A growing device for methylammonium lead bromide crystals

Abstract

The application discloses a methylamine lead bromide crystal growth device and belongs to the technical field of crystal growth. The methylamine lead bromide crystal growth device comprises a growth device, a heat preservation device, a circulating filtration device and a control device. The growth device comprises a growth tank and a crystal carrier arranged in the growth tank. The upper end of the crystal carrier is connected with a motor. The heat preservation device comprises an outer tank, a heat preservation layer and a lifting platform arranged at the bottom of the outer tank. The circulating filtration device comprises a cooling tank and a filtering tank arranged adjacently. The growth device is arranged in the heat preservation device. The device can accurately control the temperature fluctuation range of the growth solution in the growth tank, monitor the crystal growth state in real time, feed back to the computer and timely adjust and optimize the crystal growth parameters. The crystal growth solution is continuously circulated and filtered for 24 hours through a pipeline, the cleanliness of the growth solution is ensured, the problem of mixed crystals in the growth tank is overcome, and large-size high-quality crystals can be grown.

Description

Technical Field

[0001] This application relates to a growth apparatus for methylamine lead bromide crystals, belonging to the field of crystal growth technology. Background Technology

[0002] Methylamine lead bromide (CH3NH3PbBr3) crystal is a common organic-inorganic composite perovskite crystal material. It has high carrier mobility, long carrier recombination lifetime, and excellent photoelectric properties such as ionic conductivity and photoconductivity. It is widely used in solar cells, light-emitting diodes, and detection fields.

[0003] Common methods for growing large-size organic-inorganic composite perovskite single crystals include evaporation and cooling methods. However, due to limitations in container size and temperature control precision, these crystal growth methods are difficult to produce large-size, high-quality perovskite single crystals. Summary of the Invention

[0004] This application provides a growth apparatus for methylamine lead bromide crystals. The growth raw materials, methylammonium bromide (CH3NH3Br) and lead bromide (PbBr2), are dissolved in N,N-dimethylformamide (DMF), and growth is carried out using a reverse temperature method. This growth apparatus can precisely control the temperature fluctuation range of the growth solution in the growth tank, monitor the crystal growth status in real time and feed it back to the computer for timely adjustment and optimization of crystal growth parameters. The crystal growth solution is continuously circulated and filtered through pipelines for 24 hours, ensuring the cleanliness of the growth solution, overcoming the problem of impurities in the growth tank, and significantly improving the quality of the crystals.

[0005] A growth apparatus for methylamine lead bromide crystals includes a growth apparatus, a heat preservation apparatus, a circulation filtration apparatus, and a control apparatus.

[0006] The growth apparatus includes a growth tank and a crystal carrier placed inside the growth tank.

[0007] The upper end of the crystal carrier is connected to the motor;

[0008] The heat preservation device includes an outer tank, a heat preservation layer, and a lifting platform located at the bottom of the outer tank;

[0009] The circulating filtration device includes a cooling tank and a filtration tank arranged adjacent to each other;

[0010] The growth device is located within the heat preservation device;

[0011] The growth tank is located at the upper end of the lifting platform;

[0012] The circulating filtration device is located outside the heat preservation device;

[0013] The growth tank has pipes on one side and at the bottom that are connected to the circulating filtration device.

[0014] The control device is connected to the motor.

[0015] Optionally, a seed crystal is provided at the lower end of the crystal carrier.

[0016] Optionally, the upper end of the growth tank is provided with a rubber stopper;

[0017] The upper end of the rubber stopper is equipped with a liquid sealing device.

[0018] Optionally, the growth tank contains a growth solution;

[0019] The outer tank contains a heat transfer medium.

[0020] Optionally, the heat transfer medium includes water.

[0021] Optionally, the connection points between the pipe and the growth tank are respectively the solution outlet and the solution inlet.

[0022] Optionally, a temperature sensor and a heating rod are provided above the outer tank;

[0023] The temperature sensor and heating rod are both connected to the control device.

[0024] Optionally, a movable support is provided above the outer groove;

[0025] The motor is fixed on the movable support.

[0026] Optionally, the bottom of the circulating filter device is provided with a support;

[0027] The cooling tank is equipped with a condenser;

[0028] The filter tank is equipped with a filter element and a circulation pump.

[0029] Optionally, the outer groove adopts a double-layer stainless steel structure.

[0030] Optionally, a knob is provided at the bottom of the lifting platform.

[0031] Optionally, the motor is connected to the die carrier via a threaded connection, and the die carrier is rotated by means of forward and reverse rotation;

[0032] The motor's rotational speed is 0-60 r / min.

[0033] Optionally, the circulating pump is a turbopump.

[0034] Optionally, the filter element has a pore size of 0.05-0.1 μm.

[0035] According to one embodiment of this application, the outer tank is located on the outermost side of the growth apparatus and is used to place the growth tank; the lifting platform is located at the bottom of the outer tank and is used to adjust the height of the growth tank; the growth tank is placed in a water bath inside the outer tank for crystal growth; the motor is located at the top of the outer tank and is connected to the crystal carrier to drive the crystal carrier to rotate; the crystal carrier is placed inside the growth tank and is used to place the seed crystal; the cooling tank is located in the outer tank of the crystal and is used to cool the growth solution; the filter tank is adjacent to the cooling tank and is used to filter the growth solution; the circulation pump is located inside the filter tank and provides power for the circulation of the growth solution; the computer is located outside the growth apparatus and is used to monitor and optimize the crystal growth parameters in real time.

[0036] Optionally, the outer tank adopts a double-layer stainless steel structure with an internal insulation layer to provide insulation.

[0037] Optionally, the height of the lifting platform can be adjusted arbitrarily by the knob at the bottom of the lifting platform.

[0038] Optionally, the growth tank is made of glass. Preferably, the glass material is high borosilicate glass.

[0039] Optionally, the motor drives the crystal carrier to rotate in a forward and reverse manner, with the rotation speed adjustable from 0 to 60 r / min.

[0040] Optionally, the cooling tank is made of stainless steel, and the supersaturated growth solution can be cooled by entering the cooling tank through a pipe.

[0041] Optionally, the filter tank is made of stainless steel and filters the crystal growth solution continuously for 24 hours.

[0042] Optionally, the circulating pump is a turbine pump, with the pump head and impeller made of polytetrafluoroethylene. The impeller is driven to rotate by a motor, providing power for the circulation of the crystal growth solution.

[0043] Optionally, the computer monitors the crystal growth status in real time and adjusts and optimizes the crystal growth parameters in a timely manner, including but not limited to the temperature of the growth tank solution, the speed of the motor, the temperature of the cooling tank, and the power of the circulating pump.

[0044] Optionally, heating rods and temperature sensors are installed above the outer tank to precisely control the temperature of the water bath in the outer tank. The number of heating rods is 2-5, preferably 4.

[0045] Optionally, the liquid sealing device uses silicone oil for sealing; the growth tank is provided with a solution outlet and a solution inlet, the solution outlet is above the growth tank, and the solution inlet is at the bottom of the growth tank.

[0046] Optionally, the motor is fixed by a movable bracket, which allows for arbitrary adjustment of the height of the crystal carrier in the growth tank.

[0047] Optionally, the cooling tank is equipped with a condenser for cooling the water bath inside the cooling tank.

[0048] Optionally, the filter element inside the filter tank is elongated and has a pore size of 0.1 μm, used for filtering the growth solution.

[0049] The beneficial effects that this application can produce include:

[0050] This application provides a growth apparatus for methylamine lead bromide crystals, applicable to the entire crystal growth stage. The growth of large-size organic-inorganic composite perovskite single crystals is limited by factors such as container size and temperature control precision. This methylamine lead bromide crystal growth apparatus can precisely control the temperature fluctuation range of the growth solution in the growth tank, monitor the crystal growth status in real time and feed it back to the computer for timely adjustment and optimization of crystal growth parameters. The crystal growth solution undergoes 24-hour continuous circulation and filtration through pipelines, ensuring the cleanliness of the growth solution, overcoming the problem of impurities in the growth tank, and enabling the growth of large-size, high-quality crystals. Attached Figure Description

[0051] Figure 1 This is a schematic diagram of the growth apparatus for methylamine lead bromide crystals in this application.

[0052] Figure 2 This is a photograph of the single crystal obtained in Example 2.

[0053] The reference numerals in the attached figures are explained as follows:

[0054] 1. Outer tank; 2. Insulation layer; 3. Heat transfer medium; 4. Lifting platform; 5. Temperature sensor; 6. Heating rod; 7. Moving support; 8. Control device; 9. Seed crystal; 10. Growth tank; 11. Rubber stopper; 12. Liquid sealing device; 13. Motor; 14. Pipeline; 15. Growth solution; 16. Crystal carrier; 17. Solution inlet; 18. Solution outlet; 19. Cooling tank; 20. Filter tank; 21. Filter element; 22. Circulation pump; 23. Support; 24. Condenser. Detailed Implementation

[0055] The present application is described in detail below with reference to the embodiments, but the present application is not limited to these embodiments.

[0056] To better illustrate the present invention and facilitate understanding of its operational process, typical but non-limiting embodiments of the present invention are as follows.

[0057] Example 1

[0058] As one embodiment of the present invention, the methylamine lead bromide crystal growth apparatus is as follows: Figure 1 As shown, the methylamine lead bromide crystal growth apparatus consists of an outer tank 1, a lifting platform 4, a control device 8, a growth tank 10, a motor 13, a crystal carrier 16, a cooling tank 19, a filter tank 20, and a circulating pump 22. The insulation layer 2 is located in the double-layered outer tank 1. The temperature sensor 5 is located above the outer tank 1. Heating rods 6 are placed above the outer tank 1. A movable bracket 7 fixes the motor 13. Seed crystals 9 are attached to the upper surface of the crystal carrier 16. A rubber stopper 11 and a liquid sealing device 12 are located above the growth tank 10. The growth tank 10 is placed in the heat transfer medium 3 of the outer tank 1. The growth tank 10 contains a growth solution 15. Under the action of the circulating pump 22, the growth solution 15 flows through the pipe 14, through the solution outlet 18, and then through the cooling tank 19. The condenser 24 inside the cooling tank 19 operates, cooling the growth solution 15. After being filtered by the filter element 21, it returns to the growth tank 10 through the solution inlet 17, completing one cycle of filtration.

[0059] Example 2

[0060] The temperature of the heat transfer medium 3 is set to 25℃ on the control device 8. Two regularly shaped methylamine lead bromide seed crystals 9 are attached to the top of the crystal carrier 16. The prepared growth solution 15 (saturation point 30℃) is pumped into the growth tank 10 through a peristaltic pump. At this time, the seed crystals 9 are in a dissolved state. Then, the temperature of the heat transfer medium 3 is adjusted to 35℃, the motor 13 is turned on, and the speed is 30 r / min. The crystal growth is completed by using a "forward-reverse" method. Figure 2 As shown, a single crystal of methylamine lead bromide with a size of 10mm×10mm was obtained.

[0061] The above description is merely a few embodiments of this application and is not intended to limit this application in any way. Although this application discloses preferred embodiments as described above, it is not intended to limit this application. Any changes or modifications made by those skilled in the art without departing from the scope of the technical solution of this application using the disclosed technical content are equivalent to equivalent implementation cases and fall within the scope of the technical solution.

Claims

1. An apparatus for preparing methylamine lead bromide crystals, characterized in that, It includes growth equipment, heat preservation equipment, circulation filtration equipment, and control equipment; The growth apparatus includes a growth tank and a crystal carrier placed inside the growth tank. The upper end of the crystal carrier is connected to the motor; The heat preservation device includes an outer tank, a heat preservation layer, and a lifting platform located at the bottom of the outer tank; The circulating filtration device includes a cooling tank and a filtration tank arranged adjacent to each other; The growth device is located within the heat preservation device; The growth tank is located at the upper end of the lifting platform; The circulating filtration device is located outside the heat preservation device; The cooling tank is equipped with a condenser; The filter tank is equipped with a filter element and a circulation pump; The growth tank has pipes on one side and at the bottom that are connected to the circulating filtration device. The control device is connected to the motor.

2. The preparation apparatus according to claim 1, characterized in that, The lower end of the crystal carrier is provided with a seed crystal.

3. The preparation apparatus according to claim 1, characterized in that, The upper end of the growth tank is equipped with a rubber stopper; The upper end of the rubber stopper is equipped with a liquid sealing device.

4. The preparation apparatus according to claim 1, characterized in that, The growth tank contains a growth solution; The outer tank contains a heat transfer medium; The heat transfer medium includes water.

5. The preparation apparatus according to claim 1, characterized in that, The connection points between the pipe and the growth tank are the solution outlet and the solution inlet, respectively.

6. The preparation apparatus according to claim 1, characterized in that, A temperature sensor and a heating rod are installed above the outer tank; The temperature sensor and the heating rod are both connected to the control device; A movable support is provided above the outer groove; The motor is fixed on the movable support.

7. The preparation apparatus according to claim 1, characterized in that, The bottom of the circulating filtration device is equipped with a support.

8. The preparation apparatus according to claim 1, characterized in that, The outer groove adopts a double-layer stainless steel structure; A knob is provided at the bottom of the lifting platform; The motor is connected to the die carrier via a thread, and drives the die carrier to rotate in a forward and reverse manner; The motor has a rotational speed of 0-60 r / min.

9. The preparation apparatus according to claim 1, characterized in that, The circulating pump is a turbine pump.

10. The preparation apparatus according to claim 1, characterized in that, The filter element has a pore size of 0.05-0.1 μm.

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