CN108682745B - Method for preparing perovskite film based on anti-solvent dynamic spin coating - Google Patents
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Abstract
In the method for preparing the perovskite thin film based on the anti-solvent dynamic spin coating, an organic solvent capable of dissolving lead iodide is selected, and the organic solvent does not dissolve the perovskite material, is mutually soluble with the lead iodide solvent and can dissolve CH3NH3Dissolution of I (MAI)The agent acts as an anti-solvent (e.g., isopropanol); and dropwise adding the isopropanol solution of the MAI in the process of spin-coating the DMF solution of the lead iodide, and controlling the dropwise adding amount and the dropwise adding time of the isopropanol solution of the MAI to control the crystallization condition of the perovskite thin film so as to finally obtain the high-quality perovskite thin film. The perovskite thin film grown on the rough mesoporous substrate by adopting the method has the advantages of smooth and compact surface, no pin hole, grain size of several microns, great reduction of the loss of current carriers at the crystal boundary and contribution to the application of perovskite materials in the photoelectric field.
Description
Technical Field
The invention relates to a preparation method of a perovskite thin film, in particular to a method for preparing the perovskite thin film based on anti-solvent dynamic spin coating.
Background
Organic-inorganic hybrid perovskite material (CH)3NH3PBX3X ═ Cl, Br, I) is a new photovoltaic semiconductor material with excellent photoelectric properties such as direct band gap, high light absorption coefficient, high carrier mobility and free path. Since 2009, the first application of organic-inorganic complex halide perovskite materials to the field of photovoltaics by japanese scientist Miyasaka, such new photovoltaic materials gradually come into the field of view of researchers and have recently received a high level of attention. Especially perovskite-based solar cells based on such materials, the conversion efficiency of which was refreshed to 23% again in 2018, have exceeded the monocrystalline silicon-based solar cells currently commercialized. Meanwhile, compared with the traditional silicon-based and gallium arsenide-based solar cells, the perovskite-based solar cell has the advantages of simpler preparation process and low material cost, and is praised as the solar cell with the highest development speed so far.
The crystallization and film forming quality of the perovskite light absorption layer have a crucial influence on the performance of the perovskite-based solar cell, and therefore, the perovskite thin film preparation methodThe exploration of the process is extremely important. At present, the preparation method of the perovskite material mainly comprises the following steps: a vapor phase method typified by double source co-evaporation, a liquid phase method typified by spin coating, and a solid phase method in which mixed powders react to form perovskite. Among them, the vapor phase method is not suitable for industrial mass production due to the restriction factors such as vacuum requirement, high temperature evaporation energy consumption and the like. The solid phase method is usually limited to powder preparation and is not suitable for film formation. The liquid phase method, especially the liquid phase method based on the spin coating process, is the most widely studied method at present due to the advantages of low cost, simple process, easy control and the like. The spin-coating method mainly comprises a one-step solution method and a step-by-step deposition method, wherein the one-step solution method is a common method for preparing perovskite, namely PbI2And CH3NH3I (MAI) is dispersed in N, N-dimethylformamide according to a certain proportion to prepare orange-yellow precursor solution, a spin coating method is utilized to prepare a film on a substrate, and excessive solvent is removed by annealing to crystallize perovskite. However, the crystallization process is difficult to control, and the obtained perovskite thin film has poor crystallization quality. Although the following research proposes that the film formation of perovskite is assisted by using an anti-solvent such as chlorobenzene or ether, the crystal quality of the perovskite thin film formed on the mesoporous substrate with larger roughness is not improved. In order to improve the crystallization quality of perovskite thin films formed on mesoporous substrates with relatively high roughness, the Gratzel topic group proposes a step-by-step deposition method, namely PbI2And CH3NH3And I, depositing the two precursors on the substrate in sequence, and reacting the two precursors on the substrate to form the perovskite thin film. The method can effectively control the crystallization process of the perovskite, so that the perovskite film layer and the mesoporous substrate have good compatibility, but the crystal grains of the prepared perovskite film are finely divided.
Disclosure of Invention
The invention aims to provide a method for preparing a perovskite thin film based on anti-solvent dynamic spin coating, aiming at the problem of fine grain of the perovskite thin film grown on a rough mesoporous substrate in the background technology. The perovskite thin film grown on the rough mesoporous substrate by adopting the method has a smooth and compact surface and no pinholes, the grain size can reach several microns, the loss of current carriers at the grain boundary is greatly reduced, and the method is favorable for the application of perovskite materials in the photoelectric field.
In the method for preparing the perovskite thin film based on the anti-solvent dynamic spin coating, an organic solvent (such as DMF) capable of dissolving lead iodide is selected, and the organic solvent does not dissolve the perovskite material, is mutually soluble with the lead iodide solvent and can dissolve CH3NH3Solvents of formula i (mai) as anti-solvents (e.g. isopropanol); the isopropyl alcohol solution of the MAI is dripped in the process of spin-coating the DMF solution of the lead iodide, and the crystallization condition of the perovskite film can be controlled by controlling the dripping amount and the dripping time of the isopropyl alcohol solution of the MAI, so that the perovskite film which is flat in large area, has no pinholes and has the grain size reaching the micron level is finally obtained.
The technical scheme adopted by the invention is as follows:
a method for preparing a perovskite thin film based on antisolvent dynamic spin coating specifically comprises the following steps:
step 2, preparing a lead iodide solution with the mass concentration of 0.3-0.6 g/mL by using lead iodide as a solute and an organic solvent as a solvent; with iodomethylamine (CH)3NH3I, MAI) is used as a solute, isopropanol is used as a solvent, and an isopropanol solution of iodomethylamine with the mass concentration of 30-70 mg/mL is prepared;
step 3, preheating the lead iodide solution prepared in the step 2 at 60-70 ℃ for 10-15 min;
step 4, forming a perovskite thin film on the substrate cleaned in the step 1 by adopting a spin coating method, wherein the spin coating speed is 3000rpm, and the time is 30 s; the specific process is as follows: firstly, dripping the lead iodide solution preheated in the step 3 on the substrate cleaned in the step 1, and starting spin coating; and (3) after spin coating for 5-25 s, dropwise adding the isopropanol solution of iodomethylamine prepared in the step (2), and continuing spin coating, wherein the volume ratio of the lead iodide solution to the isopropanol solution of iodomethylamine is (0.6-1.6): 1; and in the process of continuing spin coating, reacting isopropanol solution of iodomethylamine with lead iodide to generate perovskite, and removing residual solution and excessive MAI on the surface layer by baking treatment to obtain the perovskite thin film.
Further, the substrate in the step 1 is conductive glass with an electron transport layer.
Further, the process of cleaning the substrate in step 1 specifically includes: a. ultrasonically cleaning the conductive glass with the electron transport layer in acetone, alcohol and water in sequence, and drying; b. and carrying out ultraviolet-ozone treatment on the conductive glass with the electron transport layer after the previous step of treatment so as to increase the hydrophilicity of the substrate.
Further, the organic solvent in step 2 is DMF (N, N-dimethylformamide), DMSO (dimethyl sulfoxide), or a mixed solvent of DMF and DMSO.
Further, steps 2 to 4 were performed in a glove box under a nitrogen atmosphere.
Further, in step 4, when the perovskite thin film was formed on the substrate cleaned in step 1 by the spin coating method, the acceleration was 1000 rpm/s.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a method for preparing a perovskite film based on antisolvent dynamic spin coating, which comprises the following steps of firstly, preparing a lead iodide solution and an isopropanol solution of iodomethylamine; and then, dropwise adding an isopropanol solution of the MAI in the process of spin-coating the lead iodide solution, and controlling the dropwise adding amount and the dropwise adding time of the isopropanol solution of the MAI to control the crystallization condition of the perovskite thin film so as to finally obtain the large-area smooth perovskite thin film without pinholes.
2. The method provided by the invention obtains the high-quality perovskite thin film on the rough and uneven mesoporous substrate, the surface of the prepared perovskite thin film is flat and compact, no pinholes exist, the grain size can reach several micrometers, the loss of current carriers at the grain boundary is greatly reduced, and the method is favorable for the application of perovskite materials in the photoelectric field.
Drawings
FIG. 1 is an SEM image of perovskite thin films obtained in comparative example 1(a), comparative example 2(b) and example 1 (c);
FIG. 2 is SEM images of pure lead iodide thin films and perovskite thin films obtained by dropwise adding an isopropanol solution of iodomethylamine after spin-coating a lead iodide solution for 0s, 5s, 10s, 15s, 20s, 25s and 30 s;
FIG. 3 is an X-ray diffraction pattern of the perovskite thin films obtained in comparative example 1, comparative example 2 and example 1.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
A method for preparing a perovskite thin film based on antisolvent dynamic spin coating specifically comprises the following steps:
1.1, sequentially ultrasonically cleaning the FTO conductive glass with the electron transport layer in acetone, alcohol and water for 20min, and drying in a vacuum drying oven;
1.2, carrying out ultraviolet-ozone treatment on the FTO conductive glass with the electron transport layer after the previous step of treatment so as to increase the hydrophilicity of the substrate;
step 2, stirring and dissolving lead iodide serving as a solute and an organic solvent serving as a solvent to prepare a lead iodide solution with the mass concentration of 0.3-0.6 g/mL; with iodomethylamine (CH)3NH3I, MAI) is used as a solute, isopropanol is used as a solvent, and the mixture is stirred and dissolved to prepare an isopropanol solution of iodomethylamine with the mass concentration of 30-70 mg/mL;
step 3, placing the lead iodide solution prepared in the step 2 on a heating and stirring table, and carrying out preheating treatment for 10-15 min at the temperature of 60-70 ℃;
step 4, forming a perovskite thin film on the substrate cleaned in the step 1 by adopting a spin coating method, wherein the spin coating speed is 3000rpm, and the time is 30 s; the specific process is as follows: firstly, dripping the lead iodide solution preheated in the step 3 on the substrate cleaned in the step 1, and starting spin coating; and (3) after spin coating for 5-25 s, dropwise adding the isopropanol solution of iodomethylamine prepared in the step (2), and continuing spin coating, wherein the volume ratio of the lead iodide solution to the isopropanol solution of iodomethylamine is (0.6-1.6): 1; and in the process of continuing spin coating, reacting an isopropanol solution of iodomethylamine with lead iodide to generate perovskite, baking at 150 ℃ for 10-60 min, and removing residual solution and excessive MAI on the surface layer to obtain the perovskite thin film.
Further, steps 2 to 4 were performed in a glove box under a nitrogen atmosphere.
Further, in step 4, when the perovskite thin film was formed on the substrate cleaned in step 1 by the spin coating method, the acceleration was 1000 rpm/s.
Example 1
A method for preparing a perovskite thin film based on antisolvent dynamic spin coating specifically comprises the following steps:
1.1 will bring TiO to2Sequentially ultrasonically cleaning FTO conductive glass of the electron transport layer in acetone, alcohol and water for 20min, and drying in a vacuum drying oven;
1.2 pairs of the treated TiO tapes2Performing ultraviolet-ozone treatment on the FTO conductive glass of the electron transport layer for 20min to increase the hydrophilicity of the substrate;
step 2, stirring for 12 hours by taking lead iodide as a solute and DMF as a solvent to prepare a lead iodide solution with the mass concentration of 0.416 g/mL; with iodomethylamine (CH)3NH3I, MAI) as a solute and isopropanol as a solvent, stirring for 12h, and preparing an isopropanol solution of iodomethylamine with the mass concentration of 50 mg/mL;
step 3, placing the lead iodide solution prepared in the step 2 on a heating and stirring table, and carrying out preheating treatment for 15min at 70 ℃;
step 4, forming a perovskite thin film on the substrate cleaned in the step 1 by adopting a spin coating method, wherein the spin coating speed is 3000rpm, the time is 30s, and the acceleration is 1000 rpm/s; the specific process is as follows: firstly, uniformly dripping 50 microliters of lead iodide solution preheated in the step 3 on the substrate cleaned in the step 1, and starting spin coating; after 10s of spin coating, 50 microliters of isopropanol solution of iodomethylamine prepared in the step 2 is dripped, and the spin coating is continued for 20 s; in the process of continuing spin coating, the isopropanol solution of iodomethylamine reacts with lead iodide to generate perovskite, and the perovskite film is baked for 10min at 150 ℃ to obtain the perovskite film.
Example 2
The perovskite thin film was prepared according to the procedure of example 1, and the time for dropping the isopropyl alcohol solution of MAI was set as: after spin coating for 0s, 5s, 15s, 20s, 25s, and 30s, an isopropyl alcohol solution of iodomethylamine is added dropwise. The SEM of the perovskite thin film obtained in example 2 is shown in fig. 2.
Comparative example 1
Comparative example 1 perovskite thin films were prepared by a conventional one-step process. The specific process is as follows:
(1) cleaning a substrate:
1.1 will bring TiO to2Sequentially ultrasonically cleaning FTO conductive glass of the electron transport layer in acetone, alcohol and water for 20min, and drying in a vacuum drying oven;
1.2 pairs of the treated TiO tapes2Performing ultraviolet-ozone treatment on the FTO conductive glass of the electron transport layer for 20min to increase the hydrophilicity of the substrate;
(2) preparing a perovskite precursor solution:
adding 0.2g of MAI and 0.578g of lead iodide into 1mL of DMF, and stirring at 60 ℃ for 12h until the solution is clear and transparent to obtain a perovskite precursor solution;
(3) preparing a perovskite thin film:
and (3) dropwise adding 50 microliters of the perovskite precursor solution obtained in the step (2) onto the substrate cleaned in the step (1), spin-coating for 30s at the rotating speed of 3000rpm, and then baking for 20min at 100 ℃ to obtain the perovskite thin film.
Comparative example 2
Comparative example 2 perovskite thin films were prepared by a conventional two-step spin coating method. Comparative example 2 compared to example 1, the difference is: when the perovskite thin film is formed on the substrate cleaned in the step 1 by adopting a spin coating method in the step 4, the specific process is as follows: firstly, dripping 50 microliters of the lead iodide solution preheated in the step 3 on a cleaned substrate, spin-coating the substrate at the rotating speed of 3000rpm for 30 seconds, and baking the substrate at 100 ℃ for 5 min; and then after the substrate treated in the previous step is cooled to room temperature, 50 microliters of isopropanol solution of iodomethylamine prepared in the step 2 is dripped on the surface of the substrate, spin-coated for 30s at the rotating speed of 3000rpm, and then baked for 20min at the temperature of 150 ℃ to obtain the perovskite thin film.
As shown in fig. 1, SEM images of the perovskite thin films obtained in comparative example 1(a), comparative example 2(b) and example 1 (c); as can be seen from FIG. 1, the perovskite thin film obtained in example 1 has a flat and dense surface, no pinholes, and a grain size of 1.86 μm.
As shown in fig. 2, SEM images of pure lead iodide thin films and perovskite thin films obtained by adding an isopropyl alcohol solution of iodomethylamine dropwise after spin-coating a lead iodide solution for 0s, 5s, 10s, 15s, 20s, 25s, and 30s, reflect the influence of the timing of adding an isopropyl alcohol solution of MAI on the resulting perovskite thin films. As can be seen from fig. 2, the obtained perovskite thin film has a large surface morphology difference by dropping the isopropyl alcohol solution of MAI at different timings, and basically shows a variation trend of a multi-pinhole film, a flat film and a fine-grained crystal film, and the morphology of the thin film obtained by dropping the isopropyl alcohol solution of MAI after spin-coating for 10 seconds is optimal.
As shown in fig. 3, X-ray diffraction patterns of the perovskite thin films obtained in comparative example 1, comparative example 2 and example 1 were shown. As can be seen from fig. 3, the perovskite thin film obtained in example 1 has a pure phase perovskite structure, and has no impurities such as lead iodide, and the like, and compared with the thin films obtained in comparative examples 1 and 2, the perovskite thin film has the strongest diffraction peak, the smallest half-height width, and the best crystal quality.
The method for preparing the perovskite thin film based on the anti-solvent dynamic spin coating effectively solves the problems that the thin film obtained by the traditional one-step spin coating method has multiple pinholes and the thin film obtained by the traditional two-step spin coating method has small crystal grains, and the high-quality perovskite thin film is finally obtained on a rough and uneven mesoporous substrate by quickly extracting lead iodide through the anti-solvent (isopropanol) and reacting the lead iodide with MAI dissolved in the anti-solvent to generate perovskite crystals.
Claims (4)
1. A method for preparing a perovskite thin film based on antisolvent dynamic spin coating comprises the following steps:
step 1, cleaning a substrate;
step 2, preparing a lead iodide solution with the mass concentration of 0.3-0.6 g/mL by using lead iodide as a solute and an organic solvent as a solvent, wherein the organic solvent is DMF, DMSO or a mixed solvent of DMF and DMSO; preparing an isopropanol solution of iodomethylamine with the mass concentration of 30-70 mg/mL by taking iodomethylamine as a solute and isopropanol as a solvent;
step 3, preheating the lead iodide solution prepared in the step 2 at 60-70 ℃ for 10-15 min;
step 4, forming the perovskite thin film on the substrate cleaned in the step 1 by adopting a spin coating method, wherein the spin coating speed is 3000rpm and the time is 30s, dropwise adding an isopropanol solution of iodomethylamine in the process of spin coating a lead iodide solution, and controlling the crystallization condition of the perovskite thin film by controlling the dropwise adding amount and the dropwise adding time of the isopropanol solution of iodomethylamine; the specific process is as follows:
firstly, dripping the lead iodide solution preheated in the step 3 on the substrate cleaned in the step 1, and starting spin coating; and (3) dropwise adding the isopropanol solution of the iodomethylamine prepared in the step (2) after spin-coating for 10-15 s, and continuing spin-coating, wherein the volume ratio of the lead iodide solution to the isopropanol solution of the iodomethylamine is (0.6-1.6): 1; and in the process of continuing spin coating, reacting an isopropanol solution of iodomethylamine with lead iodide to generate perovskite, baking at 150 ℃ for 10-60 min after the spin coating is finished, removing residual solution and excessive iodomethylamine on the surface layer, and obtaining the perovskite thin film with the grain size of micron order.
2. The method for preparing the perovskite thin film based on the anti-solvent dynamic spin coating as claimed in claim 1, wherein the substrate in the step 1 is conductive glass with an electron transport layer.
3. The method for preparing perovskite thin film based on anti-solvent dynamic spin coating according to claim 1, wherein the steps 2 to 4 are performed in a glove box under nitrogen atmosphere.
4. The method for preparing the perovskite thin film based on the anti-solvent dynamic spin coating as claimed in claim 1, wherein the acceleration in step 4 is 1000rpm/s when the perovskite thin film is formed on the substrate cleaned in step 1 by the spin coating method.
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| CN109638162B (en) * | 2018-12-14 | 2022-07-05 | 江西理工大学 | High-quality CsPbI2Preparation method of Br inorganic perovskite film |
| CN109768166A (en) * | 2019-01-16 | 2019-05-17 | 深圳市前海首尔科技有限公司 | A kind of perovskite solar battery and preparation method thereof |
| CN109950397A (en) * | 2019-01-16 | 2019-06-28 | 深圳市前海首尔科技有限公司 | A kind of preparation process of high performance calcium titanium ore solar battery thin film |
| CN109904319B (en) * | 2019-01-29 | 2022-11-18 | 安徽大学 | Preparation method of large-size perovskite flat crystal and perovskite layer and solar cell |
| US11282700B2 (en) | 2019-04-17 | 2022-03-22 | University Of Kentucky Research Foundation | Method for manufacturing perovskite-based devices in ambient air |
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