Perovskite crystallization device

Abstract

The invention discloses a perovskite crystallization device, and relates to the technical field of perovskite cell preparation, the perovskite crystallization device comprises a furnace body, an air exhaust system and a material carrying table, the furnace body is internally provided with a crystallization cavity, the air exhaust system and the material carrying table, the furnace body is internally provided with the crystallization cavity, an air exhaust opening of the air exhaust system is communicated with the crystallization cavity, and the material carrying table is arranged on the material carrying table. The material carrying table is arranged in the crystallization cavity and used for carrying a sample, and the material carrying table is configured to be capable of heating and cooling the sample. According to the perovskite crystallization device, the vacuum drying process and the annealing process of perovskite crystallization are integrated in one furnace body, a sample does not need to be transferred in the vacuum drying and annealing process, and the sample is always located in the closed crystallization cavity and does not need to be in contact with air, so that the crystallization quality of a perovskite film is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of perovskite cell preparation, and in particular to a perovskite crystallization device. Background Art

[0002] The crystallization of perovskite thin film requires vacuum drying and annealing. Currently, these two processes are carried out in two separate devices, that is, the sample is first placed in a vacuum drying device for vacuum drying, and then the sample is transferred from the vacuum drying device to the annealing device. However, when the sample is transferred, it will be exposed to the air, thus contacting the moisture and oxygen in the air, which will cause the perovskite film to deteriorate and degrade, affecting the crystallization quality. Summary of the invention

[0003] The main purpose of the present invention is to propose a perovskite crystallization device, which aims to integrate the vacuum drying process and annealing process of perovskite crystallization into one device, so that the perovskite film layer can complete crystallization without contacting air.

[0004] To achieve the above-mentioned purpose, the perovskite crystallization device proposed in the present invention includes a furnace body, an exhaust system and a loading platform. The furnace body is provided with a crystallization cavity, an exhaust system and a loading platform. The furnace body is provided with a crystallization cavity. The exhaust port of the exhaust system is connected to the crystallization cavity. The loading platform is arranged in the crystallization cavity for carrying samples, and the loading platform is configured to be able to heat and cool the sample.

[0005] In one embodiment, a cold source channel and a hot source channel are provided in the loading platform. The hot source channel is used to pass a heating agent to heat the sample, and the cold source channel is used to pass a coolant to cool the sample.

[0006] In one embodiment, the cold source channel and the hot source channel are both bent so that the heat radiation areas of the cold source channel and the hot source channel cover the entire loading platform; and the cold source channel and the hot source channel are arranged in parallel.

[0007] In one embodiment, a sample groove is recessed on the surface of the loading platform, and the sample groove is used to accommodate the sample to be loaded.

[0008] In one embodiment, an adsorption channel is disposed in the loading platform, and an air suction port of the adsorption channel is disposed on the bottom wall of the sample tank.

[0009] In one embodiment, a plurality of adsorption channels are provided, and the air inlets of the plurality of adsorption channels are arranged at intervals on the bottom wall of the sample slot, and the air inlets of the adsorption channels are arranged at least at four corners of the sample slot.

[0010] In one embodiment, the perovskite crystallization device further includes a gas supply system, wherein the gas supply system includes a gas supply nozzle, and the gas supply nozzle is connected to the crystallization chamber and is used to apply gas to the crystallization chamber to assist the crystallization of the sample.

[0011] In one embodiment, the gas supply system further includes a plurality of gas storage tanks and gas supply pipes, wherein the plurality of gas storage tanks are arranged outside the furnace body, and each gas storage tank is used to store different types of gases, and the gas supply pipe is arranged between the furnace body and the gas storage tanks, one end of the gas supply pipe is connected to the gas supply nozzle, and the other end of the gas supply pipe is connected to a plurality of gas delivery pipes, the number of the gas delivery pipes is consistent with the number of the gas storage tanks, and one gas delivery pipe is connected to one gas storage tank.

[0012] In one embodiment, the air supply system further includes an air supply horn, the air supply horn has a closed end and a flared end, the closed end is provided with an air inlet, the flared end is provided with an air outlet, the top of the furnace body is provided with a avoidance port, the air supply horn is arranged on the furnace body, and the air outlet is connected to the avoidance port, and one end of the air supply pipe facing the furnace body is connected to the air inlet. An air distribution plate is arranged inside the air supply horn, the peripheral side wall of the air distribution plate is connected to the inner peripheral wall of the air supply horn, and the air distribution holes are arranged in an array on the air distribution plate.

[0013] In one embodiment, the air-distributing plates are provided in at least two layers, and the air-distributing plates at least in the two layers are arranged in parallel and at intervals.

[0014] The technical solution of the present invention integrates the vacuum drying process and the annealing process into one furnace body, that is, the loading platform in the perovskite crystallization device not only has the function of carrying samples, but also integrates heating and cooling functions, so that the sample can be directly annealed on the loading platform after vacuum drying. As a result, the sample does not need to be transferred during the vacuum drying and annealing process, and the sample is always in a closed crystallization chamber without contact with air, thereby improving the crystallization quality of the perovskite film. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying creative work.

[0016] Figure 1 A schematic structural diagram of an embodiment of a perovskite crystallization device provided by the present invention;

[0017] Figure 2A schematic diagram of the longitudinal cross-sectional structure of an embodiment of a perovskite crystallization device provided by the present invention;

[0018] Figure 3 A schematic diagram of the longitudinal and transverse structures of an embodiment of a perovskite crystallization device provided by the present invention;

[0019] Figure 4 This is a schematic diagram of the structure of a loading platform in one embodiment of the perovskite crystallization device provided by the present invention.

[0020] Description of Figure Numbers:

[0021] 100. Perovskite crystallization device; 1. furnace body; 11. crystallization chamber; 12. chamber door; 2. loading platform; 21. cold source channel; 22. heat source channel; 23. sample slot; 24. adsorption channel; 31. air extraction port; 41. air supply nozzle; 42. air supply horn; 43. air uniforming plate.

[0022] The realization of the purpose, functional features and advantages of the present invention will be further explained in conjunction with embodiments and with reference to the accompanying drawings. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] It should be noted that if the embodiments of the present invention involve directional indications (such as up, down, left, right, front, back, etc.), the directional indications are only used to explain the relative position relationship, movement status, etc. between the components in a certain specific posture. If the specific posture changes, the directional indication will also change accordingly.

[0025] In addition, if there are descriptions involving "first", "second", etc. in the embodiments of the present invention, the descriptions of "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of technical features indicated. Therefore, the features limited to "first" and "second" may explicitly or implicitly include at least one of the features. In addition, if "and / or" or "and / or" appears in the full text, its meaning includes three parallel solutions. Taking "A and / or B" as an example, it includes solution A, solution B, or solutions that satisfy both A and B. In addition, the technical solutions between the various embodiments can be combined with each other, but it must be based on the ability of ordinary technicians in this field to implement. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0026] The crystallization of perovskite thin film requires vacuum drying and annealing. Currently, these two processes are carried out in two separate devices, that is, the sample is first placed in a vacuum drying device for vacuum drying, and then the sample is transferred from the vacuum drying device to the annealing device. However, when the sample is transferred, it will be exposed to the air, thus contacting the moisture and oxygen in the air, which will cause the perovskite film to deteriorate and degrade, affecting the crystallization quality.

[0027] To this end, the present invention proposes a perovskite crystallization device 100 .

[0028] See also Figure 1 and Figure 2 The perovskite crystallization device 100 of the present invention includes a furnace body 1, an exhaust system and a loading platform 2. The furnace body 1 is provided with a crystallization chamber 11, an exhaust system and a loading platform 2. The furnace body 1 is provided with a crystallization chamber 11. The exhaust port 31 of the exhaust system is connected to the crystallization chamber 11. The loading platform 2 is provided in the crystallization chamber 11 for carrying samples. The loading platform 2 is configured to heat and cool the samples.

[0029] The embodiment of the perovskite crystallization device 100 includes a furnace body 1, an exhaust system and a loading platform 2. A crystallization chamber 11 is provided in the furnace body 1. A chamber door 12 is provided on one side of the furnace body 1 to open or close the crystallization chamber 11. The chamber door 12 can be integrally connected with the loading platform 2, or the chamber door 12 and the loading platform 2 are separately provided. The exhaust system includes an exhaust pump (not indicated) and an exhaust pipe (not indicated). The exhaust port 31 of the exhaust pipe is provided on the bottom wall of the furnace body 1 to communicate with the crystallization chamber 11. The loading platform 2 is provided in the crystallization chamber 11 for carrying samples. During the crystallization operation, the chamber door 12 is opened, and the sample coated with the perovskite precursor solution is placed on the loading platform 2, and it is ensured that the coating surface is placed upward, and then the chamber door 12 is closed, and the exhaust pump is started to exhaust air. The solvent in the perovskite coating is rapidly volatilized in a vacuum environment, thereby achieving vacuum drying and crystallization. It is not difficult to understand that perovskite may produce certain defects during the crystallization process, such as dislocations, vacancies and grain boundaries. In order to improve the structure and performance of the crystal, perovskite will undergo an annealing process, that is, a heating process, after vacuum drying. The high temperature during the annealing process can promote the movement and reorganization of the crystal, thereby forming a more uniform and ordered crystal structure.

[0030] The traditional preparation method usually separates the vacuum drying process and the annealing process from each other, that is, vacuum drying is first performed in a vacuum drying device, and then the crystallized product is moved from the vacuum drying device to the annealing device. This preparation method not only causes the sample to contact the air during transfer, affecting the crystallization quality, but also increases the complexity of the entire set of process equipment. Different from this, the technical solution of the present invention integrates the vacuum drying process and the annealing process in one furnace body 1. That is, the loading platform 2 in the perovskite crystallization device 100 not only has the function of carrying the sample, but also integrates the heating function and the cooling function, so that the sample can be annealed directly on the loading platform 2 after completing the vacuum drying. As a result, the sample does not need to be transferred during the vacuum drying and annealing process, and the sample is always in the closed crystallization chamber 11 without contacting the air, thereby improving the crystallization quality of the perovskite film.

[0031] In order to realize the heating function and cooling function of the loading platform 2, in one embodiment of the present invention, referring to Figure 2 and Figure 3 A cold source channel 21 and a hot source channel 22 are provided in the loading platform 2. The hot source channel 22 is used for passing a heating agent to heat the sample, and the cold source channel 21 is used for passing a coolant to cool the sample.

[0032] During the vacuum drying of the perovskite film, hot water or hot oil can be introduced into the heat source channel 22 as a heating agent. The heating agent can provide sufficient heat to help the solvent in the precursor solution evaporate quickly and accelerate the crystallization rate. On the other hand, it can promote the movement and reorganization of crystals, thereby forming a more uniform and orderly crystal structure. After the vacuum drying process is completed, cold water or cold air can be introduced into the cold source channel 21 as a coolant to achieve rapid cooling of the product, effectively eliminate the thermal stress caused by high temperature treatment, and ensure the stability and durability of the material.

[0033] Furthermore, the cold source channel 21 and the hot source channel 22 are both bent, such as in a spiral or zigzag shape, so that the heat radiation area of ​​the cold source channel 21 and the hot source channel 22 covers the entire loading platform 2, thereby ensuring that the heat transfer range of the cold source channel 21 and the hot source channel 22 can cover every area of ​​the loading platform 2, thereby providing a loading platform 2 with uniform temperature for the sample, thereby ensuring that the crystals can grow uniformly.

[0034] Furthermore, the cold source channel 21 and the hot source channel 22 can be arranged in parallel. At this time, the vertical distance between the cold source channel 21 and the hot source channel 22 at any position is always kept consistent. This can avoid the problem of local overheating or local overcooling caused by uneven spacing between the cold source channel 21 and the hot source channel 22, thereby achieving uniform distribution of the temperature field.

[0035] Reference Figure 4 The surface of the loading platform 2 is provided with a sample groove 23, and the sample groove 23 is used to receive the sample to be loaded. The shape and size of the sample groove 23 are customized according to the sample to be loaded to achieve accurate positioning of the sample, thereby preventing the sample from shifting or sliding on the loading platform 2, and ensuring the stability of the sample during the entire crystallization process.

[0036] In one embodiment, an adsorption channel 24 is provided in the loading platform 2, and the air inlet of the adsorption channel 24 is provided at the bottom wall of the sample slot 23. The end of the adsorption channel 24 away from the air inlet is connected to a vacuum pump. When the vacuum pump is started, the air inlet will suck away the air at the bottom of the sample, so that the air pressure at the bottom of the sample is lower than the air pressure in the crystallization chamber 11. Due to the pressure difference, the air pressure in the crystallization chamber 11 will press the sample tightly in the sample slot 23, thereby achieving non-destructive fixation of the sample without causing any physical damage to the sample. After the crystallization process is completed, the vacuum state of the adsorption channel 24 can be gradually released to gradually separate the sample from the bottom wall, so as to facilitate the removal of the sample.

[0037] Furthermore, there are multiple adsorption channels 24, and the air inlets of the multiple adsorption channels 24 are arranged at intervals on the bottom wall of the sample slot 23, so as to ensure that the bottom of the sample is uniformly subjected to the adsorption force, and prevent the sample from being locally warped or lifted due to temperature changes during heating or cooling. And there are at least four adsorption channels 24, that is, there can be four, five, six or more adsorption channels 24. When there are only four adsorption channels, the air inlets of the four adsorption channels 24 are arranged at the four corners of the sample slot 23, so as to ensure that the four corners of the sample can be firmly adsorbed, thereby providing solid stability for the entire sample. At this time, the stability of the sample can be guaranteed while simplifying the adsorption channels 24. When the size of the product is large, the number of adsorption channels 24 can be increased to improve the adsorption force, and whether there are four, five or more adsorption channels 24, the air inlets should be evenly distributed on the bottom wall of the sample slot 23 to achieve uniform adsorption of the entire sample.

[0038] Some embodiments of the perovskite crystallization device 100 further include a gas supply system, which includes a gas supply nozzle 41 , which may be a shower head. The gas supply nozzle 41 is connected to the crystallization chamber 11 and is used to apply gas to the crystallization chamber 11 to assist sample crystallization.

[0039] Specifically, the gas supply system also includes a plurality of gas storage tanks (not marked) and gas supply pipes (not marked). The plurality of gas storage tanks are arranged outside the furnace body 1, and each gas storage tank is used to store different types of gases. The gas supply pipe is arranged between the furnace body 1 and the gas storage tanks. One end of the gas supply pipe is connected to the gas supply nozzle 41, and the other end of the gas supply pipe is connected to a plurality of gas delivery pipes (not marked). The number of gas delivery pipes is consistent with the number of gas storage tanks, and one gas delivery pipe is connected to one gas storage tank.

[0040] In this embodiment, each gas delivery tank is used to store different types of gases, such as single gases or mixed gases such as nitrogen, argon, chlorobenzene, toluene, etc. These gases are transported to the crystallization chamber 11 through gas pipes and gas delivery pipes, which can provide a suitable chemical atmosphere to promote the uniform nucleation and growth of perovskite crystals.

[0041] Among them, each gas pipeline is provided with a flow regulating valve, which is used to adjust the size of the flow cross-section of the corresponding gas pipeline, thereby allowing the operator to control the gas flow according to the specific needs of the crystallization process, optimize the chemical atmosphere during the crystallization process, and improve the quality of the perovskite crystal.

[0042] In the embodiment shown in the figure, the air supply system also includes an air supply horn 42, which has a closed end and a flared end, the closed end is provided with an air inlet, the flared end is provided with an air outlet, the top of the furnace body 1 is provided with a avoidance port, the air supply horn 42 is provided on the furnace body 1, and the air outlet is connected to the avoidance port. The air supply horn 42 and the furnace body 1 can be integrally formed, or the air supply horn 42 and the furnace body 1 can be formed separately, and then the air supply horn 42 and the furnace body 1 are connected, so that the air outlet of the air supply horn 42 is connected to the avoidance port opened on the top of the furnace body 1.

[0043] In this embodiment, the air supply horn 42 is used to deliver gas to the crystallization chamber 11, so that the gas can be diffused in an orderly manner when entering the crystallization chamber 11, ensuring that the entire sample surface can be covered by the gas. It should be noted that the size of the avoidance port is consistent with the size of the gas outlet, and the avoidance port is arranged directly opposite to the sample slot 23 on the loading platform 2, and the projection area of ​​the avoidance port on the loading platform 2 is at least two-thirds of the positive projection area of ​​the sample slot 23, so as to ensure that the area of ​​the avoidance port is large enough to ensure that the gas output from the air supply horn 42 can fully cover the front of the entire sample after diffusion.

[0044] In one embodiment, an air uniforming plate 43 is provided in the air supply horn 42, and the peripheral side wall of the air uniforming plate 43 is connected to the inner peripheral wall of the air supply horn 42, and the air uniforming plate 43 is arrayed with air uniforming holes, which may be circular holes, square holes or other shapes. The air uniforming holes can disperse the concentrated airflow into multiple small airflows, so that the gas can be more evenly diffused to the product surface, making the crystallization more uniform.

[0045] Furthermore, the gas-distributing plates 43 may be provided with one layer, two layers, three layers or even more than three layers. When more than two layers are provided, the gas-distributing plates 43 are provided in parallel and spaced apart. The multiple gas-distributing plates 43 may further disperse the gas so that the gas can be diffused to the product surface more evenly.

[0046] The above description is only an exemplary embodiment of the present invention, and does not limit the patent scope of the present invention. All equivalent structural changes made by using the contents of the present invention specification and drawings under the technical concept of the present invention, or directly / indirectly applied in other related technical fields are included in the patent protection scope of the present invention.

Claims

1. A perovskite crystallization device, characterized in that: include: A furnace body, wherein a crystallization cavity is arranged in the furnace body; An air extraction system, wherein an air extraction port of the air extraction system is connected to the crystallization chamber; A loading platform is arranged in the crystallization chamber for loading a sample, and the loading platform is configured to heat and cool the sample.

2. The perovskite crystallization device according to claim 1, characterized in that: A cold source channel and a hot source channel are arranged in the loading platform. The hot source channel is used for passing a heating agent to heat the sample, and the cold source channel is used for passing a coolant to cool the sample.

3. The perovskite crystallization device according to claim 2, characterized in that: The cold source channel and the hot source channel are both bent so that the heat radiation areas of the cold source channel and the hot source channel cover the entire loading platform; Furthermore, the cold source channel and the hot source channel are arranged in parallel.

4. The perovskite crystallization device according to claim 1, characterized in that: A sample groove is concavely arranged on the surface of the loading platform, and the sample groove is used to accommodate the sample to be loaded.

5. The perovskite crystallization device according to claim 4, characterized in that: An adsorption channel is arranged in the material loading platform, and an air suction port of the adsorption channel is arranged on the bottom wall of the sample tank.

6. The perovskite crystallization device according to claim 5, characterized in that: There are multiple adsorption channels, and the air inlets of the multiple adsorption channels are arranged at intervals on the bottom wall of the sample slot, and the air inlets of the adsorption channels are arranged at least at four corners of the sample slot.

7. The perovskite crystallization device according to any one of claims 1 to 6, characterized in that: The perovskite crystallization device further comprises a gas supply system, wherein the gas supply system comprises a gas supply nozzle, and the gas supply nozzle is connected to the crystallization chamber and is used for applying gas to the crystallization chamber to assist the crystallization of the sample.

8. The perovskite crystallization device according to claim 7, characterized in that: The air supply system also includes: A plurality of gas storage tanks, wherein the plurality of gas storage tanks are arranged outside the furnace body, and each gas storage tank is used to store different types of gases; An air supply pipe, wherein the air supply pipe is arranged between the furnace body and the gas storage tank, one end of the air supply pipe is connected to the air supply nozzle, and the other end of the air supply pipe is connected to a plurality of gas delivery pipes, the number of the gas delivery pipes is consistent with the number of the gas storage tanks, and one gas delivery pipe is connected to one gas storage tank.

9. The perovskite crystallization device according to claim 8, characterized in that: The air supply system also includes an air supply horn, the air supply horn has a closed end and a flared end, the closed end is provided with an air inlet, the flared end is provided with an air outlet, the top of the furnace body is provided with a avoidance port, the air supply horn is arranged on the furnace body, and the air outlet is connected to the avoidance port, and one end of the air supply pipe facing the furnace body is connected to the air inlet; An air uniforming plate is arranged in the air supply horn, the peripheral side wall of the air uniforming plate is connected to the inner peripheral wall of the air supply horn, and the air uniforming plate is provided with air uniforming holes arranged in an array.

10. The perovskite crystallization device according to claim 9, characterized in that: The air-distributing plates are provided with at least two layers, and the air-distributing plates at or above the two layers are arranged in parallel and at intervals.

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