Air exhaust crystallizer equipment

Abstract

The invention discloses air exhaust crystallizer equipment, which relates to the field of perovskite thin film preparation and comprises a crystallization film-forming main machine, a vacuum pump assembly and a vacuum pipeline assembly used for communicating the crystallization film-forming main machine with the vacuum pump assembly, the crystallization film-forming main machine comprises a main machine mechanical assembly and an air exhaust crystallization control system; the main machine mechanical assembly comprises a shell assembly, a main machine cavity, a rotary pressing carrying table assembly, a sealing piece, a cavity switch valve assembly, a vacuum breaking assembly, a main machine pipeline assembly, a start-stop button, a switch assembly and an air outlet connector. The air exhaust crystallization control system comprises a control assembly, a sensor assembly and an execution unit. According to the invention, the uniformity of crystallization and film formation is ensured through the combined action of chamber flow channel structure design, air exhaust process control, pressure regulation and environmental atmosphere control, and perovskite solutions with different formulas are adapted, so that the quality of a perovskite film layer is greatly improved, and the problems of poor uniformity and many defects of perovskite film crystallization are fundamentally solved.

Description

Technical Field

[0001] The present invention relates to the field of perovskite film preparation, and in particular to a vacuum crystallizer device. Background Art

[0002] Perovskite halide solar cells belong to the third generation of solar cells. Single-cell / stacked solar cells have high photoelectric conversion efficiency and are developing at an extremely high growth rate, attracting widespread attention from the market. However, the uneven film layer and many defects in the film crystallization process of perovskite solar cells lead to large resistance loss and decreased light absorption rate, which in turn causes poor battery stability, which is a pain point in the current industry. Therefore, it is of great significance to develop a high-density, low-defect film crystallization equipment. Summary of the Invention

[0003] In order to solve the above problems, the purpose of the present invention is to provide a vacuum crystallizer device, which is used to solve the pain points of uneven film layer and many defects in the film formation and crystallization process of current perovskite solar cells. The vacuum crystallizer device can solve the problems of uneven film layer and many defects in the preparation process of perovskite solar cells.

[0004] In order to achieve the above technical objectives, the present application provides a vacuum crystallizer device, comprising: A crystallization film forming main unit, a vacuum pump assembly, and a vacuum pipe assembly for connecting the crystallization film forming main unit and the vacuum pump assembly; Crystallization film forming host, including host mechanical components and vacuum crystallization control system; The main machine mechanical components include the shell assembly, main machine cavity, rotary pressing platform assembly, seal, cavity switch valve assembly, air breaking assembly, main machine pipeline assembly, start-stop button, switch assembly, and air outlet interface; The vacuum crystallization control system includes a control component, a sensor component, and an execution unit.

[0005] The vacuum pipeline assembly includes a vacuum pipeline and a dynamic pressure regulating assembly.

[0006] Preferably, the control component includes an operation component, a data integration unit, an abnormality alarm unit, and an emergency stop component; wherein the sensor component includes a first sensor, a second sensor, and a third sensor.

[0007] Preferably, the operating component has an input interface for pressure value, holding time, temperature value, heating rate, and air-breaking time, and has a module or program for achieving real-time control of vacuum crystallization parameters; The data integration unit has a module or program that can collect actual data of gas extraction crystallization, compare the actual data with preset parameters and transmit the information to the execution unit according to the comparison result, and form a data curve with the feedback data.

[0008] Preferably, the first sensor monitors the air extraction rate in real time and transmits the data to the data integration unit; The second sensor monitors the local pressure and the overall pressure in the cavity in real time and transmits the pressure data to the data integration unit; The third sensor monitors the exhaust humidity, temperature, and crystallization state in real time, and transmits the data to the data integration unit, and adjusts the exhaust parameters based on the feedback information and the data of the data integration unit.

[0009] Preferably, the rotary pressing stage assembly comprises a rotary pressing drive mechanism, a rotary arm, a support assembly and a stage; The rotary pressing stage assembly and the main body cavity can achieve self-adaptive sealing pressing.

[0010] Preferably, a lofting area can be provided on the mating surface of the carrier and the main body cavity, and the lofting area is sunken by no less than 0.5 mm compared to the outer periphery of the carrier; The carrier can also be provided with a clamping sampling groove, which is sunken by no less than 1mm compared to the outer periphery of the carrier; The carrier can also be provided with an air extraction channel, through which the sample is adsorbed and fixed on the carrier sample area; The platform can achieve temperature increase and decrease, temperature preservation and temperature change through regulation.

[0011] Preferably, the main body cavity and the carrier matching end cavity are a rotational body structure, or a centrally symmetrical structure.

[0012] Preferably, the rotary and compacting driving mechanism may be a rotating and compacting integrated structure, and the rotating and compacting moving paths may be smooth curves.

[0013] Preferably, the support assembly is a flexible and adaptive support assembly, wherein the support screw has a structure that is thin in the middle and thick at both ends, with an arc transition, and the ratio of the cross-sectional area of ​​the smaller end of the support screw to the cross-sectional area of ​​the middle region is not less than 1.5; When the support screw is subjected to vertical pressure from the rotary pressing drive mechanism, the support screw pushes the carrier to press the surface to be bonded, and according to the bonding area, the middle section of the support screw is tilted, with an inclination angle of 0-45° in the circumferential direction.

[0014] The present invention discloses the following technical effects: Compared with conventional film-forming equipment, the vacuum crystallization equipment provided by the present invention ensures uniform crystallization through chamber flow channel structure design, vacuum process control, pressure regulation, and environmental atmosphere control, and is adaptable to perovskite solutions of different formulas. Therefore, it greatly improves the quality of the perovskite film layer and fundamentally solves the problem of poor uniformity and many defects in perovskite film crystallization. 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 following briefly introduces the drawings required for use in the embodiments. 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 these drawings without paying any creative work.

[0016] Figure 1 Schematic diagram of a vacuum crystallizer device provided in an embodiment of the present invention; Figure 2 Schematic diagram of a vacuum crystallization control system provided by an embodiment of the present invention; Figure 3 It is a schematic diagram of the flexible support screw of the present invention. DETAILED DESCRIPTION

[0017] In order to make the purpose, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. The components of the embodiments of the present application generally described and shown in the drawings here can be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present application provided in the drawings is not intended to limit the scope of the application for protection, but merely represents the selected embodiments of the present application. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without making creative work are within the scope of protection of this application.

[0018] The present invention discloses a vacuum crystallizer device, comprising a crystallization film forming host 1, a vacuum pipeline component 2, and a vacuum pump component 3; The vacuum crystallizer can realize parameter adjustment, environmental control and crystallization film formation through the cooperation of the main machine mechanical component 11 of the crystallization film forming main machine 1 and the vacuum crystallization control system 12; The crystallization film forming host 1 and the vacuum pump assembly 3 are connected through the vacuum pipeline assembly 2, and the vacuum pipeline assembly 2 includes a vacuum pipeline 21 and a dynamic pressure regulating assembly 22; The main engine mechanical assembly 11 includes a housing assembly 11-1, a main engine cavity 11-2, a rotary pressing platform assembly 11-3, a seal 11-4, a cavity switch valve assembly 11-5, a piercing assembly 11-6, a main engine pipeline assembly 11-7, a start / stop button 11-8, a switch assembly 11-9, and an air outlet interface 11-10; the main engine mechanical assembly 11 can realize self-adaptive sealing and pressing between the rotary pressing platform assembly 11-3 and the main engine cavity 11-2; The rotary pressing platform assembly 11-3 includes a rotary pressing drive mechanism, a rotating arm, a support assembly, and a platform, wherein the platform can achieve temperature increase and decrease, heat preservation, and temperature change through regulation.

[0019] The vacuum crystallization control system 12 designed by the present invention includes a control component 12-1, a sensor component, and an execution unit; wherein the control component includes an operation component, a data integration unit, an abnormality alarm unit, and an emergency stop component; wherein the sensor component includes a first sensor, a second sensor, and a third sensor; The operating component can input pressure, holding time, temperature, heating rate, and air-breaking time as needed to achieve real-time adjustment of vacuum crystallization parameters; The data integration unit collects the actual data of gas extraction crystallization, and compares the actual data with the preset adjustment parameters. According to the comparison results, the information is transmitted to the execution unit. The data integration unit can form a data curve for the feedback data. The abnormal alarm unit displays abnormal information according to the state of vacuum crystallization, when the system does not work, components are damaged, or the working environment does not match, and transmits the abnormal information to the operation component; The emergency stop component can achieve emergency stop when an abnormal state occurs; The first sensor monitors the pumping rate in real time and transmits the data to the data integration unit; The second sensor monitors the local pressure and the overall pressure in the cavity in real time and transmits the pressure data to the data integration unit; The third sensor monitors the exhaust humidity, temperature, and crystallization state in real time, and transmits the data to the data integration unit. The exhaust parameters are adjusted based on the feedback information and the data from the data integration unit. The execution unit is used to implement the input parameters of the control component.

[0020] The mating surface of the carrier designed in the present invention and the main body cavity 11-2 can be provided with a sample arrangement area, and the position of the sample arrangement area is sunken by no less than 0.5 mm compared with the outer periphery of the carrier; the carrier is provided with a clamping sampling groove, and the clamping sampling groove is sunken by no less than 1 mm compared with the outer periphery of the carrier; the carrier can also be provided with an exhaust air channel, and the sample is adsorbed and fixed in the sample arrangement area of ​​the carrier by exhausting air.

[0021] The main body cavity 11 and the carrier 12 designed in the present invention have a matching end cavity that is a rotational structure or a centrally symmetrical structure.

[0022] The vacuum crystallization control system 12 designed in the present invention is arranged inside the housing component 11 - 1 to realize data transmission and operation control of the vacuum crystallization equipment.

[0023] The present invention provides a perovskite film vacuum crystallization device and method. The vacuum crystallization device can achieve vacuum crystallization through the following steps: Connect the air outlet port 11-10 to the pump port and turn on the pump switch; Open the switch assembly 11-9; Remove the rotating pressing stage assembly 11-3, place the sample on the stage, move the stage in, and press the stage tightly; Set the input parameters through the vacuum crystallization control system 12, set the vacuum time, pressure value, and air-breaking time and click the confirmation box; The first sensor is distributed inside the chamber and at the outlet of the air evacuation channel to monitor the air evacuation rate; the second sensor is distributed around the chamber and at the air outlet; the third sensor is evenly distributed inside the chamber.

[0024] The preset adjustment parameters stored in the data integration unit designed by the present invention are a result based on mathematical modeling formulas, complete databases, and big data algorithm fitting.

[0025] The execution unit designed in the present invention drives and adjusts the pump port exhaust rate, chamber heating temperature, and chamber heating and cooling rates.

[0026] The rotary pressing drive mechanism designed in the present invention is a rotating and pressing integrated structure, and the rotating and pressing moving paths are smooth curves.

[0027] The support assembly designed in the present invention is a flexible and adaptive support assembly, in which the support screw has a structure that is thin in the middle and thick at both ends, with an arc transition. The ratio of the cross-sectional area of ​​the smaller end of the support screw to the cross-sectional area of ​​the middle area is not less than 1.5.

[0028] When the support screw designed in the present invention is subjected to vertical pressure from the rotary pressing drive mechanism, the support screw pushes the carrier to press the bonded surface, and according to the bonding area, the middle section of the support screw is tilted, with an inclination angle of 0-45° in the circumferential direction.

[0029] Example: Figure 1-Figure 3 As shown, the present invention provides a vacuum crystallizer device, including a crystallization film forming host 1, a vacuum pipeline assembly 2, and a vacuum pump assembly 3; the vacuum crystallizer can achieve parameter adjustment, environmental control, and crystallization film formation through the coordinated cooperation of the film forming host 1 mechanical assembly 11 and the vacuum crystallization control system 12; the film forming host 1 and the vacuum pump assembly 3 are connected through the vacuum pipeline assembly 2, and the vacuum pipeline assembly 2 includes a vacuum pipeline 21 and a dynamic pressure regulating valve 22; In this technical solution, the main machine mechanical component 11 (including 11-1 to 11-10) includes a shell component 11-1, a main machine cavity 11-2, a rotary pressing platform component 11-3, a seal 11-4, a cavity switch valve component 11-5, a breaking component 11-6, a main machine pipeline component 11-7, a start-stop button 11-8, a switch component 11-9, and an air outlet interface 11-10; the main machine mechanical component 11 can realize the self-adaptive sealing and pressing of the rotary pressing platform component 11-3 and the main machine cavity 11-2 to form a closed chamber; the rotary pressing platform component 11-3 includes a rotary pressing drive mechanism, a rotating arm, a support component, and a platform, wherein the platform can realize temperature rise and fall, heat preservation, and temperature change by operating the vacuum crystallization control system 12.

[0030] In the present invention, the gas extraction crystallization control system 12 includes a control component 12-1, a sensor component, and an execution unit; wherein the control component includes an operation component, a data integration unit, an abnormality alarm unit, and an emergency stop component; wherein the sensor component includes a first sensor, a second sensor, and a third sensor; The operating component can input pressure, holding time, temperature, heating rate, and air-breaking time as needed to achieve real-time adjustment of the pumping crystallization parameters; the data integration unit collects the actual data of the pumping crystallization and compares the actual data with the preset adjustment parameters. Based on the comparison results, the information is transmitted to the execution unit. The data integration unit can generate a data curve for the feedback data. In the present invention, the abnormal alarm unit feeds back fault information according to the state of vacuum crystallization. When the system does not work, components are damaged, or the working environment does not match, the abnormal alarm unit displays abnormal information and transmits the abnormal information to the operating component; the emergency stop component can realize emergency stop when an abnormal state occurs; The first sensor monitors the exhaust rate in real time and transmits the data to the data integration unit; the second sensor monitors the local pressure and the overall pressure in the cavity in real time and transmits the pressure data to the data integration unit; the third sensor monitors the exhaust humidity, temperature, and crystallization state in real time and transmits the data to the data integration unit, and adjusts the exhaust parameters according to the feedback information and the data of the data integration unit; the exhaust crystallization control system 12 is arranged inside the shell assembly 11-1 to realize the data transmission and operation control of the exhaust crystallization equipment.

[0031] The execution unit is used to implement the input parameters of the control component.

[0032] Further preferably, in the present invention, a lofting area can be set on the mating surface of the carrier and the main body cavity 11-2, and the position of the lofting area is sunken by not less than 0.5mm compared with the outer periphery of the carrier. Further, the position of the lofting area is sunken by 1mm compared with the outer periphery of the carrier; the carrier is provided with a clamping sampling groove, and the clamping sampling groove is sunken by not less than 1mm compared with the outer periphery of the carrier. Further, the clamping sampling groove is sunken by 1.5mm compared with the outer periphery of the carrier; the carrier is provided with an exhaust air duct, and the sample is adsorbed and fixed in the lofting area of ​​the carrier by exhausting air.

[0033] Further preferably, the main body cavity 11 - 2 and the carrier matching end cavity are a rotational body structure, and the rotational cross-sectional profile is a smooth quadratic function curve.

[0034] Further preferably, the vacuum crystallization equipment can achieve vacuum crystallization through the following steps: Before crystallization operation, connect the air outlet interface 11-10 to the pump interface and turn on the pump switch; Open the switch assembly 11-9; Remove the rotary pressing stage assembly 11-3, place the sample on the stage, and move the stage in so that the stage presses the chamber tightly; Set the input parameters through the vacuum crystallization control system 12, set the vacuum time, pressure, and air-breaking time, and click the confirmation box to start crystallization; Further preferably, in the present invention, the first sensor is distributed inside the chamber, at the outlet of the exhaust duct, for monitoring the exhaust rate; the second sensor is distributed around the chamber, at the outlet; and the third sensor is evenly distributed inside the chamber.

[0035] Further preferably, the preset adjustment parameters stored in the data integration unit of the present invention are based on the results of mathematical modeling formulas.

[0036] In the present invention, the execution unit adjusts the pumping rate of the pump port, the chamber heating temperature, and the chamber heating and cooling rates by driving the dynamic speed control valve.

[0037] In the present invention, the rotary pressing drive mechanism may be a rotating and pressing integrated structure, and the rotating and pressing moving path is rotating, rising, and then pressing.

[0038] In an embodiment of the present invention, preferably, the support assembly is a flexible adaptive support assembly, wherein the support screw is thin in the middle and thick at both ends, with an arc transition structure, and the ratio of the cross-sectional area of ​​the smaller end of the support screw to the cross-sectional area of ​​the middle area is not less than 1.5. Furthermore, the ratio of the cross-sectional area of ​​the smaller end of the support screw to the cross-sectional area of ​​the middle area is 2.

[0039] Preferably, when the support screw is subjected to vertical pressure from the rotary pressing drive mechanism, the support screw pushes the carrier to press the surface to be bonded, and according to the bonding area, the middle area of ​​the support screw is tilted, and the tilt angle is 0-45° in the circumferential direction. Furthermore, the tilt angle is approximately 5°±1° in the circumferential direction.

[0040] Compared with conventional film-forming equipment, the vacuum crystallization equipment provided by the present invention ensures uniform crystallization through chamber flow channel structure design, vacuum process control, pressure regulation, and environmental atmosphere control, and is adaptable to perovskite solutions of different formulas. Therefore, it greatly improves the quality of the perovskite film layer and fundamentally solves the problem of poor uniformity and many defects in perovskite film crystallization.

[0041] In the description of the present invention, it should be understood that the terms "first" and "second" are used for descriptive purposes only and should not be understood to indicate or imply relative importance or implicitly specify the number of the technical features indicated. Therefore, a feature specified as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, "plurality" means two or more, unless otherwise specifically defined.

[0042] Obviously, those skilled in the art may make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if such changes and modifications fall within the scope of the claims and their equivalents, the present invention is intended to include such changes and modifications.

Claims

1. A vacuum crystallizer device, characterized in that: include: A crystallization film forming main unit (1), a vacuum pump assembly (3), and a vacuum pipeline assembly (2) for connecting the crystallization film forming main unit (1) and the vacuum pump assembly (3); The crystallization film forming host (1) comprises a host mechanical component (11) and a vacuum crystallization control system (12); The host mechanical assembly (11) includes a housing assembly (11-1), a host cavity (11-2), a rotary pressing platform assembly (11-3), a sealing member (11-4), a cavity switch valve assembly (11-5), a piercing assembly (11-6), a host pipeline assembly (11-7), a start / stop button (11-8), a switch assembly (11-9), and an air outlet interface (11-10); The vacuum crystallization control system (12) comprises a control component (12-1), a sensor component, and an execution unit; The vacuum pipeline assembly (2) comprises a vacuum pipeline (21) and a dynamic pressure regulating assembly (22).

2. The vacuum crystallizer device according to claim 1, characterized in that: The control component (12-1) includes an operating component, a data integration unit, an abnormality alarm unit, and an emergency stop component; wherein the sensor component includes a first sensor, a second sensor, and a third sensor.

3. The vacuum crystallizer device according to claim 1, characterized in that: The operating component has an input interface for pressure value, holding time, temperature value, heating rate, and air-breaking time, and has a module or program for achieving real-time control of vacuum crystallization parameters; The data integration unit has a module or program that can collect actual data of gas extraction crystallization, compare the actual data with preset parameters and transmit the information to the execution unit according to the comparison result, and form a data curve with the feedback data.

4. A vacuum crystallizer device according to claims 1-3, characterized in that: The first sensor is a sensor capable of monitoring the pumping rate in real time and transmitting the data to the data integration unit; The second sensor is a sensor capable of monitoring the local pressure and the overall pressure in the cavity in real time and transmitting the pressure data to the data integration unit; The third sensor is a sensor that monitors the exhaust humidity, temperature, and crystallization state in real time and transmits data to the data integration unit. Based on the data of the sensor, the exhaust crystallizer equipment adjusts the exhaust parameters according to the feedback information and combined with the data of the data integration unit.

5. The vacuum crystallizer device according to claim 1, characterized in that: The rotary pressing platform assembly (11-3) comprises a rotary pressing drive mechanism, a rotary arm, a support assembly and a platform; The rotary pressing platform assembly (11-3) and the main machine cavity (11-2) can achieve self-adaptive sealing pressing.

6. A vacuum crystallizer device according to claims 1-5, characterized in that: The mating surface between the carrier and the main body cavity (11-2) is provided with a lofting area, and the position of the lofting area is sunken by not less than 0.5 mm compared with the outer periphery of the carrier; The carrier is provided with a clamping sampling groove, and the clamping sampling groove is sunken by no less than 1 mm compared with the outer periphery of the carrier; The carrier is provided with an air extraction channel, through which the sample is adsorbed and fixed on the carrier sample placement area; The carrier has a module or program for achieving temperature rise and fall, temperature preservation, and temperature change through regulation.

7. A vacuum crystallizer device according to claims 1-6, characterized in that: The main body cavity (11-2) and the carrier matching end cavity are a rotational structure, or a centrally symmetrical structure.

8. A vacuum crystallizer device according to claims 1-7, characterized in that: The rotation and pressing driving mechanism is a rotation and pressing integrated structure, and the rotation and pressing moving path is a smooth curve.

9. The vacuum crystallizer device according to claims 1-8, characterized in that: The support assembly is a flexible and adaptive support assembly, wherein the support screw has a structure that is thin in the middle and thick at both ends, with an arc transition, and the ratio of the cross-sectional area of ​​the smaller end of the support screw to the cross-sectional area of ​​the middle section is not less than 1.5; When the support screw is subjected to vertical pressure from the rotary pressing drive mechanism, the support screw pushes the carrier to press the surface to be bonded, and according to the bonding area, the middle section of the support screw is tilted, and the tilt angle is 0-45° in the circumferential direction.

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