CN112436090A - Method for regulating perovskite thin film structure based on vapor phase method - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000010409 thin film Substances 0.000 title claims abstract description 47
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 19
- 239000012808 vapor phase Substances 0.000 title claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 27
- -1 amine salts Chemical class 0.000 claims abstract description 14
- 230000001276 controlling effect Effects 0.000 claims abstract description 12
- 239000011812 mixed powder Substances 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000001704 evaporation Methods 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 230000008020 evaporation Effects 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 7
- 101100080112 Parietaria judaica PMAI gene Proteins 0.000 claims description 6
- 238000002207 thermal evaporation Methods 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000007747 plating Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 238000002161 passivation Methods 0.000 description 6
- 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 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
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- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 230000005525 hole transport Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 2
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- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- UPHCENSIMPJEIS-UHFFFAOYSA-N 2-phenylethylazanium;iodide Chemical compound [I-].[NH3+]CCC1=CC=CC=C1 UPHCENSIMPJEIS-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- KFQARYBEAKAXIC-UHFFFAOYSA-N aniline;hydroiodide Chemical compound [I-].[NH3+]C1=CC=CC=C1 KFQARYBEAKAXIC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CALQKRVFTWDYDG-UHFFFAOYSA-N butan-1-amine;hydroiodide Chemical compound [I-].CCCC[NH3+] CALQKRVFTWDYDG-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- LLWRXQXPJMPHLR-UHFFFAOYSA-N methylazanium;iodide Chemical compound [I-].[NH3+]C LLWRXQXPJMPHLR-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- PPCHYMCMRUGLHR-UHFFFAOYSA-N phenylmethanamine;hydroiodide Chemical compound I.NCC1=CC=CC=C1 PPCHYMCMRUGLHR-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- 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
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- H—ELECTRICITY
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- H10K30/80—Constructional details
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- 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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- 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 method for regulating and controlling a perovskite thin film structure based on a vapor phase method. The invention adopts a mixed steam method to plate PbI2The substrate is reversely buckled on the mixed powder of the MAI and other organic amine salts, and reacts for 30-400 min at 10-1000 Pa and 150-180 ℃ to obtain the perovskite thin films with different structures. The preparation method disclosed by the invention is simple in process, high in efficiency and suitable for large-scale production.
Description
Technical Field
The invention belongs to the field of semiconductor photoelectric materials, and particularly relates to a method for regulating and controlling the structure of a perovskite thin film by using a vapor phase method.
Background
Perovskite materials have excellent optoelectronic properties making them of great interest. The perovskite material can be used for preparing solar cells, photoelectric detectors, light emitting diodes, laser devices and the like. The property of the perovskite material has abundant adjustability, and the efficiency, the stability and the like in the field of solar cells can be improved by regulating and controlling the structure of the perovskite material. In recent years, researchers have focused on the regulation of perovskite materials by solution methods. However, the preparation process of the solution method inevitably uses toxic solvents, which is not favorable for industrialized production. The perovskite solar cell prepared by the gas phase method can effectively avoid the use of toxic solvents, and is suitable for large-area preparation. However, the perovskite solar cell prepared by the current gas phase method has low efficiency. Therefore, the film forming mechanism of the perovskite thin film in the vapor phase method needs to be understood urgently, and a controllable regulation and control means for the film forming process is provided.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a method for regulating and controlling a perovskite thin film structure based on a gas phase method.
The invention adopts mixed steam to regulate the structure of the perovskite thin film, prepares the perovskite thin film with different structures, and is applied to the field of solar cells to realize the improvement of efficiency and stability.
The purpose of the invention is realized by the following technical scheme:
a method for regulating and controlling a perovskite thin film structure based on a vapor phase method comprises the following steps:
(1) will PbI2Depositing the powder on the substrate by thermal evaporation under vacuum conditions;
(2) mixing MAI (methylamine hydroiodide) powder and other organic amine salt uniformly, and plating PbI in the step (1)2The substrate is reversely buckled on mixed powder of MAI powder and other organic amine salts, and reacts for 30-400 min at 10-1000 Pa and 150-180 ℃ to obtain perovskite thin films with different structures;
and (3) the other organic amine salt in the step (2) is at least one of BAI (butylamine hydroiodide), PEAI (phenylethylamine hydroiodide), PMAI (phenylmethylamine hydroiodide) and ALI (aniline hydroiodide).
Preferably, the step (A)1) The PbI2The purity of the powder was 99.99%.
Preferably, the vacuum condition of the step (1) is that the vacuum degree is less than or equal to 10-4Pa。
Preferably, the thermal evaporation rate in step (1) is
Preferably, the PbI deposited in step (1)2The thickness of (A) is 80 to 200 nm.
Preferably, the substrate in step (1) is quartz glass, an FTO substrate or quartz glass deposited with other film layers, and the other film layers may be TiO2And/or C60。
Preferably, the reaction time in the step (2) is 60-100 min.
Preferably, the mass ratio of the MAI powder to other organic amine salts is 50-95: 50-5.
Preferably, the method for regulating the perovskite thin film structure based on the gas phase method comprises the following steps:
(1) placing the substrate in a thermal evaporation coating device, PbI2The powder is used as an evaporation source, the equipment is sealed, the vacuum pumping is carried out, and then the PbI is heated2An evaporation source to evaporate and deposit onto the substrate;
(2) mixing MAI powder and other organic amine salt, placing in a heating container, and plating PbI in step (1)2The substrate is reversely buckled on a heating container, and then the heating container is placed at 10-1000 Pa and 150-180 ℃ for reaction for 30-400 min to obtain the perovskite thin films with different structures.
More preferably, the heating container in step (2) is a heating dish made of one material of a crucible, a quartz boat and a ceramic boat.
More preferably, the heating container in step (2) has a length of 6cm, a width of 2cm and a height of 2 cm.
In the preparation method, the MAI powder in the step (2) is mixed with BAI, PEAI or PMAI to prepare the perovskite thin film with a mixed dimensional (low dimensional and three dimensional mixed) structure;
mixing the MAI powder obtained in the step (2) with PEAI, PMAI or ALI, and preparing the perovskite thin film with a passivation structure when the MAI mass ratio in the mixture is 95%;
mixing the MAI powder obtained in the step (2) with BAI or PEAI to prepare a perovskite thin film with a low n value (low dimension) structure;
if the mixed powder is MAI and BAI or MAI and PEAI, the mixing ratio is 1: 1, when the reaction time is more than or equal to 60 and t is less than 100min, generating a mixed perovskite film; and when the reaction time is 100-400 min, producing the perovskite thin film with the low n value.
The invention adopts a gas phase method and utilizes different amine salt vapors to couple PbI2The different reaction properties are used for regulating and controlling perovskite films with different structures, or the same amine salt and PbI are used2Reacting under the same condition for different time to regulate perovskite films with different structures; when the composite material is applied to a perovskite solar cell, the photoelectric conversion efficiency and stability can be improved.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the invention provides a mixed gas phase method for preparing perovskite thin films with different structures, and compared with the traditional solution method, the method is more suitable for large-area and industrialized production. The preparation method has simple process and high efficiency, and can realize large-scale preparation. Meanwhile, the method can prepare perovskite films with different structures by controlling the mixed steam so as to meet the requirements of different conditions.
Drawings
Fig. 1 is a schematic view of an apparatus for preparing a lead iodide thin film according to the present invention, where 1 is a substrate, 2 is a crystal oscillator plate, 3 is an evaporation source, and 4 is an evaporation source baffle.
FIG. 2 is a schematic view showing the reaction of lead iodide with organic amine salt vapor in the present invention, wherein 1 is a substrate plated with lead iodide, and 2 is an evaporation source.
FIG. 3 is an absorption diagram of the mixed perovskite thin film prepared in example 1 and an efficiency curve of the mixed perovskite solar cell under one sunlight at a scanning speed of 500 mV/s.
FIG. 4 is an absorption plot of the low n perovskite thin film produced in example 2 and an efficiency curve of the low n perovskite solar cell in one sun at a scan rate of 500 mV/s.
FIG. 5 is an absorption plot of the passivated perovskite thin film produced in example 3 and an efficiency curve of the passivated perovskite solar cell in one sun at a scan rate of 500 mV/s.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Those who do not specify specific conditions in the examples of the present invention follow conventional conditions or conditions recommended by the manufacturer. The raw materials, reagents and the like which are not indicated for manufacturers are all conventional products which can be obtained by commercial purchase.
The spiro-OMeTAD in the following examples is referred to herein as 2,2',7,7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene.
Example 1: preparation of mixed perovskite solar cell
Step (1): and cleaning the etched FTO conductive glass by using liquid detergent, deionized water, acetone and isopropanol in sequence, wherein the cleaning is carried out for 30 minutes each time.
Step (2): spin-coating cleaned FTO substrate with TiO2Precursor solution (TiO)2Thickness 30nm) and annealed at 500 deg.c for 30 min. Cooling, and evaporating to coat 5nm C60。
And (3): good vapor deposition C60Then, a 150nm thick lead iodide film was continuously evaporated. As shown in fig. 1. The thickness can be detected by a crystal oscillator plate, and the evaporation rate is
And (4): 50mg MAI and 50mg BAI powder (equivalent mass of PEAI or PMAI can be substituted) were mixed uniformly and spread in a quartz crucible. Taking out the substrate which is evaporated with lead iodide and reversely buckling the substrate on a quartz crucible. And (3) putting the film into a vacuum oven at 160 ℃, continuously heating the film, exhausting air and pressing the film to 100Pa, wherein the heating time is 80min, and obtaining the perovskite film with the mixed dimensional structure as shown in figure 2.
And (5): after the reaction was completed, a hole transport layer, spiro-OMeTAD (thickness 150nm), was spin-coated.
And (6): and evaporating a gold electrode with the thickness of 80 nm.
The mixed perovskite thin film prepared above was subjected to characterization test, and the results are shown in fig. 3.
The mixed victorite thin film prepared above was analyzed using an ultraviolet spectrophotometer, and as a result, as shown in fig. 3a, it can be seen from fig. 3a that the resulting perovskite thin film has a mixed structure of n-3, n-4 and 3D.
The efficiency of the prepared hybrid perovskite solar cell was characterized as shown in fig. 3 b.
Example 2: preparation of low n value perovskite solar cell
Step (1): and cleaning the etched FTO conductive glass by using detergent, deionized water, acetone and isopropanol in sequence, wherein the cleaning is carried out for 30 minutes each time.
Step (2): spin-coating cleaned FTO substrate with TiO2Precursor solution (TiO)2Thickness 30nm) and annealed at 500 deg.c for 30 min. Cooling, and evaporating to coat 5nm C60。
And (3): good vapor deposition C60Then, a 150nm thick lead iodide film was continuously evaporated. As shown in FIG. 1, the thickness can be detected by a crystal oscillator plate, and the evaporation rate is
And (4): 50mg MAI and 50mg BAI powder (equivalent mass of PEAI can be replaced) were mixed well and spread in a quartz crucible. Taking out the substrate which is evaporated with lead iodide and reversely buckling the substrate on a quartz crucible. And putting the perovskite thin film into a vacuum oven at 160 ℃, continuously heating the perovskite thin film, and exhausting air and pressing the perovskite thin film to 100Pa, wherein the heating time is 100min, and obtaining the perovskite thin film with the low n value as shown in figure 2.
And (5): after the reaction was completed, a hole transport layer, spiro-OMeTAD (thickness 150nm), was spin-coated.
And (6): and evaporating a gold electrode with the thickness of 80 nm.
The characterization test is carried out on the low n value perovskite thin film prepared above, and the result is shown in figure 4.
The low n-value perovskite thin film prepared as above was analyzed by uv spectrophotometer, and as a result, as shown in fig. 4a, it can be seen from fig. 4a that the resulting perovskite thin film has a low n-value structure in which n is 3 and n is 4.
The efficiency of the prepared low n-value titanium ore solar cell was characterized as shown in fig. 4 b.
Example 3: preparation of perovskite solar cell with passivation structure
Step (1): and cleaning the etched FTO conductive glass by using liquid detergent, deionized water, acetone and isopropanol in sequence, wherein the cleaning is carried out for 30 minutes each time.
Step (2): spin-coating cleaned FTO substrate with TiO2Precursor solution (TiO)2Thickness 30nm) and annealed at 500 deg.c for 30 min. Cooling, and evaporating to coat 5nm C60。
And (3): good vapor deposition C60Then, a 150nm thick lead iodide film was continuously evaporated. As shown in FIG. 1, the thickness can be detected by a crystal oscillator plate, and the evaporation rate is
And (4): 95mg MAI and 5mg ALI powder (equivalent mass of PEAI and PMAI can be replaced) were mixed uniformly and spread in a quartz crucible. Taking out the substrate which is evaporated with lead iodide and reversely buckling the substrate on a quartz crucible. And (3) putting the film into a vacuum oven at 160 ℃, continuously heating the film, exhausting air and pressing the film to 100Pa, wherein the heating time is 60min, and obtaining the perovskite film with the passivation structure as shown in figure 2.
And (5): after the reaction was completed, a hole transport layer, spiro-OMeTAD (thickness 150nm), was spin-coated.
And (6): and evaporating a gold electrode with the thickness of 80 nm.
The perovskite thin film with the passivation structure prepared in the above way is subjected to characterization test, and the result is shown in fig. 5.
The perovskite thin film with the passivation structure prepared in the above way is analyzed by using an ultraviolet spectrophotometer, and the result is shown in fig. 5a, and the 3D structure of the perovskite thin film obtained can be seen from fig. 5 a.
The efficiency of the prepared perovskite solar cell with a passivation structure was characterized as shown in fig. 5 b.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for regulating and controlling a perovskite thin film structure based on a vapor phase method is characterized by comprising the following steps:
(1) will PbI2Depositing the powder on the substrate by thermal evaporation under vacuum conditions;
(2) mixing MAI powder and other organic amine salt uniformly, and plating PbI in the step (1)2The substrate is reversely buckled on the mixed powder of the MAI powder and other organic amine salts, and reacts for 30-400 min at 10-1000 Pa and 150-180 ℃ to obtain the perovskite thin films with different structures.
2. The method for regulating the perovskite thin film structure based on the gas phase method as claimed in claim 1, wherein the other organic amine salt in the step (2) is at least one of BAI, PEAI, PMAI and ALI.
3. The method for regulating and controlling the perovskite thin film structure based on the vapor phase method as claimed in claim 1, wherein the mass ratio of the MAI powder to other organic amine salts is 50-95: 50-5.
4. The method for regulating the perovskite thin film structure based on the vapor phase method as claimed in claim 1, wherein the reaction time in the step (2) is 60-100 min.
5. The method for regulating perovskite thin film structure based on the vapor phase method as claimed in claim 1, wherein the PbI deposited in the step (1) is2The thickness of (A) is 80 to 200 nm.
6. The method for regulating and controlling the perovskite thin film structure based on the vapor phase method as claimed in claim 1, wherein the vacuum condition in the step (1) is that the vacuum degree is less than or equal to 10-4Pa; the rate of thermal evaporation is 0.2 to
7. The method for regulating and controlling the perovskite thin film structure based on the vapor phase method as claimed in claim 1, wherein the substrate in the step (1) is quartz glass, FTO substrate or quartz glass and FTO substrate deposited with other film layers, and the other film layers are TiO2And/or C60。
8. The method for regulating the perovskite thin film structure based on the vapor phase method as claimed in claim 1, which is characterized by comprising the following steps:
(1) placing the substrate in a thermal evaporation coating device, PbI2The powder is used as an evaporation source, the equipment is sealed, the vacuum pumping is carried out, and then the PbI is heated2An evaporation source to evaporate and deposit onto the substrate;
(2) mixing MAI powder and other organic amine salt, placing in a heating container, and plating PbI in step (1)2The substrate is reversely buckled on a heating container, and then the heating container is placed at 10-1000 Pa and 150-180 ℃ for reaction for 30-400 min to obtain the perovskite thin films with different structures.
9. The method for regulating and controlling a perovskite thin film structure based on a vapor phase method as claimed in claim 8, wherein the heating container in the step (2) is a heating vessel made of one material selected from a crucible, a quartz boat and a ceramic boat.
10. The method for regulating perovskite thin film structure based on the vapor phase method as claimed in claim 1, wherein the PbI in the step (1)2The purity of the powder was 99.99%.
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| CN113675347A (en) * | 2021-08-23 | 2021-11-19 | 西南石油大学 | Method for preparing 2D/3D organic-inorganic hybrid perovskite solar cell |
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| US10770239B1 (en) * | 2016-07-01 | 2020-09-08 | Triad National Security, Llc | High-efficiency and durable optoelectronic devices using layered 2D perovskites |
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| CN113675347B (en) * | 2021-08-23 | 2023-06-09 | 西南石油大学 | Method for preparing 2D/3D organic-inorganic hybrid perovskite solar cell |
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