskite thin film of the invention. In general, the larger the photoluminescence intensity means the less defects of the film, and it is understood that the luminescence intensity increases and decreases with the change of pressure, and reaches a maximum value at 6MPa and a minimum value at a normal pressure (0.1 MPa). In addition, the average grain size of the film is also shown, with a trend consistent with photoluminescence.
FIG. 3 is a j-v plot of a perovskite thin film of the invention. The graph shows the performance of solar cells prepared from thin films annealed at different pressures. It can be seen from the figure that the solar cell prepared by annealing at 6MPa has the highest efficiency.
Fig. 4 is a graph of various parameters of a battery device using the perovskite thin film of the present invention. The graph shows the performance parameters of solar cells prepared by annealing at different pressures.
FIG. 5 is an x-ray diffraction pattern of a perovskite thin film of the invention. The figure shows annealing under pressure, organic perovskite thin film MAPbI 3 Can bear 300 percent o C is high in temperature without decomposition and is far higher than the film can bear under normal pressure.
As described above, although the present invention has been shown and described with reference to certain preferred embodiments, it is not to be construed as limiting the invention itself. Various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. The preparation method of the perovskite thin film is characterized by comprising the following steps of:
1) Spin-coating a perovskite solution onto a semiconductor layer of a substrate with the semiconductor layer, wherein the perovskite solution is one or more of DMF, DMSO and gamma-GBL;
2) Dropping an inverse solvent before spin coating is finished;
3) Annealing the substrate in a gas environment with the pressure of 2-10MPa at 80-120 ℃ for 5-60 minutes after spin coating is finished to prepare a perovskite film;
in the step 2), the inversion solvent is one or more of isopropanol, diethyl ether and chloroform, and the dripping of the inversion solvent is carried out 5-15 seconds before the spin coating is finished;
in the step 3), the temperature rising speed of the annealing is 5-15 ℃/min.
2. The method for producing a perovskite thin film according to claim 1, wherein in step 1), the concentration of the perovskite solution is 1 to 1.5mol/L.
3. The method of claim 1, wherein in step 1), the substrate is an FTO or ITO transparent electrode, and the semiconductor layer is TiO 2 、SnO 2 ZnO, PEDOT: the thickness of the semiconductor layer is 30-50nm, which is one of PSS and NiO.
4. The method for producing a perovskite thin film according to claim 1, wherein in the step 3), the gas is one or more of nitrogen, argon, helium, and air.
5. A perovskite thin film, characterized in that it is produced by using the production method of a perovskite thin film according to any one of claims 1 to 4.
6. A perovskite solar cell comprising the perovskite thin film of claim 5.
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| CN113540270B (en) * | 2021-06-30 | 2023-06-30 | 杭州电子科技大学 | Method for obtaining flat, uniform and compact perovskite film |
| CN113571650B (en) * | 2021-07-07 | 2023-08-22 | 常州大学 | Device and method for preparing perovskite film by constant high-pressure annealing |
| CN115465885A (en) * | 2022-09-22 | 2022-12-13 | 南通南京大学材料工程技术研究院 | Highly oriented MAPbI 3 Preparation method of perovskite thin film and MAPbI 3 Perovskite thin film |
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| CN105428539A (en) * | 2016-01-18 | 2016-03-23 | 昆明学院 | Preparation method for perovskite solar cell absorption layer capable of improving photoelectric properties through controlling annealing pressure intensity atmosphere |
| CN106784322A (en) * | 2016-12-14 | 2017-05-31 | 北京大学深圳研究生院 | A kind of perovskite thin film and preparation method thereof and perovskite solar cell |
| CN111435707A (en) * | 2019-07-10 | 2020-07-21 | 杭州纤纳光电科技有限公司 | Method for improving film forming quality of perovskite thin film and perovskite solar cell |
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| CN105428539A (en) * | 2016-01-18 | 2016-03-23 | 昆明学院 | Preparation method for perovskite solar cell absorption layer capable of improving photoelectric properties through controlling annealing pressure intensity atmosphere |
| CN106784322A (en) * | 2016-12-14 | 2017-05-31 | 北京大学深圳研究生院 | A kind of perovskite thin film and preparation method thereof and perovskite solar cell |
| CN111435707A (en) * | 2019-07-10 | 2020-07-21 | 杭州纤纳光电科技有限公司 | Method for improving film forming quality of perovskite thin film and perovskite solar cell |
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