CN112186109A - 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 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 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 27
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 239000004065 semiconductor Substances 0.000 claims abstract description 15
- 238000000137 annealing Methods 0.000 claims abstract description 9
- 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 27
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000003570 air Substances 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000007789 gas Substances 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
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000144 PEDOT:PSS Polymers 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 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 6
- 238000000034 method Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 17
- 239000011521 glass Substances 0.000 description 9
- 238000005424 photoluminescence Methods 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000012046 mixed solvent Substances 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000012296 anti-solvent Substances 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
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 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
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000005259 measurement 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
- 230000000630 rising effect Effects 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 thin film, which comprises the following steps: 1) spin coating a perovskite solution onto a semiconductor layer of a substrate having the semiconductor layer, the perovskite solution having a solvent of one or more of DMF, DMSO, γ -GBL; 2) dripping an inverse solvent before the spin coating is finished; 3) and after the spin coating is finished, annealing the substrate for 5-60 minutes at 80-120 ℃ in a gas environment with the pressure of 0.1-10Mpa to obtain the perovskite thin film. The perovskite thin film prepared by the method has good stability and improved photoelectric property, 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 perovskite thin film preparation method, a prepared perovskite thin film and a perovskite solar cell.
Background
At present, the method for preparing a dense perovskite thin film generally comprises the steps of firstly preparing a perovskite solution, then dripping the solution on a substrate for spin coating, and dripping an anti-solvent (such as toluene, isopropanol, ether and the like) in the rotating process to induce the perovskite to be rapidly crystallized so as to prepare the dense perovskite thin film.
Although this method can produce a dense perovskite thin film, it has the following problems: (1) the film has poor stability, is easy to decompose under the action of water and oxygen in atmospheric environment, and is also easy to decompose at high temperature even under the packaging condition; (2) the film has smaller grain size and larger defect density, which is not beneficial to improving the photoelectric conversion efficiency. The above two factors limit the preparation of large-grain perovskite thin films by the reverse solvent rapid-induced perovskite crystallization film formation technology, and therefore, the above technology still needs 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 and large in small crystal grain defect density, so that the improvement of the photoelectric conversion efficiency is not facilitated, 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 thin film comprises the following steps:
1) spin coating a perovskite solution onto a semiconductor layer of a substrate having the semiconductor layer, the perovskite solution having a solvent of one or more of Dimethylformamide (DMF), Dimethylsulfoxide (DMSO), gamma-butyrolactone (gamma-GBL);
2) dripping an inverse solvent before the spin coating is finished;
3) and after the spin coating is finished, annealing the substrate for 5-60 minutes at 80-120 ℃ in a gas environment with the pressure of 0.1-10Mpa to obtain the perovskite thin film.
Annealing is carried out in the high-pressure gas environment, the grain size of the film is effectively increased, the defect density is effectively reduced, and the photoelectric property of the film is improved; in addition, the stability of the film annealed in the high-pressure gas environment is also improved.
In the step 1), the concentration of the perovskite solution is 1-1.5 mol/L.
In the step 1), the substrate is an FTO or ITO transparent electrode, and the semiconductor layer is TiO2、SnO2ZnO, PEDOT: PSS or NiO, and the thickness of the semiconductor layer is 30-50 nm.
In the step 2), the inversion solvent is one or more of isopropanol, ether, toluene and chloroform, and the dropwise addition of the inversion solvent is carried out 5-15 seconds before the end of the spin coating.
In the step 3), the gas is one or more of nitrogen, argon, helium and air.
In the step 3), the temperature rising speed of 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.
Has the advantages that: in the process of preparing the film by using the perovskite solution, 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 can be reduced, the quality of the perovskite film can be improved, and the stability of the film can be 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 photoluminescence intensity and average grain size of the perovskite thin film of the present invention;
FIG. 3 is a j-v plot of a perovskite thin film of the present invention;
FIG. 4 is a parameter diagram 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 present invention.
Detailed Description
The technical solution of the present invention is described in detail by the following examples, but the scope of the present invention is not limited to the examples.
Example 1
1) First perovskite (CH)3NH3PbI3) Solution spin coating of 40nm thick TiO onto FTO conductive glass2On the semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, the solvent is a mixed solvent of DMF and DMSO, and the volume ratio of the DMF to the DMSO is 5: 1;
2) then, isopropanol and diethyl ether which are used as inversion solvents are dripped into the solution 10 seconds before the spin coating is stopped, wherein the volume fraction of the isopropanol is 0.1 percent;
3) after the spin coating is finished, the substrate is placed in a high-pressure tube furnace (OTF-1200X-HP-55, the Co-Federal Crystal Material technology Co., Ltd., the same below), argon is filled to make the air pressure reach 2MPa, and then the substrate is heated to 100 ℃ at the heating rate of 10 ℃/min and is maintained for 30 minutes, so that the perovskite thin film 1 is prepared.
The perovskite solar cell 1 is manufactured by a conventional method using the perovskite thin film 1.
Example 2
1) Firstly, the perovskite solution is coated on the FTO conductive glass by spin coating, and TiO with the thickness of 40nm is coated on the FTO conductive glass2On the semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, the solvent is a mixed solvent of DMF and DMSO, and the volume ratio of the DMF to the DMSO is 5: 1;
2) then, isopropanol and diethyl ether which are used as inversion solvents are dripped into the solution 10 seconds before the spin coating is stopped, wherein the volume fraction of the isopropanol is 0.1 percent;
3) after the spin coating is finished, the substrate is placed in a high-pressure tube furnace, argon is filled into the high-pressure tube furnace, the air pressure is enabled to reach 4MPa, then the substrate is heated to 100 ℃ according to the heating rate of 10 ℃/min, and the temperature is maintained for 30 minutes, so that the perovskite thin film 2 is prepared.
The perovskite solar cell 2 is manufactured by a conventional method using the perovskite thin film 2.
Example 3
1) Firstly, the perovskite solution is coated on the FTO conductive glass by spin coating, and TiO with the thickness of 40nm is coated on the FTO conductive glass2On the semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, the solvent is a mixed solvent of DMF and DMSO, and the volume ratio of the DMF to the DMSO is 5: 1;
2) then, isopropanol and diethyl ether which are used as inversion solvents are dripped into the solution 10 seconds before the spin coating is stopped, wherein the volume fraction of the isopropanol is 0.1 percent;
3) after the spin coating is finished, the substrate is placed in a high-pressure tube furnace, argon is filled into the high-pressure tube furnace, the air pressure is enabled to reach 6MPa, then the substrate is heated to 100 ℃ according to the heating rate of 10 ℃/min, and the temperature is maintained for 30 minutes, so that the perovskite thin film 3 is prepared.
The perovskite solar cell 3 is manufactured by a conventional method using the perovskite thin film 3.
Example 4
1) Firstly, the perovskite solution is coated on the FTO conductive glass by spin coating, and TiO with the thickness of 40nm is coated on the FTO conductive glass2On the semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, the solvent is a mixed solvent of DMF and DMSO, and the volume ratio of the DMF to the DMSO is 5: 1;
2) then, isopropanol and diethyl ether which are used as inversion solvents are dripped into the solution 10 seconds before the spin coating is stopped, wherein the volume fraction of the isopropanol is 0.1 percent;
3) after the spin coating is finished, the substrate is placed in a high-pressure tube furnace, argon is filled into the high-pressure tube furnace, the air pressure is made to reach 8MPa, the substrate is heated to 100 ℃ at the heating rate of 10 ℃/min, and the temperature is maintained for 30 minutes, so that the perovskite thin film 4 is prepared.
The perovskite solar cell 4 is manufactured by a conventional method using the perovskite thin film 4.
Example 5
1) Firstly, the perovskite solution is coated on the FTO conductive glass by spin coating, and TiO with the thickness of 40nm is coated on the FTO conductive glass2On the semiconductor layer (dense layer); wherein the concentration of the perovskite solution is 1.4mol/L, the solvent is a mixed solvent of DMF and DMSO, and the volume ratio of the DMF to the DMSO is 5: 1;
2) then, isopropanol and diethyl ether which are used as inversion solvents are dripped into the solution 10 seconds before the spin coating is stopped, wherein the volume fraction of the isopropanol is 0.1 percent;
3) after the spin coating is finished, the substrate is placed in a high-pressure tube furnace, argon is filled into the high-pressure tube furnace, the air pressure is 10MPa, the substrate is heated to 100 ℃ at the heating rate of 10 ℃/min, and the temperature is maintained for 30 minutes, so that the perovskite thin film 5 is prepared.
The perovskite solar cell 5 is manufactured by a conventional method using the perovskite thin film 5.
Performance tests were performed on the perovskite thin films and perovskite solar cells prepared in examples 1, 2, 3, 4 and 5 above, respectively.
And (3) testing conditions are as follows: the surface morphology of the film was photographed by 3NTEGRA (NT-MDT) atomic force microscope, and LabR was usedThe photoluminescence spectra were measured on an AM HR Evolution (Horiba) spectrometer and in situ XRD measurements were performed on a Bruker (D8 ADVANCE) x-ray diffractometer. The simulated illumination conditions of the Newport Oriel Solar simulator (3A Class AAA, 94023A) are AM 1.5G and 1000 mW/cm2The j-v curve was measured using a digital master meter, type Keithly 2400, all tests being carried out in an air environment. The results are shown in table 1 and fig. 1 to 5.
TABLE 1
| Annealing atmosphere | 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 in a stress environment is significantly larger than that of the conventional stress (0.1 MPa), which is advantageous for the efficiency improvement of the battery device.
FIG. 2 is a graph of Photoluminescence (PL) intensity and average grain size of the perovskite thin film of the present invention. Generally, the higher the photoluminescence intensity, the less the film defects, and it is seen from the figure that the luminescence intensity increases first and then decreases with the change of pressure, reaching a maximum value at 6MPa and a minimum value at the conventional 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 present invention. The graph shows the performance of solar cells prepared from 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 parameter diagram of a battery device using the perovskite thin film of the present invention. The figure 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 present invention. The figure shows that the organic perovskite thin film MAPbI is annealed in a pressure environment3Can bear 300oThe high temperature of C does not decompose, and is far higher than the temperature which the film can bear under normal pressure.
As noted above, while the present invention has been shown and described with reference to certain preferred embodiments, it is not to be construed as limited thereto. Various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. The preparation method of the perovskite thin film is characterized by comprising the following steps:
1) spin coating a perovskite solution onto a semiconductor layer of a substrate having the semiconductor layer, the perovskite solution having a solvent of one or more of DMF, DMSO, γ -GBL;
2) dripping an inverse solvent before the spin coating is finished;
3) and after the spin coating is finished, annealing the substrate for 5-60 minutes at 80-120 ℃ in a gas environment with the pressure of 0.1-10Mpa to obtain the perovskite thin film.
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 1.5 mol/L.
3. The method for producing a perovskite thin film as claimed in claim 1, wherein in the step 1), the substrate is an FTO or ITO transparent electrode, and the semiconductor layer is TiO2、SnO2ZnO, PEDOT: PSS or NiO, and the thickness of the semiconductor layer is 30-50 nm.
4. The method for producing a perovskite thin film according to claim 1, wherein in the step 2), the inversion solvent is one or more of isopropyl alcohol, ethyl ether, toluene and chloroform, and the dropping of the inversion solvent is performed 5 to 15 seconds before the end of the spin coating.
5. 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.
6. The method for producing a perovskite thin film according to claim 1, wherein the temperature increase rate of annealing in step 3) is 5 to 15 ℃/min.
7. A perovskite thin film produced by the method for producing a perovskite thin film according to any one of claims 1 to 6.
8. A perovskite solar cell comprising the perovskite thin film according to claim 7.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113540270A (en) * | 2021-06-30 | 2021-10-22 | 杭州电子科技大学 | Method for obtaining flat, uniform and compact perovskite film |
| CN113571650A (en) * | 2021-07-07 | 2021-10-29 | 常州大学 | Device and method for preparing perovskite film through 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113540270A (en) * | 2021-06-30 | 2021-10-22 | 杭州电子科技大学 | Method for obtaining flat, uniform and compact perovskite film |
| 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 |
| CN113571650A (en) * | 2021-07-07 | 2021-10-29 | 常州大学 | Device and method for preparing perovskite film through constant high-pressure annealing |
| 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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