A temperature-controllable vacuum drying apparatus

Abstract

The utility model provides a kind of temperature-controllable vacuum drying equipment, including including process cavity and vacuum system;The process cavity is provided with the support platform for placing the product to be dried in;The vacuum system is communicated with the process cavity, for extracting vacuum to the process cavity;Heating element is provided in the cavity wall of the process cavity, and the heating element is used to adjust the inner wall temperature of the process cavity.The present application is heated in real time to the inner wall of process cavity, to promote the solvent volatilization adsorbed on the inner wall, to avoid the influence on subsequent drying crystallization process.

Description

Technical Field

[0001] This application relates to the field of semiconductor technology, and in particular to a temperature-controllable vacuum drying apparatus. Background Technology

[0002] As the perovskite industry continues to develop, perovskite modules are becoming larger and more efficient. The key to further improving efficiency in the industrialization of perovskite lies in the uniformity of large-area annealing crystallization. In particular, controlling the uniformity and repeatability of crystallization during mass production is a crucial factor in ensuring efficiency and yield.

[0003] Currently, the mainstream equipment for drying perovskite wet films is the vacuum concentration drying (VCD) system. Research has revealed that in the drying process for large-area perovskite thin films (taking 1.2m*0.6m or 1.2m*2.4m as examples), there are still problems with poor mass production yield and frequent maintenance. This is because perovskite wet films at the square meter level contain a large amount of solvent, and during the vacuum drying process, a significant amount of solvent is adsorbed inside the VCD chamber. Since the VCD chamber is generally small, as mass production continues, the amount of solvent accumulated on the inner wall of the chamber increases, directly affecting the quality of subsequent perovskite film drying. The common solution to this problem is frequent disassembly and internal maintenance of the equipment, which significantly reduces mass production output and increases labor costs.

[0004] On the other hand, existing VCD equipment relies on saturated vapor pressure for drying. The basic principle is to rapidly reduce the chamber pressure to below the saturated vapor pressure of the perovskite solvent, causing the solvent to evaporate, which is then quickly removed by a vacuum pump. However, the drying process of perovskite wet films involves complex physicochemical reactions, and often uses two or more solvents. Some perovskite formulations are even more complex, with mixtures of up to four to six solvents. Existing VCD equipment cannot meet the needs of adapting to a wider range of perovskite formulations and processes.

[0005] It should be noted that the above introduction to the technical background is only for the purpose of providing a clear and complete explanation of the technical solutions of this application and facilitating understanding by those skilled in the art. It should not be assumed that these technical solutions are known to those skilled in the art simply because they have been described in the background section of this application. Utility Model Content

[0006] To solve all or part of the problems of the prior art, this utility model provides a temperature-controllable vacuum drying device to achieve the purpose of adapting to different perovskite formulations and avoiding the retention of solvent on the inner wall of the chamber.

[0007] To achieve the above objectives, this utility model provides a temperature-controllable vacuum drying device, including a process chamber and a vacuum system;

[0008] The process chamber is equipped with a platform for placing the products to be dried.

[0009] The vacuum system is connected to the process chamber and is used to evacuate the process chamber.

[0010] A heating element is provided in the cavity wall of the process chamber, and the heating element is used to regulate the inner wall temperature of the process chamber.

[0011] This application heats the inner wall of the process chamber in real time to cause the solvent adsorbed on the inner wall to evaporate, thus avoiding the impact on the subsequent drying and crystallization process.

[0012] The process cavity includes a process cavity outer shell and a process cavity inner shell, and the heating element is disposed between the process cavity outer shell and the process cavity inner shell.

[0013] The heating element is a heating wire.

[0014] The loading platform is located on the bottom inner wall of the process chamber.

[0015] A heat-insulating material layer is provided between the loading platform and the inner wall of the process cavity.

[0016] A medium transmission pipe is provided inside the cargo platform, and the temperature of the cargo platform is regulated by introducing a flowing medium through the medium transmission pipe.

[0017] The vacuum system includes a vacuum pipeline and a vacuum pump connected in sequence; an exhaust port is provided in the process chamber, and the vacuum pipeline is connected to the exhaust port.

[0018] The exhaust port is located at the upper part of the process chamber.

[0019] A temperature sensor is also provided, which includes a first sensor for detecting the temperature of the inner wall of the process chamber and a second sensor for detecting the temperature of the loading platform.

[0020] It is also equipped with a temperature control element, which is used to receive temperature data collected by the temperature sensor and control the heating element and / or the medium transmission pipeline based on preset conditions.

[0021] Compared with existing technologies, the main advantages of this invention are as follows: By introducing a heating wire, the solvent adsorbed and accumulated inside the vacuum chamber can be quickly removed, ensuring the VCD process chamber remains relatively clean. A temperature-controlled medium transfer channel is incorporated into the platform, allowing for control of perovskite crystallization during the VCD vacuuming process. For perovskite systems with fast crystallization rates, a low-temperature medium is used to normalize the crystallization speed. For perovskite systems with slow crystallization rates, a high-temperature medium is used to accelerate crystallization. This invention offers greater applicability to perovskite systems, a wider process window, better repeatability, and contributes to improved perovskite crystallization quality. Attached Figure Description

[0022] To more clearly illustrate the technical solutions in the specific embodiments of this utility model, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0023] Figure 1 This is a schematic diagram of the vacuum drying equipment provided in this application. Detailed Implementation

[0024] The foregoing and other technical contents, features, and effects of this utility model will be clearly presented in the following detailed description of the preferred embodiments with reference to the accompanying drawings. The directional terms mentioned in the following embodiments, such as up, down, left, right, front, or back, are only for reference to the accompanying drawings. Therefore, the directional terms used are for illustrative purposes and not for limiting the scope of this utility model.

[0025] Example 1:

[0026] Figure 1 This is a schematic diagram of the vacuum drying equipment provided in this application. In this embodiment, to achieve directional temperature control and assist the vacuum drying equipment in uniform drying, and to prevent the perovskite film surface from being affected by residual solvent in the cavity, this application provides the following technical solution:

[0027] refer to Figure 1 This application provides a temperature-controllable vacuum drying device, including a process chamber and a vacuum system; a loading platform 4 for placing the product 9 to be dried 9 is provided in the process chamber; the vacuum system is connected to the process chamber and is used to evacuate the process chamber; a heating element is provided in the cavity wall of the process chamber, and the heating element is used to adjust the inner wall temperature of the process chamber.

[0028] like Figure 1As shown, the process chamber consists of an inner wall and an outer wall, meaning the process chamber comprises a process chamber outer shell 1 and a process chamber inner shell 2. The process chamber, used for vacuum drying, is constructed from the process chamber outer shell 1 and the process chamber inner shell 2. In this application, the size and shape of the process chamber outer shell 1 and the process chamber inner shell 2 are not limited; they can be customized according to the size and shape of the product 9 to be dried (i.e., the glass substrate coated with a perovskite wet film).

[0029] A controllable heating element is arranged between the outer shell 1 and the inner shell 2 of the process chamber. In this embodiment, the heating element used is a heating wire 3, which is tightly attached to the surface of the inner shell 2 to heat the inner wall of the chamber. It should be understood that during the extremely short time of rapid evacuation of the VCD device, a large amount of solvent in the perovskite wet film will evaporate. Since a large amount of solvent cannot be completely evaporated in a short time, some will be adsorbed onto the inner wall of the process chamber. Over time, the excess solvent will cause solvent mismatch problems during subsequent perovskite crystallization. The heating wire 3 can heat the inner wall of the process chamber in real time, promoting the evaporation of the solvent adsorbed on the inner wall and avoiding any impact on the subsequent drying and crystallization process. The heating wire 3 can be selected in different specifications according to actual needs, and the temperature can also be customized; generally, the heating temperature is between 25-120 degrees Celsius.

[0030] A platform 4 is provided at the bottom of the process chamber for placing the product 9 to be dried, which in this embodiment is a glass substrate coated with a perovskite wet film. The platform 4 is located on the bottom surface of the chamber and is isolated from the inner wall of the bottom by a heat-insulating material to avoid uncontrolled influence of the temperature of the inner wall of the chamber on the drying and crystallization of the platform 4.

[0031] A media transmission pipe 5 is installed in the loading platform 4. One end of the media transmission pipe 5 is connected to the plant's media inlet, and the other end is connected to the plant's media outlet. The media transmission pipe 5 can regulate the temperature of the loading platform 4 by introducing media of different types and temperatures (such as process water or oil at different temperatures), thereby achieving directional temperature control and assisting the vacuum drying equipment in achieving uniform drying. For example, for perovskite systems with fast crystallization rates, a low-temperature medium is used to control the crystallization rate to normalize it; for perovskite systems with slow crystallization rates, a high-temperature medium is used to accelerate perovskite crystallization. Therefore, it has stronger applicability to different perovskite systems, a wider process window, and better repeatability, which is beneficial to improving the crystallization quality of perovskite.

[0032] like Figure 1As shown, the vacuum system includes a vacuum pipeline 6 and a vacuum pump 7 connected in sequence. An exhaust port (not shown) is provided in the process chamber, typically located at the top. One side of the vacuum pipeline 6 connects to the exhaust port, and the other side connects to the vacuum pump 7, serving as the channel for solvent extraction from the process chamber. The vacuum pump 7 is generally located outside the VCD process chamber. Rapid evacuation by the vacuum pump 7 achieves a rapid decrease in internal pressure, thus evaporating the solvent. After evacuation, the pressure in the process chamber decreases. When the pressure falls below the saturated vapor pressure of the solvent in the product 9 to be dried, the solvent evaporates and is discharged from the vacuum system via a discharge path 8 as shown. Figure 1 As shown.

[0033] In the vacuum drying equipment, a temperature sensor (not shown in the figure) may also be installed. The temperature sensor includes at least a first sensor for detecting the temperature of the inner wall of the drying chamber and a second sensor for detecting the temperature of the loading platform. Correspondingly, a temperature control element is also provided to receive the temperature data collected by the temperature sensor and control the heating element and / or the medium transmission pipeline based on preset conditions. For example, the inner wall temperature may be increased or decreased by controlling the power of the heating element; or the loading platform may be increased or decreased by controlling the flow rate or temperature of the medium in the medium transmission pipeline.

[0034] A common operating procedure for the vacuum drying equipment provided in this application is as follows:

[0035] S1: Start vacuum pump 7 and pump the pressure in the process chamber to the set value, for example, 1 Pa;

[0036] S2: Place the product 9, which has been coated with a perovskite wet film and is to be dried, onto the loading platform 4 in the process chamber.

[0037] S3: Set the loading platform 4 to a suitable temperature, and control the evaporation of perovskite solvent and its crystallization rate by temperature control;

[0038] S4: The chamber pressure is quickly evacuated to a vacuum state using vacuum pump 7, with a chamber pressure of 10. -50 Pa;

[0039] S5: By setting the temperature of the heating wire 3 between the outer shell 1 and the inner shell 2 of the process chamber, the solvent adsorbed on the inner wall of the chamber is rapidly evaporated and extracted from the chamber.

[0040] S6: After the solvent has been completely removed, take out the product and proceed with the subsequent perovskite preparation process to complete the component preparation.

[0041] The fabrication process of a perovskite device is as follows:

[0042] The preparation process includes:

[0043] Step 1: Weigh the perovskite precursor powder. The molecular formula of the perovskite precursor solution is as follows (but not limited to this molecular formula; conventional perovskite molecular formulas are all within the scope of this invention): Cs 0.05 FA 0.95 The specific formulation of PbI3 components is as follows: at a 1M concentration, each milliliter of solution contains: CsI (19.5 mg); FAI (231.69 mg); PbI2 (682.5 mg);

[0044] Step 2: Prepare the perovskite precursor solution. Add an appropriate amount of DMF, NMP, and DMSO mixed solvent to the pharmaceutical powder from Step 1 (preparing a 1.0M perovskite solution according to an appropriate ratio). It is worth noting that if the solvent ratio is unbalanced, the α-phase perovskite film cannot be directly prepared. More specifically, in this embodiment, the solvent ratio is DMF:NMP:DMSO = 400:40:40. Place the solution on a stirring table and stir at room temperature for 4 hours to ensure complete dissolution. See the table below for the solvent ratio details.

[0045] Solvent ratio in the example DMF 400 NMP 40 DMSO 40

[0046] Step 3: The above perovskite precursor mixture is used to prepare a uniform perovskite solution wet film on a TCO substrate using a blade coating device or a slit coating device;

[0047] Step 4: Transfer the wet film substrate from Step 3 into the vacuum drying equipment and rapidly evacuate it to a vacuum level of 10 within 50-100 seconds. -50 By using a solvent within the Pa range (in the range of Pa), the solvent can be rapidly evaporated, thus preparing a perovskite thin film.

[0048] Step 5: Evaporate C60, BCP and Cu onto the perovskite substrate prepared above.

[0049] The common English terms or letters used in this utility model for the purpose of clear description are for illustrative purposes only and are not intended to be limiting or specific. They should not be used to limit the scope of protection of this application based on their possible Chinese translations or specific letters.

[0050] It should also be noted that in this article, relational terms such as “first” and “second” are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations.

Claims

1. A temperature-controllable vacuum drying device, characterized in that, Including process chambers and vacuum systems; The process chamber is provided with a platform for placing the product to be dried. A medium transmission pipe is provided inside the platform. The medium transmission pipe regulates the temperature of the platform by introducing a flowing medium. The vacuum system is connected to the process chamber and is used to evacuate the process chamber. A heating element is provided in the cavity wall of the process chamber, and the heating element is used to regulate the inner wall temperature of the process chamber.

2. The temperature-controllable vacuum drying equipment according to claim 1, characterized in that, The process cavity includes a process cavity outer shell and a process cavity inner shell, and the heating element is disposed between the process cavity outer shell and the process cavity inner shell.

3. The temperature-controllable vacuum drying equipment according to claim 2, characterized in that, The heating element is a heating wire.

4. The temperature-controllable vacuum drying equipment according to claim 1, characterized in that, The loading platform is located on the bottom inner wall of the process chamber.

5. The temperature-controllable vacuum drying equipment according to claim 4, characterized in that, A heat-insulating material layer is provided between the loading platform and the inner wall of the process cavity.

6. The temperature-controllable vacuum drying equipment according to claim 1, characterized in that, The vacuum system includes a vacuum pipeline and a vacuum pump connected in sequence; an exhaust port is provided in the process chamber, and the vacuum pipeline is connected to the exhaust port.

7. The temperature-controllable vacuum drying equipment according to claim 6, characterized in that, The exhaust port is located at the upper part of the process chamber.

8. The temperature-controllable vacuum drying equipment according to claim 5, characterized in that, A temperature sensor is also provided, which includes a first sensor for detecting the temperature of the inner wall of the process chamber and a second sensor for detecting the temperature of the loading platform.

9. A temperature-controllable vacuum drying device according to claim 8, characterized in that, It is also equipped with a temperature control element, which is used to receive temperature data collected by the temperature sensor and control the heating element and / or the medium transmission pipeline based on preset conditions.

Images