CN115360307A - Preparation method of perovskite thin film - Google Patents
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Abstract
The invention provides a preparation method of a perovskite thin film, which comprises the following steps: a) Placing the perovskite precursor solution on the surface of a substrate to obtain a perovskite precursor solution film; b) And c) carrying out vacuum anti-solvent annealing on the perovskite precursor solution film obtained in the step a) to obtain the perovskite film. Compared with the prior art, the invention provides a method for preparing the perovskite thin film under the atmosphere control condition, which is used for realizing controllable preparation of the perovskite solar cell; aiming at the defects of the existing perovskite thin film in the solution method preparation process and the current requirements for improving the performance of a perovskite battery device and a photoelectric device, a novel vacuum anti-solvent annealing mode is provided, and the perovskite thin film is annealed by using a vacuum liquid anti-solvent vaporization anti-solvent (chlorobenzene, ether and the like), so that the controllable preparation of the device can be realized, and the repeatability and the yield of the device preparation can be ensured.
Description
Technical Field
The invention relates to the technical field of solar cells, in particular to a preparation method of a perovskite thin film.
Background
The organic-inorganic hybrid perovskite solar cell is one of the hottest photovoltaic materials in the organic-inorganic hybrid perovskite materials at present, and has higher theoretical conversion efficiency than other photovoltaic materials in a theoretical angle, and the efficiency reaches 25.7 percent at present; in addition, the organic-inorganic hybrid perovskite layer has a processable optical characteristic, can realize the preparation of solar cells of the types of crystalline silicon/perovskite lamination, perovskite/perovskite lamination and organic/perovskite lamination, and provides multiple possibilities for reducing cost and improving efficiency of the solar cells. From the aspect of industrial preparation, the perovskite solar cell has low material consumption and wide raw material source, and is suitable for industrial production. Therefore, the preparation of low-cost, high-photoelectric conversion efficiency and high-stability solar cells by a simple method is a main purpose of the perovskite industrialization at present. The realization of the high-efficiency perovskite battery mainly comprises the contents of battery structure design, transmission layer selection, perovskite active layer preparation, interface passivation and the like, wherein the most significant and most challenging is the controllable preparation of the large-size perovskite active layer, and for example, small changes of material formula, preparation step control, preparation atmosphere (chemical atmosphere, environmental humidity and the like), phase formation temperature control and the like can have a significant influence on the preparation of the perovskite active layer.
Disclosure of Invention
In view of this, the present invention provides a method for preparing a perovskite thin film, which can realize controllable preparation of a device and ensure repeatability and yield of the device preparation by adopting a vacuum anti-solvent annealing manner.
The invention provides a preparation method of a perovskite thin film, which comprises the following steps:
a) Placing the perovskite precursor solution on the surface of a substrate to obtain a perovskite precursor solution film;
b) And c) carrying out vacuum anti-solvent annealing on the perovskite precursor solution film obtained in the step a) to obtain the perovskite film.
Preferably, the perovskite precursor solution is placed on the surface of the substrate in step a) by spin coating, blade coating, slot coating or spray coating.
Preferably, the thin film of perovskite precursor solution in step a) has ABX 3 A crystal structure of the form (A) is an organic cation and/or an inorganic cation, B is a divalent metal ion, and X is I - 、Br - And Cl - One or more of (a).
Preferably, the positive divalent metal ion is Pb 2+ Or Sn 2+ 。
Preferably, the antisolvent in step b) is selected from one or more of chlorobenzene, diethyl ether, acetone, toluene, ethyl acetate and chloroform.
Preferably, the vacuum anti-solvent annealing process in the step b) specifically comprises the following steps:
and transferring the perovskite precursor solution film to a vacuum cavity, vacuumizing, introducing an anti-solvent to realize vaporization, keeping for 0.5min to 2min, and then annealing to obtain the perovskite film.
Preferably, the anti-solvent is used in an amount > 1ml/m 3 。
Preferably, the vacuum degree of the vacuum pumping is less than 100Pa.
Preferably, the annealing treatment temperature is 70-200 ℃, and the time is 3-60min.
The invention provides a preparation method of a perovskite thin film, which comprises the following steps: a) Placing the perovskite precursor solution on the surface of a substrate to obtain a perovskite precursor solution film; b) And c) carrying out vacuum anti-solvent annealing on the perovskite precursor solution film obtained in the step a) to obtain the perovskite film. Compared with the prior art, the invention provides a method for preparing the perovskite thin film under the atmosphere control condition, which is used for realizing controllable preparation of the perovskite solar cell; aiming at the defects of the existing perovskite thin film in the solution method preparation process and the current requirements for improving the performance of a perovskite battery device and a photoelectric device, a novel vacuum anti-solvent annealing mode is provided, and the perovskite thin film is annealed by using a vacuum liquid anti-solvent vaporization anti-solvent (chlorobenzene, ether and the like), so that the controllable preparation of the device can be realized, and the repeatability and the yield of the device preparation can be ensured.
In addition, the preparation method provided by the invention has the advantages of simple process, mild conditions, easiness in control and wide application prospect.
Drawings
FIG. 1 is a schematic diagram of a method for preparing a perovskite thin film according to an embodiment of the invention;
FIG. 2 is a graph of current density versus voltage for a cell prepared in example 1 of the present invention;
FIG. 3 is a graph of current density versus voltage for a cell prepared in example 2 of the present invention;
fig. 4 is a graph of current density versus voltage for a cell prepared in example 3 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below with reference to embodiments of the present invention, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a preparation method of a perovskite thin film, which comprises the following steps:
a) Placing the perovskite precursor solution on the surface of a substrate to obtain a perovskite precursor solution film;
b) And b) carrying out vacuum anti-solvent annealing on the perovskite precursor solution film obtained in the step a) to obtain the perovskite film.
Firstly, placing a perovskite precursor solution on the surface of a substrate to obtain the perovskite precursor solution film.
In the invention, the perovskite precursor solution is preferably placed on the surface of the substrate by spin coating, blade coating, slit coating or spray coating; the deposition of the perovskite thin film is performed by the above-mentioned liquid phase coating method well known to those skilled in the art, and the present invention is not particularly limited thereto.
In the present invention, the perovskite precursor solution thin film preferably has ABX 3 A crystal structure of the form (A) is an organic cation and/or an inorganic cation, B is a divalent metal ion, and X is I - 、Br - And Cl - One or more of (a). In the present invention, the positive divalent metal ion is preferably Pb 2+ Or Sn 2+ More preferably Pb 2+ . On this basis, a perovskite precursor solution capable of forming a thin film of the perovskite precursor solution is known to those skilled in the art, and the method for preparing the perovskite precursor solution is not particularly limited by those skilled in the art.
In the present invention, the thin film of the perovskite precursor solution is also required to have a certain thickness (generally greater than 100 nm) and to have good adhesion to the substrate.
The type and source of the substrate are not particularly limited in the present invention, and the substrate is preferably a charge transport layer composited on a transparent conductive substrate as is well known to those skilled in the art, according to the basic requirements for preparing perovskite solar cells.
In the present invention, the transparent conductive substrate may be ITO glass, FTO glass, AZO glass, conductive PET, and other common transparent substrates known to those skilled in the art, and is preferably ITO glass or FTO glass.
In the present invention, the charge transport layer includes an electron transport layer and a hole transport layer; the electron transport layer is preferably SnO 2 Layer, tiO 2 Layer or C60 and derivatives thereof, more preferably SnO 2 A layer or a C60 electron transport layer;the thickness of the electronic transmission layer is preferably 10nm to 100nm, and more preferably 20nm to 40nm; the hole transport layer is preferably a Spiro-OMeTAD layer, a NiOx layer or a CuOx layer, more preferably a Spiro-OMeTAD layer or a NiOx layer; the thickness of the hole transport layer is preferably 10nm to 100nm, and more preferably 20nm to 60nm.
After the perovskite precursor solution film is obtained, the invention carries out vacuum anti-solvent annealing on the obtained perovskite precursor solution film to obtain the perovskite film.
In the present invention, the antisolvent is preferably selected from one or more of chlorobenzene, diethyl ether, acetone, toluene, ethyl acetate and chloroform, and more preferably chlorobenzene or diethyl ether.
In the present invention, the vacuum anti-solvent annealing process preferably includes:
transferring the perovskite precursor solution thin film to a vacuum cavity, vacuumizing, introducing an anti-solvent to realize vaporization, keeping for 0.5min to 2min, and then carrying out annealing treatment to obtain a perovskite thin film;
more preferably:
transferring the perovskite precursor solution film to a vacuum cavity, vacuumizing, introducing an anti-solvent to realize vaporization, keeping for 1min, and then annealing to obtain the perovskite film.
The source of the antisolvent in the present invention is not particularly limited, and commercially available products known to those skilled in the art may be used. The anti-solvent is placed in a container and communicated with a vacuum cavity, and the anti-solvent is controlled to enter the vacuum cavity through a valve in the middle; the anti-solvent valve is opened to release the anti-solvent in the process of introducing the anti-solvent.
In the present invention, the anti-solvent is preferably used in an amount of > 1ml/m 3 。
In the present invention, the degree of vacuum of the evacuation is preferably < 100Pa, and more preferably from 7Pa to 10Pa.
In the invention, the annealing treatment temperature is preferably 70-200 ℃, more preferably 100-150 ℃, and the time is preferably 3-60min, more preferably 10-45min.
The invention provides a method for preparing a perovskite thin film under an atmosphere control condition, which is used for realizing controllable preparation of a perovskite solar cell; aiming at the defects of the existing perovskite thin film in the solution method preparation process and the current requirements for improving the performance of a perovskite battery device and improving the performance of a photoelectric device, a novel vacuum anti-solvent annealing mode is provided (the process of realizing the anti-solvent preparation by the anti-solvent gas state under the vacuum atmosphere and the traditional liquid anti-solvent action process are abandoned), the perovskite thin film is annealed by using the vacuum liquid anti-solvent vaporization anti-solvent (chlorobenzene, ether and the like), the controllable preparation of the device can be realized, the repeatability and the yield of the device preparation are ensured, and the method is particularly suitable for preparing an organic-inorganic hybrid perovskite solar battery absorption layer (perovskite thin film).
The invention provides a preparation method of a perovskite thin film, which comprises the following steps: a) Placing the perovskite precursor solution on the surface of a substrate to obtain a perovskite precursor solution film; b) And b) carrying out vacuum anti-solvent annealing on the perovskite precursor solution film obtained in the step a) to obtain the perovskite film. Compared with the prior art, the invention provides a method for preparing a perovskite thin film under an atmosphere control condition, which is used for realizing controllable preparation of a perovskite solar cell; aiming at the defects of the existing perovskite thin film in the solution method preparation process and the current requirements for improving the performance of a perovskite battery device and a photoelectric device, a novel vacuum anti-solvent annealing mode is provided, and the perovskite thin film is annealed by using a vacuum liquid anti-solvent vaporization anti-solvent (chlorobenzene, ether and the like), so that the controllable preparation of the device can be realized, and the repeatability and the yield of the device preparation can be ensured.
In addition, the preparation method provided by the invention has the advantages of simple process, mild condition, easiness in control and wide application prospect.
In order to further illustrate the present invention, the following examples are provided for illustrative purposes.
Example 1
10ml of chlorobenzene was added to the vessel as an anti-solvent.
Indium Tin Oxide (ITO) glass (glass thickness 2mm, ITO film layer) of 1.5cm multiplied by 1.5cm is added into the glassThickness 100 nm) were respectively washed with ethanol, isopropyl alcohol (IPA) and acetone for 30 minutes, and dried with a nitrogen gun; then adding tin dioxide (SnO) 2 ) The volume ratio of stock solution to ultrapure water is 1:5, fully stirring to obtain SnO 2 Precursor solution; taking 50 mu L of SnO 2 Uniformly spreading the precursor solution on the surface of the ITO conductive glass, wherein the parameters of a spin coater are set to 4000rpm/s for 30s; then placing the mixture on a hot table at 150 ℃ for annealing for 30min to obtain SnO 2 Thin film (30 nm); snO prepared by the above 2 And (3) treating the film in an ultraviolet ozone cleaner for 30min for subsequent spin coating.
In a volume ratio of 4:1, preparing a perovskite precursor solution a (1.2M) in a mixed solvent of DMF and DMSO: pbI 2 /PbBr 2 Is 0.85:0.15, molar ratio FAI/MABr of 0.85:0.15, (PbI) 2 +PbBr 2 ) The molar ratio of (FAI + MABr) was 1:1; 60 mu.L of the solution A is uniformly paved on the annealed SnO 2 Setting parameters of a spin coater on the surface of the film at 4000rpm for 30s to obtain a perovskite precursor solution film; transferring the perovskite precursor solution film to a vacuum cavity (0.3 m multiplied by 0.2 m), quickly vacuumizing to 10Pa, opening an anti-solvent valve, releasing the anti-solvent, keeping for 1min, then heating the film to 120 ℃, and preserving heat for 15min to obtain the perovskite film.
Spin-coat a Spiro-OMeTAD solution (60. Mu.L of 70mg/mL chlorobenzene solution) at 2800rpm onto the prepared perovskite thin film for 30s; finally, the top Au layer with a thickness of 100nm was thermally evaporated by using a high vacuum evaporation apparatus, to obtain a battery device.
Comparative example 1
Obtaining a battery device by adopting the preparation method provided by the embodiment 1; the differences are that: and (3) annealing without adopting a vacuum anti-solvent, dropwise adding anti-solvent chlorobenzene in the perovskite film-forming spin coating process, heating the perovskite precursor solution film to 120 ℃, and preserving heat for 15min to obtain the perovskite film.
The performance data of the battery devices provided in example 1 and comparative example 1 are shown in table 1.
Table 1 performance data for the cells prepared in example 1 and comparative example 1
| Open circuit voltage (V) | Filling factor (%) | Current Density (mA cm) -2 ） | Photoelectric conversion efficiency (%) | |
| Example 1 | 1.05 | 72.31 | 22.03 | 16.81 |
| Comparative example 1 | 1.04 | 66.34 | 21.38 | 14.85 |
Example 2
5ml of diethyl ether was added to the vessel as an anti-solvent.
Indium Tin Oxide (ITO) glass (glass thickness is 2mm, ITO film thickness is 100 nm) with the thickness of 1.5cm multiplied by 1.5cm is respectively cleaned by ethanol, isopropanol (IPA) and acetone for 30 minutes and dried by a nitrogen gun; then adding tin dioxide (SnO) 2 ) The stock solution and the ultrapure water are in volume ratio1:5, fully stirring to obtain SnO 2 Precursor solution; taking 50 mu L SnO 2 Uniformly spreading the precursor solution on the surface of the ITO conductive glass, wherein the parameters of a spin coater are set to 4000rpm/s for 30s; then placing the mixture on a hot bench at 150 ℃ for annealing for 30min to obtain SnO 2 Thin film (30 nm); snO prepared by the above 2 And (3) treating the film in an ultraviolet ozone cleaner for 30min for subsequent spin coating.
In a volume ratio of 4:1 in a mixed solvent of DMF and DMSO, perovskite precursor solution a (1.2M): pbI 2 /PbBr 2 Is 0.85:0.15, molar ratio FAI/MABr of 0.85:0.15, (PbI) 2 +PbBr 2 ) The molar ratio of (FAI + MABr) was 1:1; 60 mu.L of the solution A is uniformly paved on the annealed SnO 2 Setting parameters of a spin coater on the surface of the film at 4000rpm for 30s to obtain a perovskite precursor solution film; transferring the perovskite precursor solution film to a vacuum cavity (0.3 m multiplied by 0.2 m), quickly vacuumizing to 10Pa, opening an anti-solvent valve, releasing the anti-solvent, keeping for 1min, then heating the film to 120 ℃, and preserving heat for 15min to obtain the perovskite film.
Spiro-OMeTAD solution (60 μ L of 70mg/mL chlorobenzene solution) was spin-coated onto the prepared perovskite thin film at 2800rpm for 30s; finally, the top Au layer with a thickness of 100nm was thermally evaporated by using a high vacuum evaporation apparatus to obtain a battery device.
Comparative example 2
Obtaining a battery device by adopting the preparation method provided by the embodiment 2; the difference lies in that: and (3) annealing without adopting a vacuum anti-solvent, dropwise adding anti-solvent ethyl ether in the perovskite film-forming spin coating process, then heating the perovskite precursor solution film to 120 ℃, and preserving heat for 15min to obtain the perovskite film.
The performance data of the battery devices provided in example 2 and comparative example 2 are shown in table 2.
Table 2 various performance data of the batteries prepared in example 2 and comparative example 2
| Open circuit voltage (V) | Filling factor (%) | Current Density (mA cm) -2 ） | Photoelectric conversion efficiency (%) | |
| Example 2 | 1.08 | 71.42 | 22.01 | 17.06 |
| Comparative example 2 | 1.07 | 68.23 | 21.33 | 15.63 |
Example 3
5ml of diethyl ether was added to the vessel as an anti-solvent.
FTO glass (thickness of glass is 1mm, thickness of FTO film layer is 200 nm) with the thickness of 10cm multiplied by 10 cm; a NiOx film (thickness 20 nm) on the surface of the substrate; the NiOx film was treated with oxygen plasma for 10min at 2kW.
Preparing 20 mass percent perovskite layer precursor solution A (CsBr: 0.15mol/L, pbI) 2 :1mol/L, FAI:0.85 mol/L), and the solvent is DMF + DMSO (volume ratio 8: 2) (ii) a 400 μ L of solution A was spread evenly on the surfacePreparing the NiOx film surface treated by the oxygen plasma by using a 400-micrometer scraper to obtain a perovskite precursor solution film; transferring the perovskite precursor solution film to a vacuum cavity (0.3 m multiplied by 0.2 m), quickly vacuumizing to 7Pa, opening an anti-solvent valve, releasing the anti-solvent, keeping for 1min, then heating the film to 150 ℃, and preserving heat for 10min to obtain the perovskite film.
A C60 electron transport layer (40 nm) is evaporated on the surface of the prepared perovskite thin film.
Finally, the electron transport layer is transferred to a thermal evaporation device, and the vacuum degree reaches 1 × 10 -5 And (3) starting to evaporate a copper electrode (Cu) under the condition of Pa, wherein the thickness is 100nm, and thus obtaining the battery device.
Comparative example 3
Obtaining a battery device by using the preparation method provided in example 3; the difference lies in that: directly heating the perovskite precursor solution film to 150 ℃ without adopting vacuum anti-solvent annealing, and preserving the heat for 10min to obtain the perovskite film.
The performance data of the battery devices provided in example 3 and comparative example 3 are shown in table 3.
Table 3 each performance data of the batteries prepared in example 3 and comparative example 3
| Open circuit voltage (V) | Filling factor (%) | Current Density (mA cm) -2 ） | Photoelectric conversion efficiency (%) | |
| Example 2 | 1.02 | 71.58 | 21.82 | 15.92 |
| Comparative example 2 | 0.98 | 63.48 | 21.45 | 13.30 |
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A preparation method of a perovskite thin film comprises the following steps:
a) Placing the perovskite precursor solution on the surface of a substrate to obtain a perovskite precursor solution film;
b) And b) carrying out vacuum anti-solvent annealing on the perovskite precursor solution film obtained in the step a) to obtain the perovskite film.
2. The method according to claim 1, wherein the perovskite precursor solution is applied to the surface of the substrate in step a) by spin coating, blade coating, slot coating or spray coating.
3. The method of claim 1Characterized in that the perovskite precursor solution thin film in the step a) has ABX 3 A crystal structure of the form (A) is an organic cation and/or an inorganic cation, B is a divalent metal ion, and X is I - 、Br - And Cl - One or more of (a).
4. The method according to claim 3, wherein the positive divalent metal ion is Pb 2+ Or Sn 2+ 。
5. The method according to claim 1, wherein the anti-solvent in step b) is one or more selected from chlorobenzene, diethyl ether, acetone, toluene, ethyl acetate and chloroform.
6. The preparation method according to claim 1, wherein the vacuum anti-solvent annealing in step b) comprises:
and transferring the perovskite precursor solution thin film to a vacuum cavity, vacuumizing, introducing an anti-solvent to realize vaporization, keeping for 0.5min to 2min, and then annealing to obtain the perovskite thin film.
7. The process according to claim 6, wherein the anti-solvent is used in an amount of > 1ml/m 3 。
8. The method of claim 6, wherein the vacuum is < 100Pa.
9. The preparation method of claim 6, wherein the annealing treatment is carried out at 70-200 ℃ for 3-60min.
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| CN114808124A (en) * | 2022-03-16 | 2022-07-29 | 暨南大学 | Preparation method of mixed halide perovskite single crystal and polycrystalline film |
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| CN209619436U (en) * | 2019-01-22 | 2019-11-12 | 苏州协鑫纳米科技有限公司 | Device based on degassing method preparation large area perovskite thin film |
| CN113809239A (en) * | 2021-08-25 | 2021-12-17 | 佛山仙湖实验室 | Perovskite thin film and anti-solvent preparation method of photoelectric detector containing perovskite thin film |
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