Multi-pipeline cavity vacuum desolventizing flash evaporation system

Abstract

The invention provides a multi-pipeline cavity vacuum desolventizing flash evaporation system. The multi-pipeline cavity vacuum desolventizing flash evaporation system comprises a heatable built-in vacuum cavity, a heating and refrigerating base station, a heating column, a rotating shaft, vacuum pipelines, a detachable large-capacity external vacuum cavity, a molecular pump, a copper pipe cold trap and a large-pumping-amount mechanical pump. Six surfaces of the built-in vacuum cavity are connected with a detachable large-capacity external vacuum cavity through vacuum pipelines, a sand core gas uniformizing sheet is mounted on the inner wall of the built-in vacuum cavity, and a heating and refrigerating base station capable of stably rotating in any direction is mounted in the built-in vacuum cavity; the detachable large-capacity external vacuum cavity is connected with a copper pipe cold trap through an air exhaust pipeline, and the copper pipe cold trap is connected with a molecular pump and a large-pumping-amount mechanical pump. According to the invention, the heatable multi-pipeline cavity is arranged to volatilize the solvent, and the sand core gas uniformizing sheet and the heating and refrigerating base station capable of stably rotating in any direction are arranged in the cavity, so that the volatile solvent can be extracted more comprehensively, quickly and stably.

Description

Technical Field

[0001] The invention belongs to the technical field of perovskite photovoltaic cells, and in particular relates to a multi-pipeline cavity vacuum desolventizing flash evaporation system. Background Art

[0002] Flash evaporation is a vacuum-based evaporation method that is particularly suitable for preparing perovskite films for solar cells. Growth pressure is a key parameter for perovskite film growth. This method adjusts the pressure of the environment to quickly vaporize the solvent in the perovskite film from the liquid phase, thereby achieving crystal precipitation and film formation. The perovskite film prepared using vacuum flash evaporation technology is uniform, dense, pinhole-free, and has a large grain size. Therefore, the flash evaporation method has great potential in the preparation of high-performance, large-area perovskite solar cells. The rate of chamber vacuum evaporation, the stability and completeness of solvent extraction are closely related to the quality of perovskite film formation.

[0003] The traditional single-channel vacuum flash evaporation system extracts vacuum from one direction and does not have a sand core gas-distributing plate design. This results in poor uniformity and stability of the vacuum pumping and uneven extraction, which requires further improvement. By carefully designing and optimizing the built-in vacuum chamber of the vacuum flash evaporation system, the solvent volatilization and removal effects can be improved, thereby obtaining high-quality perovskite films with large grain size, good crystallinity, uniform and dense film formation. This technology is crucial to significantly enhance the application potential of perovskite solar cells in large-area preparation processes. Summary of the invention

[0004] The present invention provides a multi-pipeline cavity vacuum desolventizing flash evaporation system, which solves the problems of slow, incomplete and uneven solvent extraction rate in existing flash evaporation systems, as well as condensation of volatile solvents into liquid contaminated samples due to uneven temperature in a built-in vacuum cavity. The present invention can increase the extraction rate of gaseous solvents in the cavity from the original 1-2 L / s to 10-15 L / s. In addition, the extraction of gaseous solvents is more uniform, and the cavity pressure distribution deviation is reduced to within 5%. The pipeline aperture can be quickly adjusted through a pipeline conversion head to achieve a more controllable and significant effect. Compared with traditional devices, the extraction efficiency can be increased by 70% to 90%.

[0005] To solve the above problems, the technical solution provided by the present invention is as follows:

[0006] The embodiment of the present invention provides a multi-pipeline cavity vacuum desolventizing flash evaporation system, comprising a heatable built-in vacuum cavity (1), wherein a sand core gas-distributing sheet (8) is arranged on the cavity inner wall of the built-in vacuum cavity (1); the built-in vacuum cavity (1) is equipped with a heating and cooling base (9), and the heating and cooling base (9) is supported by a heating column (11) and a rotating shaft (12), and can realize large-angle rotation and control in the temperature range of -20°C to 150°C;

[0007] The heating and cooling base (9) is connected to a heating side block (10), and the heating side block (10) is used to heat the sample in the built-in vacuum chamber (1) around the sample to achieve uniform heating of the sample and increase the solvent volatilization rate in the sample film. In addition, during the rotation of the heating and cooling base (9), the sample can rotate more stably and firmly.

[0008] The built-in vacuum chamber (1) can be heated to 25-150° C. Each cavity surface of the built-in vacuum chamber (1) is provided with a plurality of vacuum pipes (7), each of which can be connected to a detachable large-capacity external vacuum chamber (2), and the external vacuum chamber (2) is used to extract vacuum from the built-in vacuum chamber (1); the external vacuum chamber (2) is connected to a copper tube cold trap (5) via a first exhaust pipe (6-1), the copper tube cold trap (5) is connected to a molecular pump (4) and a large-volume mechanical pump (3) via a second exhaust pipe (6-2), and the molecular pump (4) and the large-volume mechanical pump (7) are connected via a third exhaust pipe (6-3).

[0009] According to an optional embodiment of the present invention, a first solenoid valve (13-1) is provided on the vacuum pipe (7), a second solenoid valve (13-2) is provided on the first air extraction pipe (6-1), two third solenoid valves (13-3) are provided on two branch pipes of the second air extraction pipe (6-2), and a fourth solenoid valve (13-4) is provided on the third air extraction pipe (6-3).

[0010] According to an optional embodiment of the present invention, the built-in vacuum chamber (1) comprises a plurality of built-in vacuum chamber surfaces (14), and a pipeline conversion head (15) is arranged on the periphery of each built-in vacuum chamber surface (14).

[0011] According to an optional embodiment of the present invention, the built-in vacuum chamber (1) is a rectangular parallelepiped structure, and its six cavity surfaces are connected to a detachable large-capacity external vacuum chamber through vacuum pipes to perform vacuum extraction from all directions, wherein the multiple pipes designed on each cavity surface of the built-in vacuum chamber (1) can adjust their apertures according to the air pressure distribution in the cavity.

[0012] According to an optional embodiment of the present invention, the thickness of the sand core air-distributing sheet (8) is 10 to 20 mm, and the pore size thereof is 100 to 200 um.

[0013] Compared with the prior art, the embodiment of the present invention provides a multi-pipeline chamber vacuum desolventizing flash evaporation system, which has the following beneficial effects: the present invention not only solves the problem of uneven temperature distribution in the built-in vacuum chamber of the traditional flash evaporation system, which causes the volatile solvent to condense into liquid and contaminate the sample, but also can vaporize the solvent on the surface of the sample in the flash evaporation vacuum chamber more quickly, and can also achieve a faster, more comprehensive and more stable extraction effect, thereby improving the vaporization rate and extraction efficiency of the solvent, which is conducive to the formation of a dense, high-quality perovskite film. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] In order to more clearly illustrate the technical solutions in the embodiments or 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 invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0015] Figure 1 A schematic diagram of a multi-pipeline chamber vacuum desolventizing flash evaporation system provided in an embodiment of the present application.

[0016] Figure 2 A schematic diagram of a built-in vacuum chamber of a multi-pipeline chamber vacuum desolventizing flash evaporation system provided in an embodiment of the present application. DETAILED DESCRIPTION

[0017] The technical solutions in the embodiments of the present application will be described clearly and completely below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the present application.

[0018] In the description of the present application, it should be noted that the orientation or positional relationship indicated by the terms "inside", "outside", etc. is based on the orientation or positional relationship shown in the drawings, or the orientation or positional relationship in which the product of the application is usually placed when in use, which is only for the convenience of describing the present application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present application. In addition, the terms "first", "second", etc. are only used to distinguish the description, and cannot be understood as indicating or implying relative importance. It should also be noted that, unless otherwise clearly specified and limited, the terms "set" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection: it can be directly connected, it can also be indirectly connected through an intermediate medium, and it can be the internal connection of two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present application can be understood according to specific circumstances. The following descriptions of the embodiments are with reference to the attached drawings to illustrate specific embodiments in which the present invention can be implemented. The directional terms mentioned in the present invention, such as "up", "down", "front", "back", "left", "right", "inside", "outside", "side", etc., are only used to refer to the directions of the attached drawings. Therefore, the directional terms used are used to illustrate and understand the present invention, but are not used to limit the present invention. In the drawings, units with similar structures are represented by the same reference numerals.

[0019] like Figure 1 As shown, an embodiment of the present invention provides a multi-pipe cavity vacuum desolventizing flash evaporation system, including a heatable built-in vacuum chamber 1, a heating and cooling base 9, a heating column 11, a rotating shaft 12, a vacuum pipeline 7, a molecular pump 4, a copper tube cold trap 5 and a large-capacity mechanical pump 3.

[0020] A sand core gas-distributing sheet 8 is provided on the inner wall of the built-in vacuum chamber 1. The thickness of the sand core gas-distributing sheet 8 is 10 to 20 mm, and the aperture thereof is 100 to 200 μm. The built-in vacuum chamber 1 is provided with a heating and cooling base 9. The heating and cooling base 9 is supported by a heating column 11 and a rotating shaft 12, and can realize large-angle rotation and control of a temperature range of -20°C to 150°C. The heating and cooling base 9 includes a heater and a cooling compressor for heating and cooling functions.

[0021] The heating and cooling base 9 is connected to a heating side block 10, which is used to heat the sample around the built-in vacuum chamber 1 to achieve uniform heating of the sample and increase the evaporation rate of the solvent in the sample film. In addition, during the rotation of the heating and cooling base 9, the sample rotation is made more stable and firm.

[0022] The built-in vacuum chamber 1 can be heated to 25-150°C. Each cavity surface of the built-in vacuum chamber 1 is provided with a plurality of vacuum pipes 7. Each vacuum pipe 7 can be connected to a detachable large-capacity external vacuum chamber 2. The external vacuum chamber 2 is used to vacuum the built-in vacuum chamber 1. The external vacuum chamber 2 is connected to a copper tube cold trap 5 through a first exhaust pipe 6-1. The copper tube cold trap 5 is connected to a molecular pump 4 and a large-volume mechanical pump 3 through a second exhaust pipe 6-2. The molecular pump 4 and the large-volume mechanical pump 7 are connected through a third exhaust pipe 6-3.

[0023] The vacuum pipe 7, the first air extraction pipe 6-1, the second air extraction pipe 6-2 and the third air extraction pipe 6-3 are all provided with solenoid valves, which are used to control the pipe switch. For example, the vacuum pipe 7 is provided with a first solenoid valve 13-1, the first air extraction pipe 6-1 is provided with a second solenoid valve 13-2, the two branch pipes of the second air extraction pipe 6-2 are provided with two third solenoid valves 13-3, and the third air extraction pipe 6-3 is provided with a fourth solenoid valve 13-4. The air intake pipe 7 in this embodiment is connected between the heatable built-in vacuum chamber 1 and the detachable large-capacity external vacuum chamber 2, and the pipe switch is controlled by the solenoid valve.

[0024] Figure 2 Combination Figure 1 The built-in vacuum chamber 1 includes a plurality of built-in vacuum chamber surfaces 14, and a pipeline conversion head 15 is arranged on the periphery of each built-in vacuum chamber surface 14. Preferably, the built-in vacuum chamber 1 is a rectangular parallelepiped structure, and its six chamber surfaces are connected to a detachable large-capacity external vacuum chamber through vacuum pipes, and vacuum extraction is performed from all directions, wherein each chamber surface of the built-in vacuum chamber 1 is designed with a plurality of pipes, and the aperture of each pipe can be adjusted according to the air pressure distribution in the chamber.

[0025] Preferably, each cavity surface of the heatable built-in vacuum cavity 1 is connected to a detachable large-capacity external vacuum cavity 2 through a vacuum pipe 7. The design of the multi-pipeline vacuum cavity allows the built-in vacuum cavity 1 to be vacuum-extracted by various pipes in various directions of the external vacuum cavity 2 at the moment the solenoid valve is opened and the gas connected to the cavity reaches equilibrium, thereby instantly extracting a large amount of volatile solvent from the cavity.

[0026] Each cavity surface of the built-in vacuum chamber 1 is connected to a vacuum pipe 7. Multiple pipe connection ports can be designed on the cavity surface of the built-in vacuum chamber. The pipe connection aperture is adjusted through the pipe conversion head 15 to control the uniformity of the exhaust. In addition, each inner wall is installed with a sand core gas-leveling sheet 8 with a thickness of 10 to 20 mm and an aperture of 100 to 200 um. While ensuring good air permeability, the vaporized solvent is extracted from all directions of the cavity in a uniform, stable and rapid manner. In addition, the heated built-in vacuum chamber 1 has a cooling and heating constant temperature system of 25 to 150°C to ensure that the volatile solvent in the cavity remains in a gaseous state for effective extraction. The other end of the detachable large-capacity external vacuum chamber is connected to a copper tube cold trap through a vacuum pipe, and the other end of the copper tube cold trap is connected to a molecular pump and a large-volume mechanical pump.

[0027] The heating and cooling base 9 provided in the built-in vacuum chamber 1 of the present invention is connected to the bottom of the chamber by a heating column 11 and a rotating shaft 12 to achieve large-angle stable rotation, so as to regulate the volatilization of the solvent in the perovskite film in all directions in the chamber, and improve the extraction and removal speed, stability and uniformity of the volatile solvent. The four sides of the rotatable heating and cooling base 9 extend upward to form a side heating side block 10 connected to the bottom of the base, so as to achieve uniform heating of the sample, and control the volatilization speed of the solvent in the sample film and the purpose of blocking and fixing.

[0028] Furthermore, the six cavity surfaces of the heatable built-in vacuum cavity are all connected by vacuum pipes to a detachable large-capacity external vacuum cavity, and the cavity is vacuumed by multiple pipes from all directions. The aperture of each pipe can be adjusted at the pipe connection as needed to control the uniform vacuum extraction in the cavity. Compared with traditional devices, the extraction efficiency and extraction uniformity of the present invention can be improved by 70% to 90%, so that the vaporized solvent in the built-in vacuum cavity can be extracted more quickly and completely, and the particles in the cavity can be effectively removed, which helps to reduce contamination of the sample.

[0029] Furthermore, the heatable built-in vacuum chamber has a cooling and heating constant temperature function of 25 to 150°C, so as to effectively control the temperature in the chamber according to the required process, and maintain the temperature of each area in the chamber consistent, preventing the vaporized solvent from condensing into liquid due to the ambient temperature difference, thereby contaminating the sample.

[0030] Furthermore, a sand core gas-distributing sheet with a thickness of 10 to 20 mm and an aperture of 100 to 200 um is installed on the inner wall of each direction of the heated built-in vacuum chamber, which can improve the uniformity of gas extraction by 2 to 3 times, optimize the uniform distribution of cavity gas and stably extract the vaporized solvent from all directions of the cavity. The lower gas emission of the sand core material helps to achieve and maintain the vacuum degree of the cavity.

[0031] Furthermore, the heating and cooling base is connected to the bottom of the built-in vacuum chamber through heating columns and heat-conducting rotating shaft supports, which can realize large-angle rotation in all directions and control the temperature range of -20℃ to 150℃, so as to promote the volatilization of the solvent in the perovskite film to all directions in the cavity and improve the extraction and removal speed, stability and uniformity of the volatile solvent.

[0032] As mentioned above, the multi-pipeline cavity vacuum desolventizing flash evaporation system provided by the present invention is applied to the flash vacuum desolventizing process in the perovskite film preparation process, which effectively solves several key problems of the traditional flash vacuum system vacuum desolventizing technology: slow solvent vaporization and extraction rate, poor extraction uniformity and stability, and the vaporized solvent condenses into liquid contaminated samples due to the difference in spatial ambient temperature in the vacuum cavity, resulting in an increase in defects in the perovskite film. This technology achieves a significant improvement in the faster, more comprehensive, more uniform and more stable extraction of solvents in the flash vacuum cavity, as well as the adjustable effect of the temperature inside the cavity and the base, optimizing the working environment and efficiency of the flash evaporation process and improving the quality of perovskite film formation.

[0033] In summary, although the present invention has been disclosed as above in terms of preferred embodiments, the above preferred embodiments are not intended to limit the present invention. A person skilled in the art may make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention shall be based on the scope defined in the claims.

Claims

1. A multi-pipeline chamber vacuum desolventizing flash evaporation system, characterized in that: The invention comprises a heatable built-in vacuum chamber (1), wherein a sand core air-distributing sheet (8) is arranged on the inner wall of the built-in vacuum chamber (1); the built-in vacuum chamber (1) is equipped with a heating and cooling base (9), and the heating and cooling base (9) is supported by a heating column (11) and a rotating shaft (12), and can realize large-angle rotation and control in the temperature range of -20°C to 150°C; The heating and cooling base (9) is connected to a heating side block (10), and the heating side block (10) is used to heat the sample in the built-in vacuum chamber (1) around the sample to achieve uniform heating of the sample and increase the solvent volatilization rate in the sample film. In addition, during the rotation of the heating and cooling base (9), the sample can rotate more stably and firmly. The built-in vacuum chamber (1) can be heated to 25-150° C. Each cavity surface of the built-in vacuum chamber (1) is provided with a plurality of vacuum pipes (7), each of which can be connected to a detachable large-capacity external vacuum chamber (2), and the external vacuum chamber (2) is used to extract vacuum from the built-in vacuum chamber (1); the external vacuum chamber (2) is connected to a copper tube cold trap (5) via a first exhaust pipe (6-1), the copper tube cold trap (5) is connected to a molecular pump (4) and a large-volume mechanical pump (3) via a second exhaust pipe (6-2), and the molecular pump (4) and the large-volume mechanical pump (7) are connected via a third exhaust pipe (6-3).

2. A multi-pipeline chamber vacuum desolventizing flash evaporation system according to claim 1, characterized in that: The vacuum pipe (7) is provided with a first solenoid valve (13-1), the first air extraction pipe (6-1) is provided with a second solenoid valve (13-2), two branch pipes of the second air extraction pipe (6-2) are provided with two third solenoid valves (13-3), and the third air extraction pipe (6-3) is provided with a fourth solenoid valve (13-4).

3. A multi-pipeline chamber vacuum desolventizing flash evaporation system according to claim 1, characterized in that: The built-in vacuum chamber (1) comprises a plurality of built-in vacuum chamber surfaces (14), and a pipeline conversion head (15) is arranged on the periphery of each built-in vacuum chamber surface (14).

4. A multi-pipeline chamber vacuum desolventizing flash evaporation system according to claim 1, characterized in that: The built-in vacuum chamber (1) is a rectangular parallelepiped structure, and its six chamber surfaces are connected to a detachable large-capacity external vacuum chamber via vacuum pipes, so that vacuum extraction can be performed from all directions, wherein the multiple pipes designed on each chamber surface of the built-in vacuum chamber (1) can adjust the aperture according to the air pressure distribution in the chamber.

5. The multi-pipeline chamber vacuum desolventizing flash evaporation system according to claim 1, characterized in that: The thickness of the sand core air-distributing sheet (8) is 10 to 20 mm, and the pore size is 100 to 200 um.

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