Perovskite precursor solution preparation device

Abstract

The utility model discloses a perovskite precursor solution preparation device, which comprises a reaction system, a stirring system, a heating system, a vacuum system and a control system, and the control system is used for setting and adjusting related parameters in the preparation process of a perovskite precursor solution so as to realize accurate control on conditions such as stirring speed and direction, heating temperature, vacuum degree and the like. The perovskite precursor solution preparation device can uniformly and efficiently mix and stir a solution according to precursor materials and solvents of different types and different doses, reduce pollution of air impurities to the solution, remove tiny bubbles in the solution, and obtain a stable perovskite precursor solution.

Description

TECHNICAL FIELD

[0001] The utility model relates to perovskite precursor material processing equipment technical field, concretely is perovskite precursor solution preparation device. BACKGROUND

[0002] Perovskite material has the advantages such as high light absorption coefficient, adjustable energy level, high mobility and low cost, and in the perovskite-based optoelectronic devices such as solar cells and photodetectors, the functional layer usually selects methylammonium iodine-based perovskite (MAPbI3), formamidinium iodine-based perovskite (FAPbI3) and other organic-inorganic hybrid metal halide perovskite thin films.

[0003] The solution deposition preparation technology of organic-inorganic hybrid metal halide perovskite thin film includes the steps of precursor solution preparation, thin film deposition and annealing, and in the perovskite precursor solution preparation process, the appropriate precursor material needs to be dissolved in the suitable solvent, and the precursor material and the solvent are fully fused to form a uniform solution by stirring, but the following problems need to be paid attention to in the solution stirring process: 1. The stirring speed will affect the uniformity of perovskite precursor material in the solvent, and proper stirring speed can reduce the collision and aggregation between the precursor materials and avoid the generation of precipitate; 2. The solution temperature will affect the solubility of perovskite precursor material in the solvent, and proper heating of the solution can improve the dissolution rate of the precursor material; 3. Impurities (such as oxygen, water vapor, etc.) in the air will mix into the solution, and chemical reaction will occur to change the chemical composition of the perovskite precursor solution; 4. Air bubbles will be introduced during stirring, resulting in different solution concentrations in different areas and affecting the stability of the perovskite precursor solution. SUMMARY

[0004] The utility model aims at providing perovskite precursor solution preparation device to accurately control the stirring speed and direction, solution temperature, vacuum environment and other conditions in the preparation process of perovskite precursor solution.

[0005] The perovskite precursor solution preparation device comprises a reaction system (1), a stirring system (2), a heating system (3), a vacuum system (4), and a control system (5). The reaction system (1) comprises a vacuum chamber cover plate (11), a sealing gasket (12), a vacuum chamber shell (13), a spring connecting rod (14), a solution tank cover plate (15), and a solution tank (16). The stirring system (2) comprises a motor (21), a rotating rod (22), a first stirring rod (23), and a second stirring rod (24). The heating system (3) comprises a heating tank (31), a heater (32), a heating wire (33), a first temperature sensor (34), a second temperature sensor (35), and a third temperature sensor (36). The vacuum system (4) comprises a first electromagnetic valve (41), a second electromagnetic valve (42), a vacuum unit (43), a vacuum sensor (44), and a vacuum gauge (45). The control system (5) comprises a logic controller (51) and a temperature controller (52).

[0006] Further, the sealing gasket (12) is arranged between the vacuum chamber cover plate (11) and the vacuum chamber shell (13) and is fastened and sealed by bolts. The vacuum chamber cover plate (11) and the solution tank cover plate (15) are connected by the spring connecting rod (14). The spring connecting rod (14) is telescopic and used to adjust the distance between the vacuum chamber cover plate (11) and the solution tank cover plate (15).

[0007] Further, the motor (21) is fixed below the vacuum chamber cover plate (11) and located inside the cavity formed by the vacuum chamber cover plate (11) and the vacuum chamber shell (13).

[0008] Further, the rotating shaft of the motor (21) is connected to the rotating rod (22), and the rotating rod (22) is connected to the first stirring rod (23) and the second stirring rod (24). The first stirring rod (23) and the second stirring rod (24) are different in size and located at different positions of the rotating rod (22). The rotating shaft of the motor (21) drives the rotating rod (22), the first stirring rod (23), and the second stirring rod (24) to rotate, thereby stirring the solution.

[0009] Further, the heating tank (31) is fixed to the bottom of the vacuum chamber shell (13), and the solution tank (16) is embedded in the heating tank (31). The heating tank (31) and the solution tank (16) are made of materials with good high-temperature resistance and heat transfer. Preferably, the heating tank (31) is made of stainless steel, and the solution tank (16) is made of a crucible.

[0010] Further, the heating groove (31) is internally provided with a heater (32), a heating wire (33), a first temperature sensor (34), a second temperature sensor (35) and a third temperature sensor (36), and the first temperature sensor (34), the second temperature sensor (35) and the third temperature sensor (36) are distributed at different positions in the heating groove (31). The heater (32) and the heating wire (33) are used for heating the heating groove (31) and improving the temperature of the solution groove (16) and the solution through heat transfer and the like. The first temperature sensor (34), the second temperature sensor (35) and the third temperature sensor (36) are used for measuring the heating temperature and detecting the uniformity of the temperature.

[0011] Further, the cavity formed by the vacuum chamber cover plate (11) and the vacuum chamber shell (13) is communicated with a vacuum unit (43) through a first electromagnetic valve (41) and communicated with external air through a second electromagnetic valve (42) through a pipeline, so as to adjust the vacuum degree in the cavity.

[0012] Further, the cavity formed by the vacuum chamber cover plate (11) and the vacuum chamber shell (13) is internally provided with a vacuum sensor (44), and the vacuum sensor (44) is connected with a vacuum gauge (45) outside the cavity through a wire, so as to measure and display the vacuum degree in the cavity.

[0013] Further, the logic controller (51) is connected with the motor (21), the first electromagnetic valve (41) and the second electromagnetic valve (42) through wires, so as to control the rotating speed and direction of the motor (21) and the opening and closing state of the first electromagnetic valve (41) and the second electromagnetic valve (42).

[0014] Further, the temperature controller (52) is connected with the heater (32), the first temperature sensor (34), the second temperature sensor (35) and the third temperature sensor (36) through wires, so as to control the heating state and collect the heating temperatures at different positions.

[0015] The beneficial effects of the utility model are as follows.

[0016] 1. According to different perovskite precursor materials and solvents, the speed and direction of stirring are accurately adjusted, in addition, the rotating rod, the first stirring rod and the second stirring rod structure are adopted, so that the solution in the solution groove rotates at the same time, and uniform stirring of the solution is ensured.

[0017] 2. The solution can be heated to improve the dissolution rate of the perovskite precursor material in the solvent, which is beneficial to improve the preparation efficiency of the solution.

[0018] 3. The solution can be prepared in a vacuum environment to reduce the pollution of impurities in the air to the solution and remove the tiny bubbles in the solution, which is beneficial to prepare a uniform and stable perovskite precursor solution. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 Is the perovskite precursor solution preparation device structure schematic view.

[0020] Reference signs:

[0021] Vacuum chamber cover plate (11), sealing gasket (12), vacuum chamber shell (13), spring connecting rod (14), solution tank cover plate (15), solution tank (16);

[0022] Motor (21), rotating rod (22), first stirring rod (23), second stirring rod (24);

[0023] Heating tank (31), heater (32), heating wire (33), first temperature sensor (34), second temperature sensor (35), third temperature sensor (36);

[0024] First solenoid valve (41), second solenoid valve (42), vacuum unit (43), vacuum sensor (44), vacuum gauge (45);

[0025] Logic controller (51), temperature controller (52). DETAILED DESCRIPTION

[0026] In order to make the technical scheme, design purpose and beneficial effects of the utility model more clear, the utility model is further described in detail below in combination with the drawings and examples. It should be understood that the specific examples described herein are only used to explain the utility model and are not used to limit the utility model.

[0027] It should be noted that if the terms indicating the orientation or position relationship such as "lower", "inner" and "bottom" appear, they are only based on the position relationship shown in the drawings for the convenience of describing the utility model, and are not specific orientations or positions that the described devices must have. It cannot be understood as a limitation on the utility model. The terms "first", "second" and the like are only used to distinguish different structures or devices, and cannot be understood as a description of relative importance. EXAMPLE

[0028] The perovskite precursor solution preparation device comprises a vacuum chamber cover plate (11), a sealing gasket (12), a vacuum chamber shell (13), a spring connecting rod (14), a solution tank cover plate (15), a solution tank (16), a motor (21), a rotating rod (22), a first stirring rod (23), a second stirring rod (24), a heating tank (31), a heater (32), a heating wire (33), a first temperature sensor (34), a second temperature sensor (35), a third temperature sensor (36), a first electromagnetic valve (41), a second electromagnetic valve (42), a vacuum unit (43), a vacuum sensor (44), a vacuum gauge (45), a logic controller (51), and a temperature controller (52).

[0029] The perovskite precursor solution preparation steps using the above device comprise:

[0030] S1: Check the integrity and sealing of the device, and clean and disinfect the device to ensure no contamination;

[0031] S2: Mix the perovskite precursor material and solvent according to the required ratio, and pour them into the solution tank (16);

[0032] S3: Cover the vacuum chamber cover plate (11) and the solution tank cover plate (15), and place the sealing gasket (12) between the vacuum chamber cover plate (11) and the vacuum chamber shell (13), and tighten the vacuum chamber cover plate (11) and the vacuum chamber shell (13) with bolts;

[0033] S4: Start the vacuum unit (43), and open the first electromagnetic valve (41) through the logic controller (51);

[0034] S5: Observe the data displayed by the vacuum gauge (45), and after the vacuum degree meets the standard, set the working parameters of the motor (21) and start it through the logic controller (51), set the heating temperature through the temperature controller (52) and start the heater (32);

[0035] S6: Observe the vacuum degree and temperature values displayed by the vacuum gauge (45) and the temperature controller (52) during stirring to ensure normal operation of the device;

[0036] S7: After the stirring work is completed, turn off the heater (32) through the temperature controller (52);

[0037] S8: Observe the data displayed by the temperature controller (52), and after the temperature drops to room temperature, close the first electromagnetic valve (41) and open the second electromagnetic valve (42) through the logic controller (51);

[0038] S9: Observe the data displayed by the vacuum gauge (45), and after the internal and external air pressures of the reaction system (1) are the same, close the motor (21) and the second electromagnetic valve (42) through the logic controller (51).

[0039] S10: Loosen the bolts and open the vacuum chamber cover plate (11), take out the mixed perovskite precursor solution. Embodiments

[0040] The heating tank (31) is provided with a first temperature sensor (34), a second temperature sensor (35) and a third temperature sensor (36) for measuring the temperatures at different positions of the heating tank (31). During the operation of the device, the temperature difference threshold values of the different sensors can be set. If the temperature measurement result exceeds the threshold value, it indicates that the heating effect of the heating system (3) is uneven, and the heater (32) and the heating wire (33) need to be replaced or other maintenance treatments are needed.

[0041] The above embodiments are only optional embodiments of the present application, and do not limit the present application. Based on the inspiration of the present application, those skilled in the art can make many forms of optimization and adjustment without departing from the purpose of the present application and the scope protected by the claims, which are all within the protection scope of the present application.

Claims

1. A perovskite precursor solution preparation apparatus, characterized in that: It includes a reaction system (1), a stirring system (2), a heating system (3), a vacuum system (4), and a control system (5); The reaction system (1) includes a vacuum chamber cover plate (11), a sealing gasket (12), a vacuum chamber shell (13), a spring connecting rod (14), a solution tank cover plate (15), and a solution tank (16). The stirring system (2) includes a motor (21), a rotating rod (22), a first stirring rod (23), and a second stirring rod (24). The heating system (3) includes a heating tank (31), a heater (32), a heating wire (33), a first temperature sensor (34), a second temperature sensor (35), and a third temperature sensor (36). The vacuum system (4) includes a first solenoid valve (41), a second solenoid valve (42), a vacuum unit (43), a vacuum sensor (44), and a vacuum gauge (45). The control system (5) includes a logic controller (51) and a temperature controller (52).

2. The perovskite precursor solution preparation apparatus according to claim 1, characterized in that: A sealing gasket (12) is placed between the vacuum chamber cover plate (11) and the vacuum chamber shell (13) and the seal is secured by bolts. The vacuum chamber cover plate (11) and the solution tank cover plate (15) are connected by a spring connecting rod (14).

3. The perovskite precursor solution preparation apparatus according to claim 1, characterized in that: The motor (21) is fixed below the vacuum chamber cover (11) and is located inside the cavity formed by the vacuum chamber cover (11) and the vacuum chamber shell (13).

4. The perovskite precursor solution preparation apparatus according to claim 1, characterized in that: The rotating shaft of the motor (21) is connected to the rotating rod (22), and the rotating rod (22) is connected to the first stirring rod (23) and the second stirring rod (24).

5. The perovskite precursor solution preparation apparatus according to claim 1, characterized in that: The heating tank (31) is fixed to the bottom of the vacuum chamber shell (13), and the solution tank (16) is embedded in the heating tank (31). The heating tank (31) and the solution tank (16) are made of materials with high temperature resistance and good heat transfer properties.

6. The perovskite precursor solution preparation apparatus according to claim 1, characterized in that: The heating tank (31) is equipped with a heater (32), a heating wire (33), a first temperature sensor (34), a second temperature sensor (35), and a third temperature sensor (36), and the first temperature sensor (34), the second temperature sensor (35), and the third temperature sensor (36) are distributed in different positions within the heating tank (31).

7. The perovskite precursor solution preparation apparatus according to claim 1, characterized in that: The cavity formed by the vacuum chamber cover (11) and the vacuum chamber shell (13) is connected to the vacuum unit (43) through a pipe via the first solenoid valve (41) and to the outside air via the second solenoid valve (42).

8. The perovskite precursor solution preparation apparatus according to claim 1, characterized in that: A vacuum sensor (44) is installed inside the cavity formed by the vacuum chamber cover (11) and the vacuum chamber shell (13). The measurement results of the vacuum sensor (44) are displayed by a vacuum gauge (45) outside the cavity.

9. The perovskite precursor solution preparation apparatus according to claim 1, characterized in that: The logic controller (51) is used to control the speed and direction of the motor (21) and the opening and closing states of the first solenoid valve (41) and the second solenoid valve (42).

10. The perovskite precursor solution preparation apparatus according to claim 1, characterized in that: The temperature controller (52) controls the heating state through the heater (32) and the heating temperature at different locations is collected by the first temperature sensor (34), the second temperature sensor (35), and the third temperature sensor (36).

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