CN107994123B - Perovskite type solar cell and preparation method thereof - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 22
- 230000005525 hole transport Effects 0.000 claims abstract description 11
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 24
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 7
- XDXWNHPWWKGTKO-UHFFFAOYSA-N 207739-72-8 Chemical compound C1=CC(OC)=CC=C1N(C=1C=C2C3(C4=CC(=CC=C4C2=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC(=CC=C1C1=CC=C(C=C13)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 XDXWNHPWWKGTKO-UHFFFAOYSA-N 0.000 claims description 6
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 6
- YSHMQTRICHYLGF-UHFFFAOYSA-N 4-tert-butylpyridine Chemical compound CC(C)(C)C1=CC=NC=C1 YSHMQTRICHYLGF-UHFFFAOYSA-N 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 229940046892 lead acetate Drugs 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical group [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000000137 annealing Methods 0.000 claims 1
- 238000002202 sandwich sublimation Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 abstract 2
- 150000001242 acetic acid derivatives Chemical class 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 12
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- ZIQVBOWGWNZWAQ-UHFFFAOYSA-N lead;pentane-2,4-dione Chemical compound [Pb].CC(=O)CC(C)=O ZIQVBOWGWNZWAQ-UHFFFAOYSA-N 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
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- 238000005137 deposition process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000013082 photovoltaic technology Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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- 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
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
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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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- 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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- 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
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Abstract
The invention discloses a perovskite type solar cell and a preparation method thereof. The perovskite type solar cell comprises FTO, an electron transport layer, perovskite, a hole transport layer and electrodes; wherein the perovskite layer is prepared by a simple close-space sublimation method. The material constituting the perovskite is selected from at least one of acetylacetone metal salts and acetates. The method not only reduces the cost, but also can prepare at low temperature, greatly improves the film coverage, can be used for manufacturing large-area devices, and provides a feasible method for future industrialization.
Description
Technical Field
The invention belongs to the field of perovskite solar cells, and relates to a perovskite solar cell and a preparation method thereof.
Background
Recently, organic-inorganic hybrid perovskite solar cells are highly valued in the field of photovoltaic technology, and perovskite materials are considered as ideal photovoltaic materials due to the advantages of high carrier mobility, low exciton binding energy, high absorption coefficient and appropriate band gap. With the benefit of contributions from chemical, material and physical communities, the conversion efficiency of perovskite solar cells has increased dramatically from the originally reported 3.8% to now 22.1% in as little as seven years.
The quality of perovskite thin films plays a crucial role in the performance of perovskite batteries, and various methods for improving the quality of perovskite thin films have been reported in the literature, for example: one-step spin coating, continuous deposition, co-evaporation, gas phase assisted liquid phase. For one-step spin coating, the solvent evaporates when the spin coater is rotated at high speed to form perovskite grains, in which case the solvent evaporates rapidly, PbI2And CH3NH3The rapid reaction of I makes it difficult to control the growth of perovskite grains, induces the formation of pinholes, and ultimately results in low coverage of the perovskite thin film. Using PbCl2Or Pb (Ac)2The perovskite film as a lead source can be smoother and better in coverage, but can release products which are unfavorable to perovskite film formation in the film forming processThe purity of the film is affected.
Therefore, Gra employs a continuous deposition process by Tzeel et al. This involves firstly a lead source PbI2Then PbI, followed by2Immersion in CH3NH3I or in PbI2Spin coating CH on film3NH3I solution, producing perovskite crystals. This approach has been successfully applied in porous nanostructures, but is difficult to apply to planar perovskite solar cells because of the absence of a scaffold, CH3NH3The I molecule is to penetrate into the compact PbI2Much harder in thin films, which leads to PbI2Incomplete reaction of (2).
Involving co-sublimation of CH under high vacuum conditions in a co-evaporation process3NH3I and PbI2Organic and inorganic materials are co-deposited. This method can give dense and pore-free high quality perovskite thin films. However, this high vacuum technique can be time and energy intensive.
To solve this problem, a method of steam-assisting the solution is proposed, where CH3NH3I vapor and Pre-deposition of PbI2The film reacts to generate a perovskite active layer, and perovskite crystal grains of 1 micron can be obtained by adopting the method. However, it is difficult to precisely control sublimed CH in this method3NH3Amount of I steam, resulting in PbI2Especially for large area devices.
Neither the above-mentioned one-step spin coating method nor the continuous deposition method nor the vapor-assisted solution method can produce high-quality large-area devices, and the co-evaporation method involves high vacuum and thus takes much effort and time.
Disclosure of Invention
The invention aims to provide a perovskite solar cell and a preparation method of the perovskite solar cell.
In order to achieve the above object, the technical solution of the present invention is as follows,
the preparation method of the perovskite type solar cell comprises the following steps:
1) respectively placing the MAI, the lead source material and the MACl in a graphite box for flattening;
2) placing the pressed MAI in the step 1) in the center of a hot plate, placing FTO glass coated with a compact layer in a rotary mode in the center of a mask plate, placing the surface coated with the compact layer and the pressed MAI in a face-to-face mode at a distance of 1-3cm, raising the temperature of the hot plate to 120-150 ℃ after vacuumizing to 0.1MPa, and closing a temperature switch after 20-30min to obtain a sheet with the MAI layer;
3) after the temperature is reduced, placing the pressed lead source material in the step 1) in the center of a hot plate, continuously placing the sheet in the step 2) on the lead source material according to the method, then raising the temperature of the hot plate to 110-130 ℃ under the normal pressure state, and closing a temperature switch after 30-40 min;
4) after the temperature is reduced, placing the MAI pressed in the step 1) in the center of a hot plate, continuously placing the sheet in the step 3) according to the method, raising the temperature of the hot plate to 130-150 ℃ after the vacuum pumping reaches 0.1MPa, and closing a temperature switch after 30-40 min;
5) after the temperature is reduced, the wafer is continuously placed on the MACl pressed in the step 1) according to the method, the vacuum pumping is carried out until the vacuum pressure reaches 0.1MPa, the temperature of the hot plate is increased to 100-120 ℃, the temperature switch is closed after 5-10min, and then the wafer is annealed at 100-110 ℃, so that the growth of the perovskite layer is completed.
The lead source material is lead acetylacetonate or lead acetate.
And 2) placing the surface with the dense layer and the pressed MAI in a face-to-face manner at a distance of 2 cm.
The perovskite type solar cell prepared by the method sequentially comprises an FTO, an electron transport layer, a perovskite layer, a hole transport layer and an electrode from bottom to top.
The thickness of the perovskite layer is 300-400 nm.
The material of the electron transport layer is TiO2。
The materials of the hole transport layer are spiro-OMeTAD, 4-tert-butylpyridine, acetonitrile solution of lithium bis (trifluoromethanesulfonyl) imide, FK102 salt and chlorobenzene.
The dosage ratio of spiro-OMeTAD, 4-tert-butylpyridine, lithium bistrifluoromethanesulfonimide, FK102 salt and chlorobenzene is 0.1 g: 9.6. mu.L: 13.6 mg: 21 mg: 1mL, wherein the dosage ratio of the acetonitrile to the lithium bis (trifluoromethanesulfonyl) imide is 1 mL: 170 mg.
The material of the electrode is gold or silver.
Wherein the perovskite layer is grown by using a simple close-space sublimation method.
The thickness of the FTO is about 450nm, the thickness of the TiO2 dense layer is about 10nm-50nm, the thickness of the perovskite is about 300nm-400nm, the thickness of the hole transport layer Spiro-OMETAD is 200-300nm, and the thickness of the Ag or Au electrode is 120 nm.
spiro-OMeTAD of
2,2 ', 7,7 ' -tetrakis (N, N-p-dimethoxy-phenylaminono) -9,9 ' -spirobifluorene.
The film forming principle of the method is as follows:
firstly, a thin layer of MAI is deposited on the FTO glass, so that the generated perovskite grows in full grains, and if the layer of MAI is not deposited, the perovskite grains grow in a needle shape, which is not beneficial to the transmission of current carriers. After lead acetate or lead acetylacetonate is deposited thereon, the sublimed MAI reacts therewith to form a perovskite thin film of MAPbI 3. And sublimating a thin MACl layer to reduce the formation of surface defects and make the film smoother.
In the perovskite type solar cell, the preparation methods of the electron transport layer and the Ag or Au electrode are conventional methods and can be prepared according to the existing preparation method.
Reference may be made to the following documents:
Highly Efficient Perovskite Solar Cells with Substantial Reduction of Lead Content.Liu C,Fan J,Li H,et al.Scientific reports,2016,6.
compared with the prior art, the invention has the following advantages and beneficial effects:
(1) after the electron transmission layer is prepared, the perovskite is generated by a near space sublimation method. Firstly, placing a source on a heating plate, placing FTO glass on a mask plate, placing the source and the FTO face to face at a distance of 2cm, vacuumizing, heating, and sublimating the material layer by layerAnd finally, carrying out a layer of modification on the FTO glass to ensure that the perovskite reaction is more complete. The method can be used for preparing the thin film at low temperature (the highest temperature is not more than 150 ℃), greatly reduces the defects of the thin film, greatly improves the coverage of the thin film, can be used for manufacturing large-area devices, and provides a feasible method for future industrialization. Compared with the PbI used by high vacuum evaporation, the source material of the invention2Although the price of lead acetylacetonate is about PbI24 times of the amount of the lead acetylacetonate, the method disclosed by the invention has the advantages of extremely small using amount, capability of recycling, capability of greatly reducing the production cost and great significance for the practical application of the perovskite solar cell. The preparation time of the invention is short, the evaporation at high temperature needs longer time for cooling, but the invention only needs to cool at the temperature which is not more than 150 ℃, the preparation cooling time of each layer can be saved by about 30min, and the whole process saves a great amount of time.
(2) The method has highly uniform perovskite thin film, and can be obtained by simply controlling the thicknesses of the lead acetylacetonate and the MAI film, the reaction time of the MAI steam and the distance of a sublimation space.
Drawings
Fig. 1 is a structural view of a battery of examples 1 and 2.
Figure 2 is an XRD profile for examples 1 and 2.
FIG. 3 is a J-V curve for examples 1 and 2.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1 preparation of perovskite solar cell with lead source of acetylacetone lead by simple close-space sublimation method
1) Preparation of the Electron transport layer
Preparing a compact film layer:
the preparation is carried out according to a conventional method, and the compact membrane layer is prepared according to the method provided by the following documents: lead Iodi peroxide sensitive All-Solid-State Submicron Cell with Efficiency evaluation 9%, H.S.Kim, C.R.Lee, J.H.Im, K.B.Lee, T.Moehl, A.Marchioro, S.J.Moon, R.Humphry-Baker, J.H.Yum, J.E.Moser, M.Gratzel and N.G.park, Scientific Reports,2012,2, 591;
the method comprises the following specific steps:
preparing a titanium dioxide compact layer by adopting a spin-coating method, coating the precursor solution of the compact layer on the surface of the conductive glass, and spinning the film for 60s under the condition that the rotating speed is 2000 rpm. Immediately after the completion, the film is placed on a hot plate preheated to 100 ℃ for heating for 10min for sufficient hydrolysis, and is heated at 500 ℃ for 30 min. The thickness of the dense layer is about 30 nm.
2) Preparation of perovskite layer:
respectively placing the MAI, the acetylacetone lead and the MACl in a graphite box for flattening to obtain source materials;
placing FTO glass coated with a compact layer in a spin mode at the center of a mask plate, reversely buckling the FTO glass on the pressed MAI, raising the temperature of a hot plate to 150 ℃ after vacuumizing, and closing a temperature switch after 30 min;
after the temperature is reduced, placing the pressed acetylacetone lead in the center of a hot plate, continuously placing the sheet on the hot plate, then raising the temperature of the hot plate to 130 ℃ under the normal pressure state, and closing a temperature switch after 40 min;
after the temperature is reduced, placing the pressed MAI in the center of a hot plate, continuously placing the sheet on the MAI, vacuumizing, raising the temperature of the hot plate to 150 ℃, and closing a temperature switch after 40 min;
after the temperature is reduced, the wafer is placed on the pressed MACl, the temperature of the hot plate is raised to 120 ℃ after the vacuum pumping, the temperature switch is closed after 10min, and then the wafer is annealed at 110 ℃, so that the growth of the perovskite layer is completed.
3) Preparation of hole transport layer
Spin-coating a hole transport layer on the surface of the perovskite obtained in the step 2), wherein the spin-coating is carried out at 2000rpm for 45s, and the thickness of the hole transport layer is about 400 nm;
wherein, the hole transport layer is composed of the following materials: 0.1g of spiro-OMeTAD (2,2 ', 7,7 ' -tetrahies (N, N-p-dimethoxy-phenylaminono) -9,9 ' -spirobilurene), 9.6 mu L of 4-tert-butylpyridine, an acetonitrile solution of lithium bistrifluoromethanesulfonylimide (the ratio of the amount of lithium bistrifluoromethanesulfonylimide to acetonitrile is 170 mg: 1mL), an acetonitrile solution of 80 mu L, FK102 salt (the ratio of the amount of FK102 salt to acetonitrile is 260 mg: 1mL), 13 mu L and 1mL of chlorobenzene.
4) Evaporation Ag/Au electrode
Evaporating an electrode on the hole transport layer at an evaporation speed of
Vacuum degree of 1.0 x 10-3Pa below, and the thickness of the electrode is 80nm-200nm, specifically 120 nm.
At AM1.5, 100mW/cm2The J-V performance curve of the cell was tested under light using KEITHLEY 4200, as shown in FIG. 3, to give a cell with a short circuit current density of 21.23mA/cm2The open circuit voltage was 0.90V, the fill factor was 0.72, and the photoelectric conversion efficiency was 14.01%.
Example 2 preparation of lead acetate perovskite solar cell as lead source by simple close-space sublimation method
Following the procedure of example 1, only the lead acetylacetonate used in step 2) was replaced by lead acetate at a temperature of 110 ℃.
At AM1.5, 100mW/cm2The J-V performance curve of the cell was tested under light using KEITHLEY 4200, as shown in FIG. 3, to give a cell with a short circuit current density of 20.05mA/cm2The open circuit voltage was 0.87V, the fill factor was 0.73, and the photoelectric conversion efficiency was 12.95%.
The perovskite solar cell is prepared by a simple close-space sublimation method, so that the perovskite solar cell can be prepared at low temperature, the coverage of a thin film is greatly improved, the perovskite solar cell can be used as a large-area device, and a feasible method is provided for future industrialization. In conclusion, the method can greatly reduce the production cost and has important significance for the practical application of the perovskite solar cell.
Claims (8)
1. The preparation method of the perovskite type solar cell is characterized in that the perovskite layer of the perovskite type solar cell is prepared by the following steps:
1) respectively placing the MAI, the lead source material and the MACl in a graphite box for flattening;
2) placing the pressed MAI in the step 1) in the center of a hot plate, placing FTO glass spin-coated with a compact layer in the center of a mask plate, placing the surface spin-coated with the compact layer and the pressed MAI in a face-to-face manner at a distance of 1-3cm, raising the temperature of the hot plate to 150 ℃ after the vacuumizing reaches 0.1MPa, and closing a temperature switch after 20-30min to obtain a sheet with the MAI layer;
3) after the temperature is reduced, placing the pressed lead source material in the step 1) in the center of a hot plate, continuously placing the sheet in the step 2) on the lead source material according to the method, then raising the temperature of the hot plate to 110-130 ℃ under the normal pressure state, and closing a temperature switch after 30-40 min;
4) after the temperature is reduced, the pressed MAI in the step 1) is placed in the center of a hot plate, the sheet in the step 3) is continuously placed according to the method, the temperature of the hot plate is increased to 130-150 ℃ after the vacuum pumping reaches 0.1MPa, and the temperature switch is closed after 30-40 min;
5) after the temperature is reduced, continuously placing the wafer on the MACl pressed in the step 1) according to the method, raising the temperature of the hot plate to 120 ℃ after the vacuum pumping reaches 0.1MPa, closing the temperature switch after 5-10min, and then annealing the wafer at 110 ℃ in 100 ℃ so as to finish the growth of the perovskite layer;
wherein the lead source material is lead acetylacetonate or lead acetate.
2. The method of claim 1, wherein the densified layer spin-coated side of step 2) and the compressed MAI are placed face-to-face at a distance of 2 cm.
3. The perovskite type solar cell prepared by the method according to any one of claims 1 to 2, which comprises FTO, an electron transport layer, a perovskite layer, a hole transport layer and an electrode in this order from bottom to top.
4. The battery of claim 3, wherein: the thickness of the perovskite layer is 300-400 nm.
5. The battery of claim 3, wherein: the material of the electron transport layer is TiO2。
6. The battery of claim 3, wherein: the materials of the hole transport layer are spiro-OMeTAD, 4-tert-butylpyridine, acetonitrile solution of lithium bis (trifluoromethanesulfonyl) imide, FK102 salt and chlorobenzene.
7. The battery of claim 6, wherein: the dosage ratio of spiro-OMeTAD, 4-tert-butylpyridine, lithium bistrifluoromethanesulfonimide, FK102 salt and chlorobenzene is 0.1 g: 9.6. mu.L: 13.6 mg: 21 mg: 1mL, wherein the dosage ratio of the acetonitrile to the lithium bis (trifluoromethanesulfonyl) imide is 1 mL: 170 mg.
8. The battery of claim 3, wherein: the material of the electrode is gold or silver.
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| US10381564B2 (en) * | 2015-08-20 | 2019-08-13 | The Hong Kong University Of Science And Technology | Organic-inorganic perovskite materials and optoelectronic devices fabricated by close space sublimation |
| CN105470400B (en) * | 2015-11-19 | 2018-06-22 | 华北电力大学 | A kind of preparation method and application of perovskite film |
| CN105470391B (en) * | 2015-11-23 | 2019-01-08 | 中国科学院上海硅酸盐研究所 | The preparation method of organic inorganic hybridization perovskite thin film and perovskite solar battery |
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