CN111710783B - Device and method for preparing large-area perovskite thin film - Google Patents
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Abstract
The invention relates to the technical field of solar cells, in particular to a device and a method for preparing a large-area perovskite thin film. The device comprises a vacuum cavity and a rapid vacuumizing pump set, wherein a metal plane electrode with a small hole is arranged in the vacuum cavity, an infrared quartz heating pipe is arranged behind the metal electrode, and infrared radiation can achieve the effect of uniform infrared light through the small hole. And a metal net used for reducing the plasma bombardment effect is arranged between the plane electrode and the substrate. The vacuum chamber is also provided with a micro control valve for supplementing inert gas. After the perovskite wet film which is subjected to spin coating or coating enters the cavity, the pressure of the cavity is rapidly reduced to about 5Pa, most of solvent in the wet film is volatilized, at the moment, the micro valve is opened to supplement inert gas, the pressure of the cavity is maintained stable, the radio frequency power supply is started to form plasma, crystallization of the film is promoted, then the cavity is deflated, and infrared radiation is started for 1-5 minutes to further promote generation of perovskite.
Description
Technical Field
The invention relates to the technical field of solar cells, in particular to a device and a method for preparing a large-area perovskite thin film.
Background
The small area efficiency of perovskite solar cells has exceeded 25%, but in almost all published literature antisolvent spin coating or two-step spin coating methods are used. In particular, the anti-solvent method requires the addition of an anti-solvent during the spin coating process to promote the formation of the perovskite thin film, and this process cannot be scaled up to a size of 5 × 5cm or more. The commercialization of perovskite solar cells requires the preparation of large-area perovskite thin films, and thus new technologies for preparing high-quality large-area perovskite thin films are required. The reduced pressure distillation method uses vacuum to remove the solvent in the perovskite wet film, uses supersaturation to promote the generation of perovskite crystal nucleus, and anneals to form the perovskite thin film, and is a possible large-area preparation method, such as CN 105239054A. However, the simple vacuum distillation method only uses supersaturation to promote nucleation of the wet film. The driving force is obviously not superior to that of the anti-solvent method, so the efficiency is lower than that of the perovskite thin film prepared by the anti-solvent method. Patent CN 209619436U combines the anti-solvent method and the reduced pressure distillation method, which has a good effect, however, the non-uniformity of the anti-solvent vapor volatilization inevitably causes the problem of non-uniformity of the film. Therefore, there is a need to develop a physical method to further promote perovskite wet film nucleation and crystallization.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the device and the method for preparing the large-area perovskite thin film are provided, and the large-scale production of the perovskite solar cell is realized.
The utility model provides a device of preparation large tracts of land perovskite film, pump package (2) including a vacuum chamber (1) and corresponding quick evacuation, pump package (2) of quick evacuation are connected to in the middle of the top of vacuum chamber (1), upper portion is equipped with metal plane electrode (3) with aperture in vacuum chamber (1), radio frequency power supply (4) (13.56 MHZ) are connected through the wire in metal electrode (3), parallel arrangement infrared quartz heating pipe (5) behind electrode (3), infrared quartz heating pipe (5) are connected to power supply through isolator (6), still have in the middle of plane electrode (3) and base (7) to be used for reducing metal mesh (8) of plasma bombardment effect. The vacuum chamber (1) is also provided with a micro-control valve (9) which can be used for supplementing inert gas and controlling the pressure to be constant.
Furthermore, the rapid vacuum pump is a cascade pump or a plurality of groups of pumps are connected in parallel, so as to achieve the purpose of rapidly reducing the pressure.
Furthermore, the metal plane electrode is provided with small holes, the diameter of the small hole which is right opposite to the quartz heating pipes is 4-5mm, the diameter of the small hole between the quartz heating pipes is 8-10mm, and the distance between the small holes is 4-5mm, so that infrared radiation can be uniformly irradiated on a sample through the small holes.
Furthermore, the quartz heating tube is provided with a disconnecting switch which is closed when the radio frequency runs so as to prevent the radio frequency or the microwave from overflowing through the quartz heating tube.
Further, the metal plane electrode is connected with a radio frequency power supply (13.56 MHZ).
Furthermore, the diameter of the metal wire of the metal grid is 0.1mm, and the metal grid is 1cm square. The metal mesh is grounded or a power supply capable of providing bias voltage is added.
Furthermore, the vacuum cavity is also provided with a micro gas valve which can be filled with inert gas for maintaining the pressure constant.
An apparatus and a method for preparing a large-area perovskite solar cell have the following processes:
(1) And placing the perovskite wet film into a vacuum cavity. The thickness of the wet film is about 2um, and the preparation method is coating or spin coating;
(2) And starting a vacuum pump, quickly reducing the vacuum of the system, starting a micro control valve when the vacuum of the system reaches 50-60Pa, supplementing air to the system, continuously exhausting air, and stabilizing the vacuum of the system to about 5-10Pa. At this time, most of the solvent in the perovskite wet film is volatilized, and the supersaturation degree pushes the interior of the perovskite wet film to form perovskite crystal nuclei.
(3) And closing an isolating switch of the quartz tube, completely isolating the power supply of the quartz heating tube from the internal connection of the vacuum cavity, and starting the radio frequency power supply to form plasma. Maintaining for 10-20s, and further promoting the nucleation of the perovskite thin film and realizing the growth of crystal nucleus due to the action of the plasma.
(4) And (3) turning off the radio frequency power supply, turning on an isolating switch of the quartz heating pipe, discharging the gas from the vacuum cavity to the atmospheric pressure, simultaneously turning on the infrared quartz heating pipe for heating, and maintaining for 1-5 minutes to form the perovskite thin film.
(5) And closing the infrared radiation, and moving the perovskite film out of the cavity.
Has the advantages that:
after the perovskite wet film which is subjected to spin coating or coating enters the cavity, the pressure of the cavity is rapidly reduced, most of solvent in the wet film volatilizes, then the micro valve is opened to supplement inert gas, the pressure of the cavity is maintained stable, the radio frequency power supply is started to form plasma, crystallization of the film is promoted, the metal grid is grounded or biased to play a role in preventing particle bombardment, then the cavity is deflated, and then infrared radiation is started for 1-5 minutes to promote generation of perovskite. The infrared radiation can achieve the effect of uniform infrared light through the small holes, and the uniform infrared radiation field is helpful for forming a uniform perovskite film.
Drawings
FIG. 1 is a schematic structural diagram of the device of the present invention, wherein 1 is a vacuum cavity, 2 is a pump set for rapid vacuum pumping, 3 is a metal plane electrode with a small hole, 4 is a radio frequency power supply, 5 is an infrared quartz heating tube, 6 is an isolating switch, 7 is a substrate, 8 is a metal net, and 9 is a micro control valve.
FIG. 2 is an X-ray diffraction pattern of comparative example 1 and example 1.
FIG. 3 is a surface scanning electron micrograph of the perovskite thin films of comparative example 1 and example 1.
Fig. 4 is a performance curve of the perovskite solar cell of comparative example 1 and example 1.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings. These drawings are simplified schematic diagrams each illustrating the basic structure of the present invention only in a schematic manner, and thus show only the constitution related to the present invention.
Example 1
This embodiment is exemplified by a 10cm by 10cm substrate,
1. in a block of 10X 10cm FTO/TiO 2 Coating perovskite precursor solution on the substrate to form a perovskite wet film. The film thickness was about 2um and the method used was slot coating. The perovskite precursor solution comprises the following components: cs0.1fa0.85ma0.05pbi3 at a concentration of 1.35M, solvent and formulation (DMF: DMSO = 4.
2. Transferring the wet film into a vacuum cavity, wherein the internal size of the vacuum cavity is as follows: length 15 cm wide and height 10cm, and the vacuum chamber door was closed.
According to the embodiment, two quartz tubes are arranged behind the metal planar electrode, the power of each quartz tube is 400W, the diameter of each quartz tube is 5mm, the diameter of each quartz tube is 10mm, and the distance between every two quartz tubes is 5mm.
A metal net is arranged between the metal plane electrode and the substrate, the diameter of the metal wire is 0.1mm, and the size of the metal grid is 1 square centimeter.
3. And (3) starting a vacuum pump set, vacuumizing the system, opening a trace gas valve when the vacuum of the system is reduced to 50Pa after about 15s, and introducing argon gas with the flow of about 0.5sccm to form the perovskite mesophase thin film.
4. After about 30s, the vacuum of the system is reduced to about 5Pa, at this time, a disconnecting switch of the quartz tube is opened, the power of the radio frequency power supply is opened for about 5W, the power is maintained for 15s, and the radio frequency power supply is closed. The perovskite intermediate phase film forms more crystal nuclei and promotes the growth of the crystal nuclei due to the given energy of the plasma.
5. The system is rapidly deflated to reach the atmospheric pressure, an isolating switch of the quartz heating tube is closed, then a power supply of a power regulator of the quartz heating tube is turned on, the output power of the power supply is regulated to be 80%, and at the moment, the temperature near the sample is about 150 ℃ and is maintained for about 2 minutes. At this time, a perovskite thin film is formed.
6. And closing the quartz heating pipe, and moving the film out of the cavity.
Fig. 2 and 3 are X-ray diffraction patterns and surface scanning electron micrographs of the perovskite thin films of example 1 and comparative example 1, and it can be seen from fig. 2 and 3 that the diffraction peaks of the perovskite thin films of example 1 have higher intensity and larger and more uniform crystal grains.
It can be seen from fig. 4 that the perovskite solar cell prepared based on the present invention has higher efficiency than that using the anti-solvent method.
Example 2
This example exemplifies a 10cm to 10cm substrate,
1. in a block of 10X 10cm FTO/TiO 2 Coating perovskite precursor solution on the substrate to form a perovskite wet film. The film thickness was about 2um, and the method used was slit coating. The perovskite precursor solution comprises the following components: cs0.1fa0.85ma0.05pbi3 at a concentration of 1.35M, in a solvent and ratio (DMF: DMSO = 4.
2. Transferring the wet film into a vacuum cavity, wherein the internal size of the vacuum cavity is as follows: length 15 cm, width 15 cm and height 10cm, the door of the vacuum chamber was closed.
According to the embodiment, two quartz tubes are arranged behind the metal planar electrode, the power of each quartz tube is 400W, the diameter of each quartz tube is 5mm, the diameter of each quartz tube is 10mm, and the distance between every two quartz tubes is 5mm.
A metal mesh is arranged between the metal plane electrode and the substrate, the diameter of the metal wire is 0.1mm, and the size of the metal mesh is 1 square centimeter.
3. And (3) starting a vacuum pump set, vacuumizing the system, opening a micro gas valve when the vacuum of the system is reduced to 50Pa for about 15s, introducing argon gas at the flow rate of about 0.5sccm, and forming the perovskite mesophase thin film.
4. After about 30s, the vacuum of the system is reduced to about 5Pa, at this time, a disconnecting switch of the quartz tube is opened, the power of the radio frequency power supply is opened for about 10W, the power is maintained for 8s, and the radio frequency power supply is closed. The perovskite intermediate phase film forms more crystal nuclei and promotes the growth of the crystal nuclei due to the given energy of the plasma.
5. The system is rapidly deflated to reach the atmospheric pressure, an isolating switch of the quartz heating tube is closed, then a power supply of a power regulator of the quartz heating tube is turned on, the output power of the power supply is regulated to be 80%, and at the moment, the temperature near the sample is about 150 ℃ and is maintained for about 2 minutes. At this time, a perovskite thin film is formed.
6. And closing the quartz heating pipe, and moving the film out of the cavity.
Example 3
This example exemplifies a 10cm to 10cm substrate,
1. in a 10X 10cm FTO/TiO mass 2 Coating perovskite precursor solution on the substrate to form a perovskite wet film. The film thickness was about 2um and the method used was slot coating. The perovskite precursor solution comprises the following components: cs0.1fa0.85ma0.05pbi3 at a concentration of 1.35M, in a solvent and ratio (DMF: DMSO = 4.
2. Transferring the wet film into a vacuum cavity, wherein the internal size of the vacuum cavity is as follows: 15 cm x 10cm, the door of the vacuum chamber was closed.
According to the embodiment, two quartz tubes are arranged behind the metal planar electrode, the power of each quartz tube is 400W, the diameter of each quartz tube is 5mm, the diameter of each quartz tube is 10mm, and the distance between every two quartz tubes is 5mm.
A metal mesh is arranged between the metal plane electrode and the substrate, the diameter of the metal wire is 0.1mm, and the size of the metal mesh is 1 square centimeter.
3. And (3) starting a vacuum pump set, vacuumizing the system, opening a micro gas valve when the vacuum of the system is reduced to 50Pa for about 15s, introducing argon gas with the flow of about 1sccm, and forming the perovskite mesophase thin film.
4. After about 25s, the vacuum of the system is reduced to about 10Pa, at this time, a disconnecting switch of the quartz tube is opened, the power of the radio frequency power supply is opened for about 5W, the power is maintained for 15s, and the radio frequency power supply is closed. The perovskite intermediate phase film forms more crystal nuclei and promotes the growth of the crystal nuclei due to the given energy of the plasma.
5. The system is quickly deflated to reach the atmospheric pressure, the isolating switch of the quartz heating tube is closed, then the power supply of the power regulator of the quartz heating tube is turned on, the output power of the power supply is regulated to be 80%, and at the moment, the temperature near the sample is about 150 ℃ and is maintained for about 2 minutes. At this time, a perovskite thin film is formed.
6. And closing the quartz heating pipe, and moving the film out of the cavity.
Example 4
1. In a block of 10X 10cm FTO/TiO 2 Coating perovskite precursor solution on the substrate to form a perovskite wet film. The film thickness was about 2um, and the method used was slit coating. The perovskite precursor solution comprises the following components: cs0.1fa0.85ma0.05pbi3 at a concentration of 1.35M, solvent and formulation (DMF: DMSO = 4.
2. Transferring the wet film into a vacuum cavity, wherein the internal size of the vacuum cavity is as follows: 15 cm by 10cm, the door of the vacuum chamber was closed.
Based on the embodiment, two quartz tubes are arranged behind the metal planar electrode, the power of each quartz tube is 400W, the diameter of each quartz tube is 5mm, the diameter of each quartz tube is opposite to the diameter of each small hole of the infrared radiation tube is 10mm, and the distance between the small holes is 5mm.
A metal net is arranged between the metal plane electrode and the substrate, the diameter of the metal wire is 0.1mm, and the size of the metal grid is 1 square centimeter.
3. And (3) starting a vacuum pump set, vacuumizing the system, opening a micro gas valve when the vacuum of the system is reduced to 50Pa for about 15s, introducing nitrogen with the flow of about 0.5sccm, and forming the perovskite mesophase thin film.
4. After about 30s, the vacuum of the system is reduced to about 5Pa, at this time, a disconnecting switch of the quartz tube is opened, the power of the radio frequency power supply is opened for about 5W, the power is maintained for 15s, and the radio frequency power supply is closed. The perovskite intermediate phase film forms more crystal nuclei and promotes the growth of the crystal nuclei due to the given energy of the plasma.
5. The system is rapidly deflated to reach the atmospheric pressure, an isolating switch of the quartz heating tube is closed, then a power supply of a power regulator of the quartz heating tube is turned on, the output power of the power supply is regulated to be 100%, and at the moment, the temperature near the sample is about 170 ℃ and is maintained for about 1 minute. At this time, a perovskite thin film is formed.
6. And closing the quartz heating pipe, and moving the film out of the cavity.
Comparative example 1
Preparation of perovskite thin film by anti-solvent method
1. In a 2.5X 2.5cm FTO/TiO mass 2 On the substrate, 50ul of perovskite solution was dropped, the perovskite precursor solution had the composition Cs0.1FA0.85MA0.05PbI3 at a concentration of 1.35M and the solvent (DMF: DMASO = 4.
2. The spin coating speed of the substrate was 4000 rpm, the spin coating time was 50s, and 100ul of chlorobenzene after 35s was sprayed onto the rotating substrate. At this time, a mesophase perovskite thin film is formed.
3. The mesophase perovskite thin film is annealed at 110 degrees for 20 minutes. Forming a perovskite thin film.
The performance data of the films obtained in the examples of the invention and the comparative examples are shown in Table 1.
TABLE 1
| V OC (V) | Jsc(mA/cm 2 ) | FF(％) | PCE(％) | |
| Example 1 | 1.06 | 23.24 | 78.20 | 19.43 |
| Example 2 | 1.05 | 23.16 | 77.26 | 18.78 |
| Example 3 | 1.05 | 23.19 | 76.88 | 18.72 |
| Example 4 | 1.02 | 22.56 | 76.01 | 17.49 |
| Comparative example 1 | 1.05 | 23.13 | 77.44 | 18.81 |
Claims (6)
1. The device for preparing the large-area perovskite thin film is characterized by comprising a vacuum cavity (1) and a pump set (2) which is connected to the middle of the top of the vacuum cavity and is used for quickly vacuumizing, wherein a metal plane electrode (3) with a small hole is arranged at the upper part in the vacuum cavity (1), the metal plane electrode (3) is connected with a radio frequency power supply (4) through a lead, infrared quartz heating pipes (5) are arranged behind the metal plane electrode (3) in parallel, the infrared quartz heating pipes (5) are connected to a power supply through isolating switches (6), a metal net (8) for reducing the plasma bombardment effect is arranged between the metal plane electrode (3) and a substrate (7), and the vacuum cavity (1) is further provided with a micro-control valve (9) capable of supplementing inert gas and controlling the constant pressure;
wherein, the rapid vacuum pumping means that the time for the pressure of the vacuum cavity to be reduced to 50-60Pa is not more than 15 seconds.
2. The apparatus for preparing large area perovskite thin film as claimed in claim 1, wherein the pump set (2) for rapid vacuum pumping is a cascade pump or a plurality of sets of pumps connected in parallel.
3. The apparatus for preparing large area perovskite thin film as claimed in claim 1, wherein the diameter of the small hole of the metal plane electrode (3) facing the infrared quartz heating tube (5) is 4-5mm, the diameter of the small hole between the infrared quartz heating tubes is 8-10mm, and the distance between the small holes is 4-5mm.
4. The apparatus for preparing large area perovskite thin film as claimed in claim 1, wherein a metal mesh is arranged between the metal plane electrode (3) and the substrate (7), the diameter of the metal wire is 0.1mm, the size of the metal mesh is 1 square centimeter, and the metal mesh is grounded or connected with a power supply capable of providing bias voltage.
5. A method of making a large area perovskite thin film, the method comprising the steps of:
(1) The perovskite wet film enters a vacuum cavity;
(2) Starting a vacuumizing pump set, rapidly reducing the pressure of the cavity to 50-60Pa, and volatilizing most of the solvent in the wet film;
the time for the pressure of the cavity to drop to 50-60Pa is not higher than 15 seconds;
(3) Opening a micro control valve to supplement inert gas and maintaining the pressure of the cavity;
(4) Starting a radio frequency power supply to form plasma and promote the crystallization of the film;
(5) The cavity is deflated, and then infrared radiation is started for 1-5 minutes to further promote the generation of the perovskite film;
(6) And closing the infrared radiation, and moving the perovskite film out of the cavity.
6. The method for preparing large area perovskite thin film as claimed in claim 5, wherein the step (3) opens the micro control valve to supplement inert gas and stabilize the vacuum pressure of the system to 5-10Pa.
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