CN112002815A - Production method of perovskite thin film and preparation method of perovskite solar cell - Google Patents
Production method of perovskite thin film and preparation method of perovskite solar cell Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 89
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 105
- 239000000758 substrate Substances 0.000 claims abstract description 66
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000000576 coating method Methods 0.000 claims abstract description 50
- 239000010408 film Substances 0.000 claims abstract description 49
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- 230000005525 hole transport Effects 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 24
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- 238000004528 spin coating Methods 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
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- 229910003437 indium oxide Inorganic materials 0.000 description 5
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- 238000006243 chemical reaction Methods 0.000 description 4
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- 239000011787 zinc oxide Substances 0.000 description 4
- SHWZFQPXYGHRKT-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;nickel Chemical compound [Ni].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O SHWZFQPXYGHRKT-FDGPNNRMSA-N 0.000 description 3
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- HBUKSGRCRAUHHN-UHFFFAOYSA-L magnesium diacetate dihydrate Chemical compound O.O.[Mg++].CC([O-])=O.CC([O-])=O HBUKSGRCRAUHHN-UHFFFAOYSA-L 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001771 vacuum deposition Methods 0.000 description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 229910005855 NiOx Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- PDZKZMQQDCHTNF-UHFFFAOYSA-M copper(1+);thiocyanate Chemical compound [Cu+].[S-]C#N PDZKZMQQDCHTNF-UHFFFAOYSA-M 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
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- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 238000003852 thin film production method Methods 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- JAHFQMBRFYOPNR-UHFFFAOYSA-N iodomethanamine Chemical compound NCI JAHFQMBRFYOPNR-UHFFFAOYSA-N 0.000 description 1
- RQQRAHKHDFPBMC-UHFFFAOYSA-L lead(ii) iodide Chemical compound I[Pb]I RQQRAHKHDFPBMC-UHFFFAOYSA-L 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
-
- 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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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Photovoltaic Devices (AREA)
Abstract
The application provides a production method of a perovskite thin film and a preparation method of a perovskite solar cell, and relates to the technical field of thin film production. The production method of the perovskite thin film comprises the following steps: providing a substrate; providing a perovskite solution; wherein the solvent in the perovskite solution comprises a mixture of N, N-dimethylformamide and an alcohol; coating the perovskite solution on a substrate to obtain a perovskite liquid film; and curing the perovskite liquid film to obtain the perovskite thin film. The perovskite solution has small surface tension, forms good infiltration with the substrate, is easy to form an even perovskite liquid film, reduces the film forming difficulty, improves the utilization rate of the perovskite solution, reduces the using amount of the perovskite solution, reduces the material waste and reduces the environmental pollution. With the reduction of the film forming difficulty, the uniform perovskite liquid film can be produced by using a coating mode, and the mass production of large-area perovskite films is facilitated.
Description
Technical Field
The invention relates to the technical field of film production, in particular to a perovskite film production method and a perovskite solar cell preparation method.
Background
The perovskite solar cell with large area has higher photoelectric conversion efficiency, thus having wide application prospect. And large-area perovskite solar cells require large-area perovskite thin films.
At present, the production methods of large-area perovskite thin films mainly include a coating method, a vacuum evaporation method and the like. Among them, the vacuum evaporation method requires a high degree of vacuum, and has high requirements for equipment, high energy consumption, and high cost. For the vacuum evaporation method, the coating method is relatively mature in process, but the coating method is difficult to realize mass production preparation of large-area perovskite thin films, and has high requirements on equipment, high process cost and great process difficulty.
Disclosure of Invention
The invention provides a production method of a perovskite thin film and a preparation method of a perovskite solar cell, and aims to solve the problems of high production cost, high process difficulty and difficulty in mass production of large-area perovskite thin films.
According to a first aspect of the present invention, there is provided a method of producing a perovskite thin film, comprising the steps of:
providing a substrate;
providing a perovskite solution; wherein the solvent in the perovskite solution comprises a mixture of N, N-dimethylformamide and an alcohol;
coating the perovskite solution on the substrate to obtain a perovskite liquid film;
and curing the perovskite liquid film to obtain the perovskite thin film.
Optionally, the volume of N, N-dimethylformamide in the solvent is greater than or equal to the volume of alcohol.
Optionally, in the solvent, N-dimethylformamide is mixed with an alcohol in a volume ratio of 1:1 to 4: 1.
Optionally, the alcohol is selected from: at least one of methanol, ethanol and isopropanol.
Optionally, the coating is selected from any one of spin coating, blade coating, slit coating, ultrasonic spraying, and drop casting.
Optionally, in the blade coating, slit coating, ultrasonic spraying, or drop casting, the coating is performed while the temperature of the substrate is maintained at 25 ℃ or lower.
Optionally, the step of curing the perovskite liquid film comprises:
and curing the perovskite liquid film by adopting a protective gas blowing and spraying mode to obtain the perovskite film.
Optionally, the step of providing a substrate includes:
providing a substrate;
sequentially arranging a front electrode layer and a first current carrier transmission layer on the substrate; the first carrier transport layer is: one of a hole transport layer or an electron transport layer.
Optionally, the thickness of the perovskite thin film is 100-1000 nm.
Optionally, the concentration of the perovskite solution is greater than or equal to 0.2mol/L and less than or equal to 1.5 mol/L.
In the embodiment of the invention, the solvent of the perovskite solution comprises a mixture formed by N, N-dimethylformamide and alcohol, the perovskite solution has small surface tension and can form good infiltration with a substrate, so that a uniform perovskite liquid film is easy to form, the film forming difficulty is reduced, the utilization rate of the perovskite solution is improved, the using amount of the perovskite solution is reduced, the material waste is reduced, and the environmental pollution is reduced. Meanwhile, with the reduction of the film forming difficulty, the uniform perovskite liquid film can be produced by using a coating mode, and the mass production of large-area perovskite thin films is facilitated.
According to a second aspect of the present invention, there is provided a method of fabricating a perovskite solar cell, comprising the steps of:
obtaining a perovskite thin film formed on a substrate by using any one of the above perovskite thin film production methods;
forming a second carrier transmission layer and a back electrode layer on one side of the perovskite thin film far away from the substrate in sequence; wherein the second carrier transport layer and the first carrier transport layer included in the substrate are of opposite types.
The preparation method of the perovskite solar cell has the same or similar beneficial effects as the production method of the perovskite thin film, and the repeated description is avoided.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments of the present invention will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without inventive exercise.
FIG. 1 is a flow chart illustrating the steps of a method for producing a perovskite thin film in accordance with an embodiment of the invention;
FIG. 2 shows a schematic structural diagram of a perovskite thin film disposed on a substrate in an embodiment of the invention;
FIG. 3 is a flow chart illustrating steps of a method for fabricating a perovskite solar cell according to an embodiment of the invention;
fig. 4 shows a schematic structural diagram of a perovskite solar cell in an embodiment of the invention.
Description of the figure numbering:
1-substrate, 2-front electrode layer, 3-first carrier transmission layer, 4-perovskite thin film, 5-second carrier transmission layer and 6-back electrode layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The inventor of the present invention finds that, in the prior art, the main reasons for the problems of high production cost, large process difficulty and difficulty in mass production of large-area perovskite thin films produced by a coating method are as follows: the solvent in current perovskite solutions is mainly N, N-Dimethylformamide (DMF). In the process of producing the perovskite thin film by adopting a liquid phase method, the surface tension of the existing perovskite solution is large, the wettability with a substrate is poor, the film forming difficulty of the perovskite liquid film is large, the material utilization rate is low, a large-area perovskite thin film is difficult to prepare, and in order to prepare the perovskite thin film with the quality up to the standard, excessive perovskite solution is required to be used, so that the material waste is caused, and the environmental pollution is also caused.
In an embodiment of the present invention, referring to fig. 1, fig. 1 shows a flow chart of the steps of a method for producing a perovskite thin film in an embodiment of the present invention. The method comprises the following steps:
in step S1, a substrate is provided.
The substrate is a matrix for supporting the perovskite solution. The material and structure of the substrate are not particularly limited.
Step S2, providing a perovskite solution; wherein the solvent in the perovskite solution comprises a mixture of N, N-dimethylformamide and an alcohol.
The perovskite solute in the perovskite solution may be equimolar PbI2(lead iodide) and CH3NH3I (iodomethylamine). The solvent contains at least a mixture of DMF and an alcohol. The alcohol may be one kind of alcohol or a mixture of two or more kinds of alcohols, and is not particularly limited in the examples of the present invention. For example, the alcohol may be ethanol. Alternatively, the alcohol may be a mixture of methanol and ethanol.
The perovskite solution formed by the perovskite solute and the solvent has different molecular sizes of DMF and alcohol, so that internal stress is generated on the liquid surface, the surface tension of the solvent is changed, the perovskite solution has lower surface tension, the perovskite solution and the substrate can be completely infiltrated, and the film forming difficulty of the perovskite liquid film is reduced.
Specifically, the surface tension of the perovskite solution is tested by a capillary method, and the following results are obtained under the condition that the perovskite solutes are the same: the perovskite solution obtained by using pure DMF as a solvent can be raised by 51mm in a capillary tube with the inner diameter of 0.5 mm; a perovskite solution obtained with a 1:1 volume ratio of a mixture of DMF and ethanol as solvent can be raised by 89mm in a 0.5mm internal diameter capillary. From the above experiments, it can be seen that the surface tension of the perovskite solution obtained with a mixture of DMF and an alcohol as a solvent for the perovskite solute is reduced and the wettability is excellent.
And step S3, coating the perovskite solution on the substrate to obtain a perovskite liquid film.
The perovskite solution has lower surface tension, so that the perovskite solution and the substrate can be completely infiltrated, the film forming difficulty of the perovskite liquid film is reduced, the utilization rate of the perovskite solution is improved, the using amount of the perovskite solution is reduced, the material waste is reduced, and the environmental pollution is reduced. Meanwhile, with the reduction of the film forming difficulty, the uniform perovskite liquid film can be produced by using a coating mode, and the mass production of large-area perovskite thin films is facilitated.
And step S4, solidifying the perovskite liquid film to obtain the perovskite thin film.
In the process of curing the perovskite liquid film, the temperature is usually about 100-150 ℃, and the boiling point of the alcohol is usually less than 100 ℃, so that in the process of curing the perovskite liquid film, the alcohol volatilizes, and further, the alcohol basically cannot remain in the perovskite thin film, and cannot influence the perovskite thin film. For example, ethanol has a boiling point of about 80 ℃, and ethanol in the cured perovskite liquid film is substantially completely volatilized in the process of curing the perovskite liquid film.
Optionally, in the above solvent, the volume of DMF is greater than or equal to the volume of alcohol, and the solubility of the particular perovskite solute in DMF is greater than the solubility in alcohol. In the solvent, the volume of DMF is more than or equal to that of alcohol, so that a perovskite solution with higher concentration is easily obtained, and the production efficiency is favorably improved.
Optionally, in the solvent, DMF and alcohol are mixed according to a volume ratio of 1:1-4:1, so that a perovskite solution with a high concentration is easily obtained, and the cost is low.
Optionally, the alcohol is selected from: at least one of methanol, ethanol and isopropanol, wherein the alcohol is common and low in cost, and the perovskite solution formed by the alcohol has better wetting performance with the substrate.
Alternatively, the concentration of the perovskite solution is greater than or equal to 0.2mol/L (mol/L) and less than or equal to 1.5mol/L, i.e. dissolving the perovskite solute by a solvent comprising a mixture of N, N-dimethylformamide and an alcohol still allows obtaining a perovskite solution with a suitable concentration range which is advantageous for obtaining a uniform perovskite liquid film.
Optionally, the coating in the step S3 is specifically selected from any one of five ways, namely spin coating, blade coating, slit coating, ultrasonic spraying and drop casting. The dropping casting is to drop the perovskite solution on the substrate, and the perovskite solution is automatically cast on the substrate to form a uniform perovskite liquid film. Now, in the prior art, only spin coating or slit coating of the coating methods can be adopted, in the embodiment of the present invention, since the wettability of the perovskite solution to the substrate is excellent, a uniform perovskite liquid film can be easily obtained in any one of the five methods, which is beneficial to the mass production of large-area perovskite thin films, and the production method of the perovskite thin films is widened.
Optionally, the four modes of the five modes of spin coating, blade coating, slit coating, ultrasonic spraying and drop casting in the coating mode are blade coating, slit coating, ultrasonic spraying and drop casting, and the perovskite solution is coated on the substrate under the condition that the temperature of the substrate is kept to be less than or equal to 25 ℃. Typically, room temperature, i.e., less than or equal to 25 ℃, requires no additional treatment for room temperature. For example, the perovskite solution is coated on the substrate while the temperature of the substrate is maintained at 0 ℃ or lower. Compared with the prior art that the substrate needs to be heated in a slit coating mode, so that the substrate is kept at about 100 ℃ to improve the wettability of the perovskite solution to the substrate in the prior art, the perovskite solution provided by the embodiment of the invention has better wettability to the substrate, and the substrate does not need to be heated, so that a uniform perovskite liquid film can be formed on the substrate under the condition that the substrate is kept at 25 ℃ or lower. Meanwhile, in the prior art, the substrate is kept at about 100 ℃, so that perovskite crystals in the perovskite liquid film are easy to grow, the preparation of a large-area perovskite thin film is not facilitated, and the uniformity of the perovskite thin film is poor. In the embodiment of the invention, the substrate is kept at a lower temperature of less than or equal to 25 ℃, so that the growth of perovskite crystals in the perovskite liquid film can be fully inhibited, the preparation of a large-area perovskite thin film is facilitated, and the uniformity of the perovskite thin film is improved.
Optionally, the step S4 may include: and curing the perovskite liquid film coated on the substrate by adopting a protective gas blowing and spraying mode to obtain the perovskite thin film. The shielding gas may be an inert gas such as nitrogen. In the prior art, because the perovskite solution in the prior art has poor wettability to the substrate, a reverse extraction solvent is required to be used in the process of solidifying the perovskite liquid film, so that the process difficulty is increased, the production cost is increased, and the risk of environmental pollution is increased. The perovskite solution applied by the invention has excellent wettability to the substrate, only needs to protect the gas blowing and annealing, and then is heated and annealed at the temperature of less than or equal to 150 ℃, without using a reverse extraction solvent, thereby reducing the process difficulty, the production cost and the risk of environmental pollution.
The temperature of the shielding gas in the shielding gas showering process may be room temperature, and the like, which is not particularly limited in this embodiment of the present invention.
Optionally, the step S1 may include the following steps: providing a substrate; sequentially arranging a front electrode layer and a first carrier transmission layer on a substrate; the first carrier transport layer is: one of a hole transport layer or an electron transport layer. The substrate may be glass. A part of the perovskite solar cell can thereby be obtained. For example, referring to fig. 2, fig. 2 shows a schematic structural view of a perovskite thin film disposed on a substrate according to an embodiment of the present invention. In fig. 2, 1 is a substrate, 2 is a front electrode layer, 3 is a first carrier transport layer, such as a hole transport layer, and 4 is a perovskite thin film.
The material of the front electrode layer 2 may be at least one selected from FTO (fluorine doped tin oxide), ITO (tin doped indium oxide), AZO (aluminum doped zinc oxide), IZO (zinc doped indium oxide), IWO (tungsten doped indium oxide), ITIO (titanium doped indium oxide). The front electrode layer 2 may be prepared by magnetron sputtering. E.g. at 1X 10-5And under the Pa background vacuum degree, FTO with the thickness of 450nm is formed by magnetron sputtering to form a front electrode layer 2.
In the case where the first carrier transport layer 3 is a hole transport layer, the material of the first carrier transport layer 3 may be selected from: CuSCN (cuprous thiocyanate), NiOx(Nickel oxide), NiMgOx(magnesium-doped nickel oxide) V2O5(vanadium pentoxide) and MoO3Of molybdenum trioxideOne of them is less. For example, the first carrier transport layer 3 may be NiOx、NiMgOxAt least one of (1). It should be noted that x in the chemical formula is a suitable value that can be selected by those skilled in the art according to actual situations.
In the case where the first carrier transport layer 3 is an electron transport layer, the material of the first carrier transport layer 3 may be selected from: TiO 22(titanium dioxide) SnO2(tin dioxide), ZnO (Zinc oxide), PCBM ([6, 6)]-phenyl-C61-butyric acid isopropyl ester), C60-bis, BCP (bathocuproine). For example, the first carrier transport layer 3 may be TiO2With SnO2。
The chemical formula of the perovskite thin film 4 is ABXmY3-mOne or more materials of a crystalline structure of type (I) wherein A is CH3NH3(methylamine), C4H9NH3(n-butylamine), NH2＝CHNH2(methyl ether) or Cs (cesium); b is Pb (lead) and Sn (tin); x is Cl (chlorine), Br (bromine) or I (iodine), Y is Cl, Br or I, and X and Y are not the same element at the same time; m is 1, 2 or 3.
Optionally, the thickness of the perovskite thin film is 100-1000nm, and the perovskite solar cell formed by the perovskite thin film with the thickness is high in photoelectric conversion efficiency. More preferably, the thickness of the perovskite thin film is 300-650 nm.
The embodiment of the invention also provides a preparation method of the perovskite battery, which is shown in the figure 3. Fig. 3 shows a flow chart of steps of a method for manufacturing a perovskite solar cell according to an embodiment of the invention. The method comprises the following steps:
and (II) adopting the perovskite thin film production method as described in any one of the previous steps to obtain the perovskite thin film formed on the substrate.
The side, far away from the substrate, of the perovskite thin film is sequentially provided with a second carrier transmission layer and a back electrode layer; wherein the second carrier transport layer and the first carrier transport layer included in the substrate are of opposite types.
The preparation method of the perovskite solar cell can be shown in fig. 4, and fig. 4 shows a schematic structural diagram of a perovskite solar cell in an embodiment of the invention. In fig. 4, reference may be made to corresponding descriptions in fig. 2 from 1 to 4. 5 is a second carrier transport layer, and 6 is a back electrode layer. In fig. 4, 3 is a first carrier transport layer, and 5 is a second carrier transport layer of a type different from 3. For example, if 3 is a hole transport layer, 5 may be an electron transport layer. The material of the back electrode layer 6 may be selected from: at least one of Au (gold), Ag (silver), Cu (copper), Al (aluminum), Pt (platinum), ITO (tin-doped indium oxide), FTO (fluorine-doped tin oxide) or AZO (aluminum-doped zinc oxide). For example, the material of the back electrode layer 6 may be Ag.
For the preparation method of the perovskite battery, reference can be made to the related content of the production method of the perovskite thin film, and the same or similar beneficial effects can be achieved, so that the repeated description is omitted here for avoiding the repetition.
The invention is further illustrated by the following specific examples.
Example 1
The production method of the perovskite solar cell comprises steps SA1-SA 5:
step SA1, providing transparent conductive glass, and cleaning the transparent conductive glass.
The transparent conductive glass is ultrasonically cleaned by using a detergent, deionized water, absolute ethyl alcohol, acetone and isopropanol in sequence for 10min (minutes), and then is dried by nitrogen. The transparent conductive glass is a combination of a substrate and a front electrode layer, and one side of the conductive glass is provided with the front electrode layer.
Step SA2, preparing a hole transport layer on the side of the transparent conductive glass having the front electrode layer.
Specifically, the hole transport layer is NiMgOxIt should be noted that x in the chemical formula is required, and those skilled in the art can select an appropriate value according to actual situations. Preparing a mixture of nickel acetylacetonate and magnesium acetate dihydrate, wherein the mass ratio of the nickel acetylacetonate to the magnesium acetate dihydrate is 10:1, the solvent is acetonitrile and ethanol, the volume ratio of the acetonitrile to the ethanol is 19:1, the solution concentration is more than 0.01mol (mol), and stirring to obtain a light green transparent clear liquid. Placing the transparent conductive glass on a high-temperature heating table to be heated to 450 DEG CSpraying the mixture of nickel acetylacetonate and magnesium acetate dihydrate on the side of the transparent conductive glass with the front electrode layer to obtain NiMgOxThe layer acts as a hole transport layer.
Step SA3, preparing a perovskite thin film on the side of the hole transport layer away from the front electrode layer.
Specifically, under the protection of nitrogen, the perovskite thin film is prepared on one side of the hole transport layer, which is far away from the front electrode layer or the transparent conductive glass, through a spin coating mode in a coating mode. Equimolar of PbI2And CH3NH3And I is jointly dissolved in a mixture of DMF and ethanol, and the volume ratio of the DMF to the ethanol is 4:1, so that 1mol/L perovskite solution is obtained. That is, the solvents for the perovskite solution of example 1 were: DMF and ethanol in a volume ratio of 4: 1. Taking 30 microliter of perovskite solution, spin-coating the perovskite solution on the surface of the hole transport layer at 3000rpm for 30s, blowing with nitrogen after the spin-coating is stable, and then heating and annealing at 100 ℃ for 20min to form CH with the thickness of 400nm3NH3PbI3A perovskite thin film.
Step SA4, preparing an electron transport layer on the side of the perovskite thin film far away from the hole transport layer.
Specifically, under the protection of nitrogen, the electron transport layer is prepared on the side of the perovskite thin film far away from the hole transport layer in a spin coating mode, 20mg of PCBM is added into 1mL of chlorobenzene, dissolved to prepare a solution, the solution is spin-coated on the surface of the perovskite thin film, the rotating speed is 3000rpm, the time is 30s, and then the PCBM layer with the thickness of 100nm is obtained through heating annealing at 70 ℃ for 20 min. And then preparing a BCP layer on the PCBM layer by adopting a spin-coating method, taking a methanol saturated solution of the BCP to spin-coat on the surface of the PCBM layer, rotating at 6000rpm for 30s, and then heating and annealing at 70 ℃ for 20min to obtain the BCP layer with the thickness of 10 nm.
Step SA5, preparing a back electrode layer.
Specifically, a silver electrode is prepared on the side of the electron transport layer far away from the perovskite thin film by adopting a thermal evaporation mode at 1 multiplied by 10-5And (3) forming a back electrode layer by vacuum evaporation of a silver film with the thickness of 100nm under the Pa vacuum degree.
Example 2
The production method of the perovskite solar cell comprises the steps of SB1-SB 5:
step SB1, providing transparent conductive glass, and cleaning the transparent conductive glass.
At step SB2, a hole transport layer is prepared on the side of the transparent conductive glass having the front electrode layer.
Steps SB1 to SB2 correspond to SA1 to SA2, respectively, and are not described herein again to avoid repetition.
And step SB3, preparing the perovskite thin film on the side of the hole transport layer far away from the front electrode layer.
Specifically, under the protection of nitrogen, the perovskite thin film is prepared on one side of the hole transport layer, which is far away from the front electrode layer or the transparent conductive glass, through a blade coating mode in a coating mode. Equimolar of PbI2And CH3NH3I are jointly dissolved in a mixture of DMF and ethanol, the volume ratio of DMF to ethanol is 4:1, and 0.5mol/L perovskite solution is obtained. That is, the solvents for the perovskite solution of example 2 were: DMF and ethanol in a volume ratio of 4: 1. And putting a certain amount of perovskite solution on the surface of the hole transport layer for blade coating, wherein the blade coating speed is 2cm/s, the height of a scraper from a substrate is 0.1mm, the temperature of the substrate is kept to be less than or equal to 25 ℃, an air knife is additionally arranged behind the scraper for nitrogen blowing, and the air speed of nitrogen is 5 m/s. Heating and annealing the sample at 100 ℃ for 20min after blade coating to form CH with the thickness of 300nm3NH3PbI3A perovskite thin film.
And step SB4, preparing an electron transport layer on the side of the perovskite thin film far away from the hole transport layer.
Step SB5, a back electrode layer is prepared.
Steps SB4 and SB5 correspond to SA4 and SA5, respectively, and are not described herein again to avoid repetition.
Example 3
The production method of the perovskite solar cell comprises the steps SC1-SC 5:
step SC1, providing transparent conductive glass, and cleaning the transparent conductive glass.
At step SC2, a hole transport layer is prepared on the side of the transparent conductive glass having the front electrode layer.
Steps SC1 to SC2 correspond to SA1 to SA2, respectively, and are not described herein again to avoid repetition.
Step SC3, preparing a perovskite thin film on the side of the hole transport layer away from the front electrode layer.
Specifically, under the protection of nitrogen, the perovskite thin film is prepared on one side of the hole transport layer, which is far away from the front electrode layer or the transparent conductive glass, through a slit coating mode in the coating mode. Equimolar of PbI2And CH3NH3And I is jointly dissolved in a mixture of DMF and ethanol, and the volume ratio of the DMF to the ethanol is 4:1, so that 1mol/L perovskite solution is obtained. That is, the solvents for the perovskite solution of example 3 were: DMF and ethanol in a volume ratio of 4: 1. Coating a certain amount of perovskite solution on the surface of a hole transport layer by using slit coating equipment, wherein the speed of a slit coating tool bit is 5cm/s, the liquid inlet speed is 50uL/s (microliter/second), the temperature of a substrate is kept to be less than or equal to 25 ℃, and after the slit coating is finished, a sample is heated and annealed at 100 ℃ for 20min to form CH with the thickness of 400nm3NH3PbI3A perovskite thin film.
Step SC4, an electron transport layer is prepared on the side of the perovskite thin film away from the hole transport layer.
Step SC5, a back electrode layer is prepared.
Step SC4 and step SC5 correspond to SA4 and SA5, respectively, and are not described herein again to avoid repetition.
Example 4
The production method of the perovskite solar cell comprises the steps SD1-SD 5:
and step SD1, providing transparent conductive glass and cleaning the transparent conductive glass.
At step SD2, a hole transport layer is prepared on the side of the transparent conductive glass having the front electrode layer.
The steps SD1 to SD2 correspond to the same steps SA1 to SA2, respectively, and are not described herein again to avoid repetition.
And step SD3, preparing the perovskite thin film on the side of the hole transport layer far away from the front electrode layer.
In particular, under nitrogenUnder protection, preparing the perovskite thin film on one side of the hole transport layer, which is far away from the front electrode layer or the transparent conductive glass, by an ultrasonic spraying mode in a coating mode. Equimolar of PbI2And CH3NH3I are jointly dissolved in a mixture of DMF and ethanol, the volume ratio of DMF to ethanol is 4:1, and 0.5mol/L perovskite solution is obtained. That is, the solvents for the perovskite solution of example 4 were: DMF and ethanol in a volume ratio of 4: 1. Spraying a certain amount of perovskite solution on the surface of the hole transport layer by using ultrasonic spraying equipment, wherein the power of an ultrasonic spray head is 0.5W, the distance between a spray nozzle and a substrate is 8cm, the driving air pressure is 20Pa, the liquid inlet speed is 20uL/s, the moving speed of the spray head is 50mm/s, the temperature of the substrate is kept to be less than or equal to 25 ℃, continuously keeping a sample on a sample table after the ultrasonic spraying is finished, blowing and spraying for 20s by using nitrogen, and then heating and annealing for 20min at 100 ℃ to form CH with the thickness of 300nm3NH3PbI3A perovskite thin film.
And step SD4, preparing an electron transport layer on the side of the perovskite thin film far away from the hole transport layer.
And step SD5, preparing a back electrode layer.
The steps SD4 and SD5 correspond to the same steps SA4 and SA5, respectively, and are not described herein again to avoid repetition.
Example 5
The production method of the perovskite solar cell comprises the steps of SE1-SE 5:
step SE1, providing transparent conductive glass, and cleaning the transparent conductive glass.
Step SE2, preparing a hole transport layer on the side of the transparent conductive glass having the front electrode layer.
Steps SE1 to SE2 correspond to SA1 to SA2, respectively, and are not described herein again to avoid repetition.
Step SE3, preparing a perovskite thin film on the side of the hole transport layer remote from the front electrode layer.
Specifically, under the protection of nitrogen, the perovskite thin film is prepared on one side of the hole transport layer, which is far away from the front electrode layer or the transparent conductive glass, through a dripping and casting mode in a coating mode. Equimolar of PbI2And CH3NH3I are jointly dissolved in a mixture of DMF and ethanol, the volume ratio of DMF to ethanol is 4:1, and 0.5mol/L perovskite solution is obtained. That is, the solvents for the perovskite solution of example 5 were: DMF and ethanol in a volume ratio of 4: 1. 15 microliter of perovskite solution is dripped on the surface of the hole transport layer, the perovskite solution is automatically cast into a uniform perovskite liquid film, and the temperature of the substrate is kept to be less than or equal to 25 ℃. Spraying with nitrogen gas for 20s, and annealing at 100 deg.C for 20min to obtain CH with thickness of 250nm3NH3PbI3A perovskite thin film.
Step SE4, an electron transport layer is prepared on the side of the perovskite thin film remote from the hole transport layer.
Step SE5, a back electrode layer is prepared.
The steps SE4 and SE5 correspond to the same steps SA4 and SA5, respectively, and are not described herein again to avoid repetition.
Comparative example
The production method of the perovskite solar cell comprises the steps of SF1-SF 5:
step SF1, providing transparent conductive glass, and cleaning the transparent conductive glass.
Step SF2, preparing a hole transport layer on the side of the transparent conductive glass having the front electrode layer.
The steps SF1 to SF2 are respectively the same as the steps SA1 to SA2, and are not described herein again to avoid redundancy.
And step SF3, preparing the perovskite thin film on the side, far away from the front electrode layer, of the hole transport layer.
Specifically, under the protection of nitrogen, the perovskite thin film is prepared on one side of the hole transport layer, which is far away from the front electrode layer or the transparent conductive glass, through a spin coating mode in a coating mode. Equimolar of PbI2And CH3NH3I was co-dissolved in DMF to give a 1.5mol/L perovskite solution. That is, the solvents of the perovskite solution of the comparative example were: DMF. Taking 60 microliter of perovskite solution, adopting a spin coating mode in a coating mode to spin-coat on the surface of the hole transport layer, rotating at 6000rpm (revolutions per minute) for 30s, using 1000 microliter of diethyl ether as a reverse extraction solvent after the spin coating is stable, and then heating and annealing at 100 ℃ for 20min to form the perovskite/hole transport layer450nm thick CH3NH3PbI3A perovskite thin film.
Step SF4, an electron transport layer is prepared on the side of the perovskite thin film remote from the hole transport layer.
Step SF5, preparing a back electrode layer.
The step SF4 and the step SF5 correspond to the aforementioned SA4 and SA5, respectively, and are not described herein again to avoid repetition.
And (3) performance testing:
the perovskite solar cells manufactured in example 1, example 2, example 3, example 4, example 5 and comparative example have an effective area of 1cm2The test conditions are as follows: spectral distribution AM1.5G, illumination intensity 1000W/m2AAA solar simulator, I-V curves were measured using a Keithly model 2400 digital Source Meter, all tests were performed in an atmospheric environment (25 deg.C, 45 RH%). The test results are given in table 1 below.
Wherein, table 1 is: the test results of the perovskite solar cells prepared by example 1, example 2, example 3, example 4, example 5 and comparative example are shown in the table. In table 1, Isc is the short circuit current density of the perovskite solar cell, and the unit is: mA/cm2. Voc is the open circuit voltage of the perovskite solar cell in V. FF is the fill factor of the perovskite solar cell. Eff is the conversion efficiency of the perovskite solar cell. RS is the reverse sweep and FS is the forward sweep.
Table 1: test results of perovskite solar cells manufactured in example 1, example 2, example 3, example 4, example 5 and comparative example respectively
Comparison table
As can be seen from table 1, the short-circuit current density, the open-circuit voltage, the fill factor, and the conversion efficiency of the perovskite solar cells manufactured in examples 1, 2, 3, 4, 5, and the comparative examples are all approximately equal.
Compared with the conventional perovskite solar cell or the conventional perovskite solar cell production method in the comparative example, the perovskite solar cell production method in the embodiment of the invention has the advantages of easy formation of a uniform perovskite liquid film, low film forming difficulty, high utilization rate of the perovskite solution, less material waste, reduction of environmental pollution, contribution to mass production of large-area perovskite thin films and the like, and is basically consistent with the performance of the perovskite solar cell obtained by the perovskite solar cell production method in the prior art.
It should be noted that for simplicity of description, the method embodiments are described as a series of acts or combination of acts, but those skilled in the art will recognize that the present invention is not limited by the illustrated order of acts, as some steps may occur in other orders or concurrently depending on the embodiment of the invention. Furthermore, those skilled in the art will appreciate that the embodiments described in the specification are presently preferred and that no particular act is required to implement the invention.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative rather than restrictive, and it will be apparent to those skilled in the art that many more modifications and variations can be made without departing from the spirit of the invention and the scope of the appended claims.
Claims (11)
1. A method of producing a perovskite thin film, comprising the steps of:
providing a substrate;
providing a perovskite solution; wherein the solvent in the perovskite solution comprises a mixture of N, N-dimethylformamide and an alcohol;
coating the perovskite solution on the substrate to obtain a perovskite liquid film;
and curing the perovskite liquid film to obtain the perovskite thin film.
2. The production method of the perovskite thin film as claimed in claim 1, wherein a volume of N, N-dimethylformamide in the solvent is equal to or larger than a volume of alcohol.
3. The production method of a perovskite thin film as claimed in claim 1, wherein N, N-dimethylformamide is mixed with an alcohol in a volume ratio of 1:1 to 4:1 in the solvent.
4. The production method of the perovskite thin film as claimed in claim 1 or 2, wherein the alcohol is selected from the group consisting of: at least one of methanol, ethanol and isopropanol.
5. The production method of the perovskite thin film as claimed in claim 1 or 2, wherein the coating is any one selected from spin coating, blade coating, slit coating, ultrasonic spray coating, and drop casting.
6. The method for producing a perovskite thin film according to claim 5, wherein the coating is performed while the temperature of the substrate is kept at 25 ℃ or lower in each of the blade coating, slit coating, ultrasonic spraying, or drop casting.
7. The method for producing a perovskite thin film as claimed in claim 1, wherein the step of curing the perovskite liquid film comprises:
and curing the perovskite liquid film by adopting a protective gas blowing and spraying mode to obtain the perovskite film.
8. The method for producing a perovskite thin film as claimed in claim 1 or 2, wherein the step of providing a substrate comprises:
providing a substrate;
sequentially arranging a front electrode layer and a first current carrier transmission layer on the substrate; the first carrier transport layer is: one of a hole transport layer or an electron transport layer.
9. The production method of a perovskite thin film as claimed in claim 1 or 2, wherein the thickness of the perovskite thin film is 100-1000 nm.
10. The production method of a perovskite thin film as claimed in claim 1 or 2, wherein the concentration of the perovskite solution is 0.2mol/L or more and 1.5mol/L or less.
11. The preparation method of the perovskite solar cell is characterized by comprising the following steps:
obtaining a perovskite thin film formed on a substrate by the method for producing a perovskite thin film as defined in any one of claims 1 to 10;
forming a second carrier transmission layer and a back electrode layer on one side of the perovskite thin film far away from the substrate in sequence; wherein the second carrier transport layer and the first carrier transport layer included in the substrate are of opposite types.
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| CN109545988A (en) * | 2018-11-26 | 2019-03-29 | 西安交通大学 | Hot glue film original position rapid-curing cutback crystallization preparation method is climbed in the cold base suppression of the liquid film of the uniform perovskite film of flannelette |
| CN109817811A (en) * | 2019-02-11 | 2019-05-28 | 西南大学 | Exempt to anneal, the perovskite photovoltaic device for exempting from anti-solvent and preparation method thereof |
| CN110311037A (en) * | 2019-06-24 | 2019-10-08 | 浙江理工大学 | A kind of flexibility perovskite hole transmission layer used for solar batteries and its preparation method and application |
| CN110335946A (en) * | 2019-06-26 | 2019-10-15 | 上海黎元新能源科技有限公司 | A kind of the perovskite extinction layer material and solar battery of perovskite solar battery |
| CN110379889A (en) * | 2019-07-31 | 2019-10-25 | 浙江天地环保科技有限公司 | A kind of preparation method of high efficiency high stability full-inorganic perovskite solar battery |
| CN111430554A (en) * | 2020-03-25 | 2020-07-17 | 杭州纤纳光电科技有限公司 | Preparation method of perovskite thin film added with triiodide, preparation method of battery and battery |
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