CN115020598A - Promote inorganic CsPbI 3 Method for stabilizing perovskite film environment - Google Patents

Promote inorganic CsPbI 3 Method for stabilizing perovskite film environment Download PDF

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CN115020598A
CN115020598A CN202210670084.4A CN202210670084A CN115020598A CN 115020598 A CN115020598 A CN 115020598A CN 202210670084 A CN202210670084 A CN 202210670084A CN 115020598 A CN115020598 A CN 115020598A
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perovskite
cspbi
film
inorganic
thin film
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李蔚
江炀
杜红强
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Wuhan University of Technology WUT
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    • 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
    • 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
    • H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. 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
    • 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
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

The invention relates to a method for improving inorganic CsPbI 3 The method for stabilizing the perovskite film environment comprises the following specific steps: 1) will prepare CsPbI 3 Dissolving a powder raw material of perovskite in N, N-dimethylformamide to prepare a perovskite precursor solution; 2) dissolving methylamine iodine powder in isopropanol to prepare MAI solution; 3) will be coated with TiO 2 Carrying out ultraviolet ozone treatment on FTO conductive glass of the electron transport layer, coating a perovskite precursor solution on the surface of the FTO conductive glass, then carrying out primary annealing treatment, and cooling to obtain a perovskite thin film; 4) spin-coating MAI solution on the perovskite film by using a spin-coating method, and then carrying out secondary annealing treatment to obtain CsPbI with good stability 3 A perovskite solid film. The method provided by the invention enables the MAI to be aligned with the inorganic CsPbI 3 The crystal boundary and other defects of the perovskite film are subjected to surface passivation, so that the inorganic CsPbI is improved 3 Environmental stability of perovskite thin films.

Description

Promote inorganic CsPbI 3 Method for stabilizing perovskite film environment
Technical Field
The invention belongs to the technical field of selection of semiconductor device materials, and particularly relates to a method for improving inorganic CsPbI 3 Method for stabilizing perovskite film environment。
Background
Perovskite materials are more and more favored in the photovoltaic field due to the characteristics of long carrier diffusion length, accurate and adjustable band gap, high light absorption coefficient, high defect tolerance and the like. Methylamine lead iodide (MAPbI) synthesized since 2009 japan Kojima et al (j.am. chem. soc., 2009, 131, 6050- 3 ) After the perovskite solar cell is applied to a solar cell for the first time and the power conversion efficiency of 3.8% is obtained, the research of the perovskite solar cell is well-blown in 13 years, and the authentication efficiency of 25.5% is obtained at present (Nature, 2021, 598, 444-450). However, the commercial application of perovskite is limited in the conventional organic-inorganic hybrid perovskite solar cell due to the instability of organic cation. In view of this, all-inorganic perovskites are of great interest because of the excellent thermal stability exhibited at high temperatures (330 ℃).
Wherein CsPbI in the all-inorganic perovskite 3 The system has received attention from researchers because the optical bandgap of-1.70 eV is a suitable bandgap for use as a top cell in perovskite-silicon tandem solar cells (Science, 2020, 370, 1300-. However, CsPbI 3 Perovskite materials also have drawbacks due to the optically active black CsPbI 3 The phase formation energy is higher than that of non-optically active yellow CsPbI 3 The phase promotes the black phase perovskite film to be easily changed into yellow phase in the environment, and further the inorganic CsPbI 3 The industrial application of perovskites poses certain obstacles. Aiming at the problem, the invention provides a method for improving inorganic CsPbI 3 The method for stabilizing the perovskite thin film environment has important significance for the development of perovskite solar cells.
Disclosure of Invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a method for enhancing the CsPbI 3 A method for environmental stability of perovskite thin film.
In order to realize the aim of the invention, the specific technical scheme is as follows:
promote inorganic CsPbI 3 Thin perovskiteThe method for stabilizing the membrane environment comprises the following specific steps:
1) will prepare CsPbI 3 Dissolving a powder raw material of perovskite in N, N-dimethylformamide to prepare a perovskite precursor solution;
2) dissolving methylamine iodide (MAI) powder in Isopropanol (IPA) to prepare MAI solution;
3) will be coated with TiO 2 Carrying out ultraviolet ozone treatment on FTO conductive glass of the electron transport layer, coating the perovskite precursor solution obtained in the step 1) on the surface of the FTO conductive glass, then carrying out first annealing treatment, and cooling to obtain a perovskite thin film;
4) spin-coating the MAI solution obtained in the step 2) on the perovskite film obtained in the step 3) by using a spin-coating method, and then carrying out secondary annealing treatment to obtain CsPbI with good stability 3 Perovskite solid film.
According to the scheme, the CsPbI is prepared in the step 1) 3 The perovskite powder raw materials are cesium iodide (CsI) and lead iodide (PbI) 2 ) Dimethylamine hydroiodide (DMAI). Preferably, the molar ratio of cesium iodide, lead iodide and dimethylamine hydroiodide is 1: 1: 1.
according to the scheme, the molar volume ratio of the cesium iodide in the step 1) to the N, N-dimethylformamide is 0.6-0.7 mmol/mL.
According to the scheme, the molar concentration of the MAI solution in the step 2) is 5-15 mM (mmol/L).
According to the scheme, the process conditions for coating the perovskite precursor solution on the surface of the FTO conductive glass in the step 3) are as follows: spin-coating at 3000rpm/min for 30-40 s.
According to the scheme, the process conditions of the first annealing treatment in the step 3) are as follows: annealing at 210 deg.C for 5 min. The first annealing treatment enables the perovskite precursor solution to form a solid film.
According to the scheme, the coating amount of the MAI solution in the step 4) on the surface of the perovskite film is 14-18 mu L/cm 2 。
According to the scheme, the process conditions for spin-coating the MAI solution on the perovskite thin film in the step 4) are as follows: spin-coating at 3500rpm/min for 30-40 s.
According to the scheme, the process conditions of the second annealing treatment in the step 4) are as follows: annealing at 120 deg.C for 10 min. The purpose of the second anneal is to remove residual solvent.
The second purpose of the present invention is to provide an inorganic CsPbI with good stability prepared by the above method 3 A perovskite thin film.
The specific technical scheme is as follows:
the inorganic CsPbI with good stability prepared by the method 3 Perovskite thin film, the inorganic CsPbI 3 The perovskite film can be stably stored for more than 1h under the conditions of room temperature (15-35 ℃) and relative humidity of 60-70%.
It is another object of the present invention to provide the above inorganic CsPbI 3 Application of perovskite thin film.
The specific technical scheme is as follows:
the inorganic CsPbI 3 Use of a perovskite thin film in a perovskite/silicon based tandem solar cell.
The principle of the invention is as follows: the invention is characterized in that a layer of MAI solution is spin-coated on the perovskite solid film, and the inorganic CsPbI is subjected to MAI 3 The surface passivation is carried out on defects such as the grain boundary of the perovskite thin film, and when MAI is accumulated at the grain boundary of inorganic perovskite, stress is applied to inhibit CsPbI 3 The black phase is converted into the yellow phase, so that the stability of the film is improved. Experimental results show that when the concentration of the MAI solution is 5-15 mM, the obtained perovskite crystal grains are large in size, the particle size distribution of the thin film is uniform, and the stability of the thin film is improved.
The invention has the beneficial effects that: 1. the method provided by the invention enables the MAI to be aligned with the inorganic CsPbI 3 The crystal boundary and other defects of the perovskite film are subjected to surface passivation, so that the inorganic CsPbI is improved 3 Environmental stability of the perovskite thin film; 2. the inorganic CsPbI provided by the invention 3 The perovskite thin film has the excellent characteristics of uniform grain size, good crystallinity, strong stability and the like.
Drawings
FIG. 1 shows four inorganic CsPbI solutions with different concentrations prepared in example 1 of the present invention 3 Scanning electron of perovskite thin filmMicroscopic and particle size statistical plots;
FIG. 2 shows four inorganic CsPbI solutions prepared in example 1 by treatment with different concentrations of MAI solutions 3 An X-ray diffraction pattern of the perovskite thin film;
FIG. 3 shows four inorganic CsPbI solutions prepared in example 1 by treatment with different concentrations of MAI solutions 3 Atomic force microscopy of perovskite thin films;
FIG. 4 is the inorganic CsPbI prepared in example 1 by treatment with MAI solutions at concentrations of 0mM and 15mM 3 The perovskite thin film is placed in an environment and changes with time in an ultraviolet-visible light spectrum diagram.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
The raw materials used in the embodiment of the invention are weighed in the glove box, and the stirring process adopts vibration stirring in the glove box.
Example 1
Promote inorganic CsPbI 3 A method for environmental stabilization of perovskite thin films, comprising the steps of:
1) respectively cleaning an FTO conductive glass substrate (2.5cm multiplied by 2.5cm) by using a cleaning agent, ultrapure water and alcohol, carrying out ultraviolet ozone treatment on the cleaned FTO conductive glass substrate for 15 minutes, then spin-coating a bis (acetylacetone) diisopropyl titanate solution (a commercially available raw material) with the concentration of 0.2M on the FTO conductive glass by a spin-coating method, carrying out spin-coating for 30s at the speed of 4000rpm/s, annealing at 100 ℃ for 10min, and preparing TiO on the surface of the FTO conductive glass 2 An electron transport layer;
2) respectively weighing 0.6 mmol of cesium iodide, lead iodide and dimethylamine hydroiodide, and dissolving in 1 ml of N, N-dimethylformamide to obtain a perovskite precursor solution;
3) dissolving MAI powder medicines with different dosages in 1 ml of isopropanol to prepare MAI solutions (0mM, 5mM, 15mM and 30mM) with different molar concentrations;
4) coating the surface obtained in the step 1) with TiO 2 Ultraviolet treatment of FTO conductive glass of electron transport layerOzone treatment is carried out for 15 minutes, then 50 microliter of perovskite precursor solution prepared in the step 2) is spin-coated on FTO conductive glass by utilizing a spin-coating method, spin-coating is carried out for 30 seconds at the rotating speed of 3000rpm/min, then annealing is carried out at 210 ℃ for 5min, and then natural cooling is carried out to room temperature;
5) spin-coating 100 microliters of the MAI solution prepared in the step 3) on the perovskite thin film obtained in the step 4) within 3 seconds of the beginning of spin-coating by using a spin-coating method, spin-coating for 35 seconds at the rotating speed of 3500rpm/min, then annealing at 120 ℃ for 10min, and naturally cooling to room temperature to obtain the inorganic CsPbI 3 Perovskite thin film (the sample with MAI solution concentration of 0mM is marked as Control sample).
FIG. 1 shows four inorganic CsPbI solutions prepared in this example by treatment with different concentrations of MAI solutions 3 Scanning electron microscopy images and particle size statistics of the perovskite thin films. In comparison, the Control-like perovskite thin film without MAI solution surface treatment has poor compactness and pores, and the average particle size is 586 nm. The uniformity of perovskite crystals subjected to surface treatment by the MAI solution with a proper concentration is gradually improved, the average grain size of the crystals is increased (the average grain size of a film after surface treatment by the MAI solution with concentrations of 5mM and 15mM is 612nm and 627nm respectively), pores in the film gradually disappear, the appearance of the film is obviously improved, but when the concentration of the MAI solution is further increased to 30mM, the grain size of the film is obviously reduced, the average grain size is 571nm, and a large amount of unreacted white substances (MAI) are accumulated on the surface of the film. The result shows that the appearance of the all-inorganic perovskite thin film can be influenced to a certain extent by regulating the concentration of the MAI solution, and the preferred concentration range of the MAI solution is 5-15 mM.
FIG. 2 shows four inorganic CsPbI solutions with different concentrations prepared in this example 3 X-ray diffraction pattern of perovskite thin film. Compared with a Control-like perovskite thin film which is not treated by the MAI solution, the thin film which is treated by the MAI solution with the concentration of 5mM has the highest diffraction peak intensity and the best preferred orientation. However, further increasing the concentration of the MAI solution causes a significant decrease in the intensity of the diffraction peak and a gradual deterioration in crystallinity.
FIG. 3 shows four inorganic CsPbI solutions with different concentrations prepared in this example 3 Atomic force of perovskite thin filmA micromirror diagram. In contrast, the roughness of the film surface increased with increasing MAI solution, with the lowest roughness for films treated with MAI solutions at concentrations of 5mM and 15mM, consistent with the results from the SEM image of FIG. 1.
FIG. 4 shows the inorganic CsPbI prepared in this example by treatment with MAI solutions at concentrations of 0mM and 15mM 3 And (3) a UV-Vis stability change map of the perovskite thin film. And (3) placing the film sample at room temperature and relative humidity of 60-70% for a certain time, and testing the stability of the sample by using UV-Vis. In the figure, the comparison shows that the UV-Vis absorption intensity of the Control-like film is obviously reduced within 1h, and the absorption peak (730 nm) of the black perovskite phase cannot be detected in the 60 th-min film, which indicates that the Control-like film is rapidly degraded from the black photoactive perovskite phase to the yellow non-photoactive perovskite phase within 1 h; and the thin film treated by the MAI solution is placed in the environment for 1h, and the absorption peak (730 nm) of the black perovskite phase can be detected, so that the thin film can exist in the form of the black phase of the optically active perovskite. This shows that the stability of the film after treatment with the MAI solution is significantly better than that of the untreated Control-like film.
Various corresponding changes and modifications can be made by those skilled in the art based on the above technical solutions and concepts, and all such changes and modifications should be included in the protection scope of the present invention.

Claims (10)

1. Promote inorganic CsPbI 3 The method for stabilizing the perovskite thin film environment is characterized by comprising the following specific steps:
1) will prepare CsPbI 3 Dissolving a powder raw material of perovskite in N, N-dimethylformamide to prepare a perovskite precursor solution;
2) dissolving methylamine iodine powder in isopropanol to prepare MAI solution;
3) will be coated with TiO 2 Carrying out ultraviolet ozone treatment on FTO conductive glass of the electron transport layer, coating the perovskite precursor solution obtained in the step 1) on the surface of the FTO conductive glass, carrying out first annealing treatment, and cooling to obtain perovskiteA film;
4) spin-coating the MAI solution obtained in the step 2) on the perovskite thin film obtained in the step 3) by using a spin-coating method, and then carrying out secondary annealing treatment to obtain CsPbI with good stability 3 Perovskite solid film.
2. The boosted inorganic CsPbI of claim 1 3 The method for preparing the CsPbI film with environmental stability is characterized in that the CsPbI film is prepared in the step 1) 3 The perovskite powder is prepared from cesium iodide, lead iodide and dimethylamine hydroiodide.
3. The boosted inorganic CsPbI of claim 1 3 The method for stabilizing the perovskite thin film environment is characterized in that the molar volume ratio of cesium iodide to N, N-dimethylformamide in the step 1) is 0.6-0.7 mmol/mL.
4. The boosted inorganic CsPbI of claim 1 3 The method for stabilizing the perovskite thin film environment is characterized in that the molar concentration of the MAI solution in the step 2) is 5-15 mM.
5. The boosted inorganic CsPbI of claim 1 3 The method for stabilizing the perovskite film environment is characterized in that the process conditions of coating the perovskite precursor solution on the surface of the FTO conductive glass in the step 3) are as follows: spin-coating at a rotating speed of 3000rpm/min for 30-40 s; the process conditions of the first annealing treatment in the step 3) are as follows: annealing at 210 deg.C for 5 min.
6. The boosted inorganic CsPbI of claim 1 3 The method for stabilizing the perovskite film environment is characterized in that the MAI solution in the step 4) is coated on the surface of the perovskite film in an amount of 14-18 mu L/cm 2 。
7. The boosted inorganic CsPbI of claim 1 3 The method for stabilizing the perovskite thin film environment is characterized in that the process conditions of spin coating of the MAI solution on the perovskite thin film in the step 4) are as follows: at 350Spin coating at 0rpm/min for 30-40 s.
8. The boosted inorganic CsPbI of claim 1 3 The method for stabilizing the perovskite thin film environment is characterized in that the process conditions of the second annealing treatment in the step 4) are as follows: annealing at 120 deg.C for 10 min.
9. An inorganic CsPbI with good stability prepared according to the method of any one of claims 1 to 8 3 Perovskite thin film, characterized in that the inorganic CsPbI 3 The perovskite film can be stably stored for more than 1h under the conditions of room temperature and relative humidity of 60-70%.
10. The inorganic CsPbI of claim 9, wherein the inorganic CsPbI is selected from the group consisting of 3 Use of a perovskite thin film in a perovskite/silicon based tandem solar cell.
CN202210670084.4A 2022-06-14 2022-06-14 Promote inorganic CsPbI 3 Method for stabilizing perovskite film environment Pending CN115020598A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115536058A (en) * 2022-09-19 2022-12-30 上海钙晶科技有限公司 Method for reducing band gap of perovskite thin film by introducing iodine three anions through secondary annealing

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115536058A (en) * 2022-09-19 2022-12-30 上海钙晶科技有限公司 Method for reducing band gap of perovskite thin film by introducing iodine three anions through secondary annealing
CN115536058B (en) * 2022-09-19 2023-12-05 上海钙晶科技有限公司 Method for reducing perovskite film band gap by introducing iodine triple anions through secondary annealing

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