CN111048668B - Method for preparing perovskite film based on solution method, perovskite film and application - Google Patents

Method for preparing perovskite film based on solution method, perovskite film and application Download PDF

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CN111048668B
CN111048668B CN201911352144.2A CN201911352144A CN111048668B CN 111048668 B CN111048668 B CN 111048668B CN 201911352144 A CN201911352144 A CN 201911352144A CN 111048668 B CN111048668 B CN 111048668B
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perovskite
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CN111048668A (en
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麦耀华
刘冲
杨玉照
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Guangzhou Jinan University Science Park Management Co ltd
Mai Yaohua
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    • H—ELECTRICITY
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    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
    • H01L31/0264—Inorganic materials
    • H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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    • 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
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    • H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
    • H10K71/441—Thermal treatment, e.g. annealing in the presence of a solvent vapour in the presence of solvent vapors, e.g. solvent vapour annealing
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    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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Abstract

The invention belongs to the field of thin film solar cells, and discloses a preparation method of a perovskite thin film based on a liquid phase method. The method specifically comprises the following steps: depositing a perovskite precursor solution on a substrate to form a liquid film, then placing a heat conduction module on a hot table, suspending the substrate on the hot table for baking, and taking down the substrate and placing the substrate on the surface of the hot table for annealing treatment after the color of the perovskite thin film substrate is gradually deepened to obtain the perovskite thin film. According to the invention, the heat conducting module is arranged on the heat platform at the central position of the substrate, so that the baking temperature of the substrate in the central area is increased, perovskite crystal nuclei on the edge area and the central area of the substrate are simultaneously precipitated, and the problem of film nonuniformity caused by hysteresis phenomenon existing in the precipitation of the crystal nuclei is solved. Meanwhile, the method can adjust the size and the shape of the heat conduction module, so that the central area of the substrate is ensured not to cause the lag of crystal nucleus precipitation due to the increase of the size of the substrate.

Description

Method for preparing perovskite film based on solution method, perovskite film and application
Technical Field
The invention belongs to the field of thin film solar cell devices, and particularly relates to a method for preparing a perovskite thin film based on a solution method, the perovskite thin film and application.
Background
In recent years, with the development of industry and the increase of population, the demand of global energy is increasing, which leads to the increase of the dependence on fossil energy, but the conventional combustion of fossil energy causes serious environmental pollution and energy crisis. Therefore, the development and utilization of renewable energy have been receiving wide attention, wherein solar energy is an inexhaustible green renewable energy, and a solar cell is a photovoltaic device for directly converting solar energy into electric energy. At present, the silicon crystal solar cell is the dominant industrial solar cell, but the pollution is still generated in the production process, and in addition, the cost reduction is still limited by the complex preparation process, so that the development of a novel high-efficiency and low-cost solar cell is still heavy and far-going. Perovskite solar cells are a novel solar cell technology using perovskite materials as absorption layers, and due to the low preparation cost, flexible and variable preparation processes and the fast improvement of energy conversion efficiency, more and more attention has been paid. The preparation method of the perovskite thin film can be mainly divided into: solution processes, gas phase processes, and gas phase assisted liquid phase processes, and the like. The liquid phase method is simple to operate and is the most widely used perovskite thin film preparation method at present. The liquid phase method also includes spin coating, knife coating, screen printing, ink jet printing and the like, wherein the spin coating is widely adopted due to the characteristics of simple preparation process, high local film forming uniformity and the like. Antisolvent methods developed based on spin coating, i.e. using poor solvents such as: chlorobenzene, ether and the like promote the perovskite crystal nucleus to be separated out from the solvent, and then the solvent is volatilized rapidly through the annealing process, so that crystals grow up along the crystal nucleus to cover the whole substrate, and a compact and fully-covered perovskite thin film is formed. However, the anti-solvent method is applicable to a narrow process window, and is sensitive to the size of the substrate, the anti-solvent dropping time and the anti-solvent addition amount, which finally causes a problem of poor reproducibility. Aiming at the problem, a two-step temperature control method is adopted, namely a low-temperature heating process is introduced, in the process, along with the slow volatilization of a solvent, partial perovskite crystal nucleus is separated out, the effect similar to that of an anti-solvent can be achieved, and then the high-density and full-coverage perovskite thin film can be obtained through high-temperature annealing. However, the method has the defect that the crystal nucleus precipitation is asynchronous in each area on the substrate due to the nonuniformity of the thermal field distribution at low temperature, so that the problem is more prominent along with the enlargement of the size of the substrate, and therefore, the method develops a new two-step temperature control method, and has very important significance for preparing the perovskite thin film on the large-size substrate.
Disclosure of Invention
The invention mainly aims to provide a method for preparing a perovskite thin film based on a solution method. By adopting the preparation method, a uniform perovskite thin film can be obtained on a large-area substrate.
The invention also aims to provide the perovskite thin film prepared by the method.
The invention further aims to provide the application of the perovskite thin film in a solar cell.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a perovskite thin film based on a solution method comprises the following steps:
depositing a perovskite precursor solution on a substrate to form a liquid film, then placing a heat conduction module on a hot table, suspending the substrate on the hot table for baking, taking down the substrate and placing the substrate on the surface of the hot table for annealing treatment after the color of the perovskite thin film substrate is gradually deepened, thereby obtaining the perovskite thin film.
Preferably, the solute in the perovskite precursor solution is PbI 2 、PbBr 2 、InCl 3 At least one of CsI, and formamidinium iodide (FAI). The solvent in the perovskite precursor solution is at least one of dimethyl sulfoxide, Dimethylformamide (DMF) and gamma-hydroxy-butyrolactone (GBL).
Preferably, the concentration of each solute in the perovskite precursor solution is 0.5-1000 mg/mL independently; more preferably 1 to 800 mg/mL.
Preferably, the substrate is prepared by the following method: and spin-coating an organic solution containing the charge transport layer material on transparent conductive glass and drying to obtain the substrate.
Wherein the charge transport layer material is a hole transport layer material or an electron transport layer material; wherein the hole transport layer is made of nickel oxide, cuprous iodide, cuprous thiocyanate, PEDOT: one of PSS (poly (3, 4-ethylenedioxythiophene): poly (styrenesulfonic acid)), PTAA (poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine ]); the electron transport layer material is one of titanium oxide, zinc oxide, tin oxide, PCBM and C60.
More preferably, when the hole transport layer material is nickel oxide, the nickel source precursor is spin-coated on the transparent conductive glass and then dried. The nickel source is at least one of nickel acetate, nickel chloride and nickel nitrate.
The transparent conductive glass is one of FTO (fluorine-doped tin oxide), ITO (indium tin oxide) and AZO (aluminum-doped zinc oxide). The thickness of the transparent conductive glass is 300-600 nm.
The drying temperature is 100-600 ℃, and the drying time is 10-60 minutes; preferably, the drying temperature is 400 ℃ and the drying time is 30 minutes.
More preferably, the transparent conductive glass is firstly cleaned, specifically, the transparent conductive glass is ultrasonically cleaned by water and ethanol, then dried, and then is subjected to oxygen plasma treatment.
Preferably, the perovskite thin film is deposited by at least one of a spin coating method, a doctor blading method, a screen printing method and an ink jet printing method. More preferably, the perovskite thin film is deposited by a spin coating method; wherein the spin coating speed is 1000-5000 rpm, preferably 2500 rpm.
Preferably, the substrate is suspended on the hot stage at a distance of 2mm to 20 mm.
Preferably, the heat conducting module is made of metal, glass or ceramic material.
Preferably, the heat conducting module is located at the center position below the substrate, and the area of the heat conducting module is smaller than or equal to that of the substrate.
Preferably, the temperature of the heating table during baking is 100-300 ℃, and the baking is stopped when the color of the film is dark to brown; more preferably, the temperature of the hot stage at the time of baking is 160 ℃.
The annealing temperature is 100-300 ℃, and the annealing time is 5-20 min; more preferably, the temperature of the annealing treatment is 160 ℃ and the time is 10 min.
A perovskite thin film is prepared by the method for preparing the perovskite thin film based on the solution method.
Preferably, the perovskite thin film has a structure of: transparent conductive electrode/charge transport layer/perovskite layer.
Wherein the perovskite layer is an organic-inorganic hybrid perovskite material or an all-inorganic perovskite material.
The thickness of the charge transport layer is 10nm-50nm, and the thickness of the perovskite layer is 300nm-600 nm.
The perovskite thin film is applied to a solar cell.
Compared with the prior art, the invention has the following advantages and effects:
(1) the invention enhances the baking temperature intensity of the substrate in the central area by placing the heat conduction module under the suspension substrate, thereby simultaneously precipitating perovskite crystal nuclei on the edge area and the central area of the substrate and improving the problem of non-uniformity of a film caused by hysteresis phenomenon existing in the precipitation of the crystal nuclei.
(2) The invention can adjust the size and the shape of the heat conduction module according to the increase of the size of the substrate, thereby ensuring that the central area of the substrate does not cause the lag of crystal nucleus precipitation due to the increase of the size of the substrate, and the method can be suitable for depositing the perovskite thin film on the large-size substrate.
Drawings
FIG. 1 is a schematic diagram of a process for preparing the present invention.
FIG. 2 is a graph showing a comparison of heating processes before and after the modification in example 1, wherein (a) and (b) are before the modification and (c) and (d) are after the modification.
FIG. 3 is a comparison of perovskite thin films prepared before and after the improvement of example 1.
Detailed Description
The invention will be further elucidated with reference to the following specific examples and the drawing, without being limited thereto. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1 preparation of an all-inorganic perovskite thin film having a substrate size of 5 × 5 cm
1) Cleaning FTO conductive glass:
and ultrasonically cleaning the FTO conductive glass by deionized water and ethanol, drying the FTO conductive glass in a blast drying oven, and then carrying out oxygen plasma treatment for 10 minutes.
2) Preparing a nickel oxide hole transport layer:
the nickel acetate powder was dissolved in absolute ethanol at a concentration of 25mg/mL and spin-coated on FTO conductive glass at 5000rpm, followed by sintering at a high temperature of 400 ℃ for 30 minutes.
3) Preparing an all-inorganic perovskite precursor solution:
277mg of PbI was taken 2 220mg of PbBr 2 1.3mg of InCl 3 316mg of CsI was dissolved in 1mL of dimethyl sulfoxide solvent, and the mixture was heated and stirred at 80 ℃ until all the CsI was dissolved.
4) Preparation of all-inorganic perovskite thin film
And spin-coating the perovskite precursor solution on the nickel oxide hole transport layer at 2500rpm by adopting a spin-coating method. And then, supporting and suspending the substrate on a 160 ℃ hot table by using a high-temperature-resistant adhesive tape to bake, and placing curved glass on the hot table at the central position of the substrate. And when the color of the perovskite thin film substrate is changed into brown, taking down the substrate, and then placing the substrate on a 160 ℃ hot table for annealing for 10 minutes to obtain the all-inorganic perovskite thin film.
The preparation method of the non-heat-conducting module before improvement is used as comparison. The difference from the above method is that step (4) adopts a spin coating method, and the perovskite precursor solution is spin coated on the nickel oxide hole transport layer at 2500 rpm. And then, supporting the substrate by using a high-temperature resistant adhesive tape, suspending the substrate on a 160 ℃ hot table, and baking the substrate, wherein the curved glass is not placed at the center of the substrate. And when the color of the perovskite thin film substrate is changed into brown, taking down the substrate, and then placing the substrate on a 160 ℃ hot bench for annealing for 10 minutes to obtain the all-inorganic perovskite thin film.
As shown in fig. 2a, the temperature of the substrate before being modified is raised from the edge region of the substrate first and then diffused to the central region, so that there is a lag in the temperature of the central region compared to the edge region, which results in the agglomeration of the perovskite crystal nuclei in the edge region after the perovskite crystal nuclei are precipitated in the central region, and finally a certain defect region is formed in the edge region after high temperature annealing, as shown in fig. 3 a.
As shown in fig. 2b, the improved temperature raising manner of the substrate is to raise the temperature of the edge region of the substrate and the central region of the substrate at the same time, so as to ensure that the temperature of each region on the substrate can be raised synchronously, reduce the hysteresis effect of temperature raising between the regions, and finally obtain the perovskite thin film with uniform film formation after high-temperature annealing, as shown in fig. 3 b.
Example 2 preparation of all-inorganic perovskite thin films of different hole transport layers with substrate dimensions of 5 x 5 cm
Following the procedure of example 1, only step 2) was changed to prepare solutions of different hole transport layer materials. The rest of the procedure was the same as in example 1.
The hole transport layer cuprous iodide is specifically operated as follows: a solution of cuprous iodide in acetonitrile was spin coated onto FTO conductive glass at 3000 rpm and subsequently annealed at 150 c for 10 minutes.
Hole transport layer PEDOT: the PSS specifically operates as follows: PEDOT: the aqueous PSS solution was spin coated onto FTO conductive glass at 3000 rpm, followed by annealing at 150 ℃ for 15 minutes.
The hole transport layer PTAA is specifically operative to: a1.5 mg/ml PTAA chlorobenzene solution was prepared and spin coated onto FTO conductive glass at 3000 rpm followed by annealing at 100 ℃ for 10 minutes.
The perovskite thin films prepared from the 3 different hole transport layers in this example are similar in picture to fig. 2b and 3 b. The temperature rise mode of the substrate temperature before improvement is that the temperature rise is firstly carried out on the edge area of the substrate and then the substrate temperature rises and then the substrate temperature is diffused to the central area, so that the temperature of the central area is lagged compared with that of the edge area, the perovskite crystal nuclei in the edge area are agglomerated after the perovskite crystal nuclei are separated out from the central area, and finally a certain defect area is generated in the edge area after high-temperature annealing.
The improved temperature rise mode of the substrate is that the edge area of the substrate and the central area of the substrate are simultaneously heated, so that the temperature of each area on the substrate can be synchronously raised, the hysteresis effect of temperature rise among the areas is reduced, and finally the perovskite thin film with uniform film formation can be obtained after high-temperature annealing.
Example 3 preparation of organic-inorganic hybrid perovskite thin film having substrate size of 5 x 5 cm
The steps of example 1 are followed, only step 3) is changed to prepare an organic-inorganic hybrid perovskite precursor solution.
The specific operation is as follows: 553.2mg of PbI are taken 2 175.44mg of FAI and 46.8mg of CsI were dissolved in a mixed solvent of 0.7mL of DMF and 0.3mL of GBL, and the mixture was stirred with heating at 80 ℃ until all the FAI and CsI were dissolved. The rest of the procedure was the same as in example 1.
As a result, as in example 1, the temperature of the substrate before being improved is raised from the edge region of the substrate first and then diffused to the central region, so that the temperature of the central region is delayed compared with that of the edge region, which results in that the perovskite crystal nuclei in the edge region are agglomerated after the perovskite crystal nuclei are precipitated in the central region, and finally a certain defect region is formed in the edge region after high-temperature annealing.
The improved temperature raising mode of the substrate is that the edge area of the substrate and the central area of the substrate are simultaneously raised, so that the temperature of each area on the substrate can be synchronously raised, the hysteresis effect of temperature raising among the areas is reduced, and finally the perovskite thin film with uniform film formation can be obtained after high-temperature annealing.
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 preparing a perovskite thin film based on a solution method is characterized by comprising the following steps:
depositing a perovskite precursor solution on a substrate to form a liquid film, then placing a heat conduction module on a hot table, suspending the substrate on the hot table for baking, taking down the substrate and placing the substrate on the surface of the hot table for annealing treatment after the color of the perovskite thin film substrate is gradually deepened, so as to obtain a perovskite thin film;
the heat conduction module is located at the center position below the substrate, and the area of the heat conduction module is smaller than or equal to that of the substrate.
2. The solution-based process for producing a perovskite thin film according to claim 1, characterized in that:
the solute in the perovskite precursor solution is PbI 2 、PbBr 2 、InCl 3 At least one of CsI and formamidinium iodide; the solvent in the perovskite precursor solution is at least one of dimethyl sulfoxide, dimethylformamide and gamma-hydroxy-butyrolactone.
3. The solution-based process for producing a perovskite thin film according to claim 1, characterized in that: the concentration of each solute in the perovskite precursor solution is 0.5-1000 mg/mL independently.
4. The solution-based process for producing a perovskite thin film according to claim 1, wherein the substrate is produced by: spin-coating an organic solution containing a charge transport layer material on transparent conductive glass and drying to obtain a substrate;
wherein the charge transport layer material is a hole transport layer material or an electron transport layer material; wherein the hole transport layer is made of nickel oxide, cuprous iodide, cuprous thiocyanate, PEDOT: one of PSS and PTAA; the electron transport layer material is one of titanium oxide, zinc oxide, tin oxide, PCBM and C60;
the transparent conductive glass is one of FTO, ITO and AZO;
the drying temperature is 100-600 ℃, and the drying time is 10-60 minutes.
5. The solution-based process for producing a perovskite thin film according to claim 1, characterized in that: the distance between the substrate and the hot stage in a suspended mode is 2mm-20 mm.
6. The solution-based process for producing a perovskite thin film according to claim 1, characterized in that: the heat conduction module is made of metal, glass or ceramic materials.
7. The solution-based process for producing a perovskite thin film according to claim 1, characterized in that:
the temperature of the heating table is 100-300 ℃ during baking, and the baking is stopped when the color of the film is deepened to brown;
the annealing treatment temperature is 100-300 ℃, and the time is 5-20 min.
8. A perovskite thin film prepared by the method for preparing a perovskite thin film based on the solution method according to any one of claims 1 to 7.
9. The perovskite thin film of claim 8, wherein:
the perovskite thin film has the structure as follows: transparent conductive electrode/charge transport layer/perovskite layer;
wherein the perovskite layer is an organic-inorganic hybrid perovskite material or an all-inorganic perovskite material;
the thickness of the charge transport layer is 10nm-50nm, and the thickness of the perovskite layer is 300nm-600 nm.
10. Use of the perovskite thin film according to claim 8 in a solar cell.
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