CN115036430A - Method for preparing perovskite film with assistance of external electric field and photoelectric device - Google Patents
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- CN115036430A CN115036430A CN202210948439.1A CN202210948439A CN115036430A CN 115036430 A CN115036430 A CN 115036430A CN 202210948439 A CN202210948439 A CN 202210948439A CN 115036430 A CN115036430 A CN 115036430A
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- 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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- H—ELECTRICITY
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- 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
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Abstract
The invention provides a method for preparing a perovskite film with the assistance of an external electric field and a photoelectric device, wherein the method comprises the following steps: forming a liquid film on the transparent electrode-charge transport layer substrate by adopting a liquid-phase film forming method on a precursor solution of the perovskite active layer; directly annealing the liquid film; or annealing after film forming by an anti-solvent method; or annealing after vacuum flash evaporation film forming to obtain a perovskite film; in the annealing process, an external electric field is applied to induce crystallization, and the voltage of the external electric field is more than 3V; the direction of the applied electric field is perpendicular to the film plane. According to the invention, the perovskite crystallization is assisted by the additional battery, so that the grain size of the perovskite material is increased, and the crystallinity is improved; the annealing temperature can be reduced compared to the annealing temperature without applying an external electric field. The perovskite battery prepared by the perovskite thin film prepared by the method provided by the invention has the advantages that the photoelectric conversion effect is optimized, and the stability of the device is enhanced.
Description
Technical Field
The invention belongs to the technical field of photoelectric devices, and particularly relates to a method for preparing a perovskite film by external electric field assistance and a photoelectric device.
Background
Perovskite oxides have been of great interest to researchers due to their abundant physical properties and application value. The photoelectric property is one of the properties of the perovskite oxide, and the perovskite oxide can be prepared into solar cells, photoelectric detectors and the like by applying the photoelectric property.
In order to prepare a high-photovoltaic perovskite solar cell, it is necessary to control the crystallization process of a perovskite material, reduce defects of a perovskite film layer, improve the grain size and crystallinity, and control the crystallization direction, and thus the research direction of those skilled in the art is always directed.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing a perovskite thin film with the aid of an external electric field, and an optoelectronic device, wherein the method can assist perovskite crystallization, and the prepared perovskite thin film is applied to a battery, so that the battery has high photoelectric conversion efficiency.
The invention provides a method for preparing a perovskite thin film with the assistance of an external electric field, which comprises the following steps:
forming a liquid film on the transparent electrode-hole transport layer substrate by adopting a liquid-phase film forming method for a precursor solution of the perovskite active layer;
directly annealing the liquid film; or annealing after film forming by an anti-solvent method; or annealing after vacuum flash evaporation film forming to obtain a perovskite film;
in the annealing process, an external electric field is applied to induce crystallization, and the voltage of the external electric field is more than 3V; the direction of the applied electric field is perpendicular to the film plane.
In the invention, the annealing temperature is 60-200 ℃.
In the invention, the annealing temperature is 60-200 ℃, preferably 90-170 ℃, and more preferably 100-150 ℃; in specific embodiments, the annealing temperature is 150 ℃, 100 ℃ or 130 ℃;
in the invention, the time of the external electric field is 5-60 min; in specific embodiments, the time for applying the electric field is 15min, 10min or 20 min.
In the invention, the voltage of the external electric field is adjustable in quadrature and direct current. The voltage is >3V, preferably > 5V; in a specific embodiment, the voltage of the applied electric field is 10V.
In the invention, the external electric field adopts a metal electrode and an oxide electrode;
the metal electrode is connected with the positive electrode; the oxide electrode is connected with the negative electrode. The distance between the two electrodes is 4mm, 5mm or 6 mm.
In the present invention, the metal electrode is selected from Au, Ag, Cu or Al;
the oxide electrode is selected from ITO, FTO and SnO 2 Or Al 2 O 3 。
According to the invention, the perovskite crystallization is assisted by an additional battery, so that the grain size of the perovskite material is increased, and the crystallinity is improved; the annealing temperature can be reduced compared to the annealing temperature without applying an external electric field. The perovskite battery prepared by the perovskite thin film prepared by the method provided by the invention has the advantages that the photoelectric conversion effect is optimized, and the stability of the device is enhanced.
In the present invention, the composition of the perovskite thin film is AMX 3 (ii) a In certain embodiments, the perovskite thin film is MAPbI 3 Or FA 0.85 Cs 0.15 PbI 2.55 Br 0.45 。
A is an organic cation and/or an inorganic cation;
the M is a divalent metal ion;
x is selected from I - 、Br - 、Cl - And/or F - 。
The invention provides a photoelectric device which comprises the perovskite thin film prepared by the preparation method in the technical scheme.
In the present invention, the optoelectronic device may be a perovskite solar cell, a perovskite light emitting diode, or a perovskite photodetector.
In the invention, the perovskite solar cell comprises a transparent electrode layer, a hole transport layer, a perovskite thin film layer, an electron transport layer and an electrode layer which are sequentially arranged. In a specific embodiment, the transparent electrode layer is an FTO thin film with a thickness of 100 nm; the hole transport layer is NiO x A film (x is less than or equal to 1) with the thickness of 20 nm; the electron transport layer is C60 and has a thickness of 40 nm; the electrode was an Au electrode with a thickness of 100 nm.
In the invention, the raw material adopted by the perovskite thin film layer comprises a precursor solution A;
the precursor solution comprises PbI 2 And CsI; or the precursor solution comprises PbI 2 MAI and DMF; or the precursor solution A comprises CsBr and PbI 2 And FAI; the solvent in the precursor solution is DMF and/or DMSO.
The invention provides a preparation method of an external electric field assisted perovskite thin film, which comprises the following steps: forming a liquid film on the transparent electrode-hole transport layer substrate by adopting a liquid-phase film forming method for a precursor solution of the perovskite active layer; directly annealing the liquid film; or annealing after film forming by an anti-solvent method; or annealing after vacuum flash evaporation film forming to obtain a perovskite film; in the annealing process, an external electric field is applied to induce crystallization, and the voltage of the external electric field is more than 3V; the direction of the applied electric field is perpendicular to the film plane. According to the invention, the perovskite crystallization is assisted by the additional battery, so that the grain size of the perovskite material is increased, and the crystallinity is improved; the annealing temperature can be reduced compared to the annealing temperature without applying an external electric field. The perovskite battery prepared by the perovskite thin film prepared by the method provided by the invention has the advantages that the photoelectric conversion effect is optimized, and the stability of the device is enhanced.
Drawings
FIG. 1 is a schematic diagram of perovskite crystallization assisted by an applied electric field provided by the present invention;
FIG. 2 is a voltage-current density curve of a battery prepared in example 1 of the present invention;
fig. 3 is an SEM image of a perovskite layer of the battery prepared in example 1 of the present invention;
fig. 4 is an SEM image of a perovskite layer of the battery prepared in comparative example 1 of the present invention;
fig. 5 is an XRD pattern of a perovskite layer of the battery prepared in example 1 of the present invention;
fig. 6 is a voltage-current density curve of a battery prepared in example 2 of the present invention;
FIG. 7 is a voltage-current density curve of a battery prepared in example 3 of the present invention;
fig. 8 is a statistical graph of the conversion efficiency of the batteries prepared in example 4 of the present invention and comparative example 4.
Detailed Description
For further illustration of the present invention, the following examples are provided to describe the method for preparing perovskite thin film assisted by external electric field and the optoelectronic device in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
The glass of 1 x 1cmFTO film (thickness of glass 2mm, thickness of FTO film layer 100 nm) was washed with ethanol, Isopropanol (IPA) and acetone for 30 minutes, respectively, and dried with a nitrogen gun. Sputtering a layer of compact NiO on the surface layer of the FTO film glass by adopting a magnetron sputtering method x The film (thickness 20nm, x is less than or equal to 1) has sputtering power of 80W for 30 min. Treating the sputtered film by oxygen plasma for 10min with the power of 2 kW;
600mg of lead iodide (PbI) are weighed 2 ) And 6mg of cesium iodide (CsI) were dissolved in 900. mu. L N, N-Dimethylformamide (DMF) and 100. mu.L of dimethyl sulfoxide (DMSO) and sufficiently dissolved by heating and stirring at 70 ℃ to obtain PbI 2 And (4) precursor solution A. Dissolving 80mg of formamidine hydroiodide (FAI) and 8mg of methylamine chloride (MACl) in 1mL of IPA solution, and stirring to fully dissolve the materials to obtain an organic salt solution B;
and (3) uniformly spreading 40 mu L of solution A on the surface of the annealed film, wherein the parameters of a spin coater are as follows: speed 2000rpm, time 30 s; then, the plate was placed on a 75 ℃ hot stand for 1min to form a coating. 70 μ L of organic salt solution B was spread evenly over the PbI-coated substrate 2 After precursor solutionThe parameters of the spin coater on the surface of the formed coating are as follows: speed 3000rpm, time 30 s; then placing the glass tube under 30V external field voltage (5 x 5cm Ag metal electrode, 5 x 5cm FTO electrode, 5mm distance between the two electrodes) and annealing for 15min at 150 ℃; and (3) likewise, no external electric field is added, and the heating platform annealing is carried out at 150 ℃ for 15min, so as to respectively obtain the perovskite thin film (400 nm).
Evaporating a C60 electron transport layer (40 nm) on the surface of the prepared perovskite film; then transferring the mixture into a thermal evaporation device, wherein the vacuum degree reaches 1 x 10 -5 Under the condition of Pa, evaporating an electrode (Au) on the electron transport layer with the thickness of 100nm to obtain a battery; these are referred to as example 1 and comparative example 1, respectively.
Table 1 performance test results of the batteries
Example 2
The glass of 1 x 1cmFTO film (thickness of glass 2mm, thickness of FTO film layer 100 nm) was washed with ethanol, Isopropanol (IPA) and acetone for 30 minutes, respectively, and dried with a nitrogen gun. Sputtering a layer of compact NiO on the surface layer of the FTO film glass by adopting a magnetron sputtering method x The film (thickness 20nm, x is less than or equal to 1) has sputtering power of 80W for 30 min. And (3) treating the sputtered film for 10min by using oxygen plasma with the power of 2 kW.
Weigh 4.61g PbI 2 Dissolving 1.50g of MAI in 6mL of DMF, heating at 70 ℃, and stirring for 15 minutes to fully dissolve the MAI, thereby obtaining a perovskite precursor solution A; uniformly spreading 50 mu L of perovskite precursor solution on a substrate to be spin-coated, wherein the parameters of a spin coater during spin coating are set as follows: accelerating at 4000 rpm, rotating at 3700 rpm for 30s, quickly dripping 1mL of chlorobenzene solution onto a spin-coated sheet when the spin-coating time reaches 7 s, and then annealing the film on a 100 ℃ hot table for 15min under 70V external field voltage (5 cm for Ag metal electrodes, 5cm for FTO electrodes and 4mm for two electrodes); and (3) likewise, no external electric field is added, and the heating table annealing is carried out at 100 ℃ for 15min, so as to respectively obtain the perovskite thin film (380 nm).
Respectively evaporating a layer of C6 on the surface of the prepared perovskite film0 electron transport layer (40 nm); transferring the electron transport layer to a thermal evaporation device with a vacuum degree of 1 × 10 -5 Evaporating an electrode (Au) under the Pa condition, wherein the thickness is 100nm, and obtaining a battery; these are referred to as example 2 and comparative example 2, respectively.
Table 2 results of performance test of the battery prepared in example 2
Example 3
The glass of 1 x 1cmFTO film (thickness of glass 2mm, thickness of FTO film layer 100 nm) was washed with ethanol, Isopropanol (IPA) and acetone for 30 minutes, respectively, and dried with a nitrogen gun. Sputtering a layer of compact NiO on the surface layer of the FTO film glass by adopting a magnetron sputtering method x The film (thickness is 20nm, x is less than or equal to 1) has the sputtering power of 80W for 30 min. And (3) treating the sputtered film for 10min by using oxygen plasma with the power of 2 kW.
Preparing 20 mass percent perovskite layer precursor solution (CsBr: 0.15mol/L, PbI) 2 : 1mol/L, FAI: 0.85 mol/L), taking DMF as a solvent, preparing a perovskite active layer on the surface of the polymer interface layer by adopting a spin coating method, wherein the spin coating speed is 3500 rpm, and the time is 40 s; transferring the spin-coated wet film to a vacuum device, quickly vacuumizing to below 20Pa for 20s, taking out a sample, and annealing at 130 ℃ for 15min under the external field voltage of 10V (5 x 5cm for an Ag metal electrode, 5 x 5cm for an FTO electrode, and 6mm distance between the two electrodes); and (3) likewise, no external electric field is added, and the thermal annealing is carried out at 130 ℃ for 15min, so as to respectively obtain the perovskite thin film (400 nm).
Evaporating a C60 electron transport layer (40 nm) on the surface of the prepared perovskite thin film, transferring the electron transport layer into a thermal evaporation device, and enabling the vacuum degree to reach 1 × 10 -5 Respectively starting to evaporate electrodes (Au) under the condition of Pa, wherein the thickness of the Au is 100 nm; then placing the mixture in an oxygen glove box for 12 hours, and oxidizing to obtain a battery; these are referred to as example 3 and comparative example 3, respectively.
Table 3 results of performance test of the battery prepared in example 3
Example 4
The glass of 4 x 4cmFTO film (thickness of glass 2mm, thickness of FTO film 100 nm) was washed with ethanol, Isopropanol (IPA) and acetone for 30 minutes, respectively, and dried with a nitrogen gun. Sputtering a layer of compact NiO on the surface layer of the FTO film glass by adopting a magnetron sputtering method x The film (thickness is 20nm, x is less than or equal to 1) has the sputtering power of 80W for 30 min. And (3) treating the sputtered film for 10min by using oxygen plasma with the power of 2 kW.
Preparing 20 mass percent perovskite layer precursor solution (CsBr: 0.15mol/L, PbI) 2 : 1mol/L, FAI: 0.85 mol/L) and a solvent of DMF DMSO (9: 1), coating a film on the surface of the substrate by a blade coating method (the blade coating parameters are that 100mL of the film is dripped on a scraper, blade coating is carried out after the substrate surface is spread, the speed is controlled to be 5 cm/s), then transferring the spin-coated wet film to a vacuum device, rapidly vacuumizing until the pressure is below 20Pa and keeping for 20s, then taking out a sample, and placing the sample under an external field voltage of 10V (5 cm for Ag metal, 5cm for FTO, and 4mm for two electrodes) for thermal stage annealing at 130 ℃ for 15 min; likewise, no external electric field is added, and the heating platform is annealed at 130 ℃ for 15min to respectively obtain perovskite thin films (400 nm);
evaporating a C60 electron transport layer (40 nm) on the surface of the prepared perovskite film;
then respectively transferring the obtained product into a thermal evaporation device, wherein the vacuum degree reaches 1 × 10 -5 Under the condition of Pa, an electrode (Au) is evaporated on the electron transport layer, and the thickness is 100 nm; then placing the battery in an oxygen glove box for 12 hours, and oxidizing to obtain a battery; these are referred to as example 4 and comparative example 4, respectively.
The cell prepared in example 4 of the present invention has four subcells, 4 subcells were tested in the following manner, denoted as example 4-1, example 4-2, example 4-3, example 4-4, and comparative example 4-1, comparative example 4-2, comparative example 4-3, and comparative example 4-4, respectively, and the test results are shown in table 4:
and (3) testing: the current density-voltage (JV) curves of the batteries prepared by the PCE test examples and comparative examples were measuredTesting is finished in a ketleley 2400 system; and (3) testing conditions are as follows: the simulated light intensity is 100mW cm -2 (AM 1.5G) Scan Rate of 0.1V s -1 (step size 0.02V, time delay 200 ms), scanning interval 1.2V to-0.2V, xenon lamp power output by NERL (national Renewable Energy laboratory) standard KG5 standard Si battery calibration.
Table 4 performance test results of the batteries
From the above embodiments, the present invention provides a method for preparing a perovskite thin film with the aid of an external electric field, comprising the following steps: forming a liquid film on the transparent electrode-hole transport layer substrate by adopting a liquid-phase film forming method for a precursor solution of the perovskite active layer; directly annealing the liquid film; or annealing after film forming by an anti-solvent method; or annealing after vacuum flash evaporation film forming to obtain a perovskite film; in the annealing process, an external electric field is applied to induce crystallization, and the voltage of the external electric field is more than 3V; the direction of the applied electric field is perpendicular to the film plane. According to the invention, the perovskite crystallization is assisted by the additional battery, so that the grain size of the perovskite material is increased, and the crystallinity is improved; the annealing temperature can be reduced compared to the annealing temperature without external electric field. The perovskite battery prepared by the perovskite thin film prepared by the method provided by the invention has the advantages that the photoelectric conversion effect is optimized, and the stability of the device is enhanced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A method for preparing a perovskite thin film with the assistance of an external electric field comprises the following steps:
forming a liquid film on the transparent electrode-hole transport layer substrate by adopting a liquid-phase film forming method for a precursor solution of the perovskite active layer;
directly annealing the liquid film; or annealing after film forming by an anti-solvent method; or annealing after vacuum flash evaporation film forming to obtain a perovskite film;
in the annealing process, an external electric field is applied to induce crystallization, and the voltage of the external electric field is more than 3V; the direction of the external electric field is vertical to the plane of the film;
the annealing temperature is 60-200 ℃.
2. The method of claim 1, wherein the time of the applied electric field is 5-60 min.
3. The method of claim 1, wherein the voltage of the applied electric field is quadrature dc adjustable.
4. The method of claim 1, wherein the applied electric field employs metal electrodes and oxide electrodes;
the metal electrode is connected with the positive electrode; the oxide electrode is connected with the negative electrode.
5. The method of claim 4, wherein the metal electrode is selected from Au, Ag, Cu, or Al;
the oxide electrode is selected from ITO, FTO and SnO 2 Or Al 2 O 3 。
6. The method according to claim 1, wherein the composition of the perovskite thin film is AMX 3 ；
A is an organic cation and/or an inorganic cation;
m is a divalent metal ion;
x is selected from I - 、Br - 、Cl - And/or F - 。
7. An optoelectronic device comprising the perovskite thin film produced by the production method according to any one of claims 1 to 6.
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| CN105256374A (en) * | 2015-11-05 | 2016-01-20 | 浙江大学城市学院 | Device and method for preparing organic perovskite thin film |
| CN107118110A (en) * | 2017-05-11 | 2017-09-01 | 陕西师范大学 | A kind of method that perovskite CH3NH3PbI3 films are prepared with transverse current |
| JP2019071496A (en) * | 2019-02-12 | 2019-05-09 | 株式会社東芝 | Photoelectric conversion element and manufacturing method thereof |
| CN110518130A (en) * | 2019-08-28 | 2019-11-29 | 上海交通大学 | A kind of method of electric field regulation perovskite crystal grain diauxic growth |
| JP2020107912A (en) * | 2020-04-06 | 2020-07-09 | 株式会社東芝 | Method for manufacturing photoelectric conversion film and method for manufacturing photoelectric conversion element |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105256374A (en) * | 2015-11-05 | 2016-01-20 | 浙江大学城市学院 | Device and method for preparing organic perovskite thin film |
| CN107118110A (en) * | 2017-05-11 | 2017-09-01 | 陕西师范大学 | A kind of method that perovskite CH3NH3PbI3 films are prepared with transverse current |
| JP2019071496A (en) * | 2019-02-12 | 2019-05-09 | 株式会社東芝 | Photoelectric conversion element and manufacturing method thereof |
| CN110518130A (en) * | 2019-08-28 | 2019-11-29 | 上海交通大学 | A kind of method of electric field regulation perovskite crystal grain diauxic growth |
| JP2020107912A (en) * | 2020-04-06 | 2020-07-09 | 株式会社東芝 | Method for manufacturing photoelectric conversion film and method for manufacturing photoelectric conversion element |
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Application publication date: 20220909 |