Perovskite quantum dot and compound preparation method and production equipment thereof

Abstract

The invention discloses a preparation method and production equipment of perovskite quantum dots and compounds thereof, and relates to the technical field of preparation of perovskite quantum dots and compounds thereof. The lifting mechanism comprises an annular groove formed in the inner wall of the reaction furnace, two mounting frames are symmetrically and slidably connected to the inner wall of the annular groove, first rods are rotatably connected to the inner walls of the two mounting frames, lifting plates are fixedly connected to the side walls of the first rods, and two limiting rods are symmetrically and fixedly connected to the inner wall of the reaction furnace; the side walls of the two limiting rods are jointly in sliding connection with a sliding block. Compared with a traditional hot injection method, industrial batch production can be carried out through a solid-phase sintering method, AlO (OH) is adopted as a matrix, the size of CsPbX3 cannot be increased along with temperature rise due to limitation of the pore diameter of the AlO (OH) at the high temperature, the quantum confinement effect is reserved, participation of surface ligands is not needed, dry solid powder can be synthesized, and the preparation method is suitable for large-scale industrial production. And the harm to the environment is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of preparation of perovskite quantum dots and their composites, and in particular to a preparation method and production equipment of perovskite quantum dots and their composites. Background Art

[0002] In recent years, quantum dot materials have the advantage of high color saturation corresponding to their unique narrow emission spectrum, which can significantly improve the color display range of display devices and have been applied in the field of flat panel displays.

[0003] At present, the preparation of perovskite quantum dots and their composites are all done by hot injection. However, the perovskite quantum dots synthesized by the traditional hot injection method cannot be dried into solid powder due to the presence of environmentally harmful surface oily ligands, which will pollute the environment. In addition, the experimental operation is cumbersome. The participation of condensed water, three-necked flasks, and nitrogen makes this method only suitable for small-scale production at the laboratory level, and is not suitable for industrial mass production, which seriously limits its practical application. In addition, due to the quantum confinement effect of perovskite quantum dots, the increase in sintering temperature will make CsPbX 3 The grain size grows uncontrollably.

[0004] Based on this, we propose a method and production equipment for preparing perovskite quantum dots and their composites. Summary of the invention

[0005] The purpose of the present invention is to solve the shortcomings of the prior art and to propose a method and production equipment for preparing perovskite quantum dots and their composites.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions: A method for preparing perovskite quantum dots and their composites comprises the following steps: S1. First, weigh appropriate amounts of CsBr and PbBr according to the ratio. 2 and AlO(OH), (CsBr: PbBr 2 The feed ratio of ) and AlO(OH) is 0.082 mmol and 2.46 mmol; S2, weigh the CsBr and PbBr 2 Grind AlO(OH) into powder for 30 min to make it fully mixed; S3, then the powdered CsBr, PbBr 2 and AlO(OH) are placed in the equipment for sintering. The sintering temperature is controlled at 650 degrees Celsius, and nitrogen is introduced during the sintering process for protection. S4. After sintering, perovskite quantum dots of blue, green and red quantum dot powders can be obtained.

[0007] A production device for perovskite quantum dots and their composites, comprising: Reactor; The material lifting mechanism comprises an annular groove provided on the inner wall of the reaction furnace, the inner wall of the annular groove is symmetrically and slidably connected to two mounting frames, the inner walls of the two mounting frames are both rotatably connected to a first rod, the side wall of the first rod is fixedly connected to a lifting plate, the inner wall of the reaction furnace is symmetrically and fixedly connected to two limit rods, the side walls of the two limit rods are commonly slidably connected to a slider, the side wall of the slider is provided with a limit groove, the inner wall of the limit groove is symmetrically and slidably connected to two L-shaped rods, the other ends of the two L-shaped rods are fixedly connected to the mounting rods, the side walls of the mounting rods are symmetrically and fixedly connected to two L-shaped frames, the side wall of the lifting plate is fixedly connected to a second rod, the side walls of the two L-shaped frames are provided with two slide grooves, and the side wall of the second rod is slidably connected to the inner walls of the two slide grooves; A driving mechanism is installed on the reaction furnace.

[0008] Preferably, the driving mechanism includes a rotating shaft rotatably connected to the top of the reaction furnace, a reciprocating screw is fixedly connected to the lower end of the rotating shaft, the side wall of the reciprocating screw is threadedly connected to the slider, a motor is fixedly connected to the upper end of the reaction furnace, and the output end of the motor passes through the upper end of the reaction furnace and is fixedly connected to the rotating shaft.

[0009] Preferably, the driving mechanism also includes two driving rods symmetrically fixedly connected to the side walls of the reciprocating screw, the lower ends of the two driving rods are respectively fixedly connected to the upper ends of the two mounting frames, the side walls of the mounting rods are provided with vertical grooves, the vertical grooves penetrate the side walls of the mounting rods, and the side walls of the driving rods are slidably connected to the inner walls of the vertical grooves.

[0010] Preferably, two fixing rods are fixedly connected to the lower ends of the two mounting frames, and an annular cover is fixedly connected to the other ends of the two fixing rods, and the lower end of the annular cover is arranged to fit the bottom of the reactor.

[0011] Preferably, a material gathering mechanism is installed on the annular cover, and the material gathering mechanism includes two T-shaped rods symmetrically and slidably connected to the side wall of the annular cover, one end of the two T-shaped rods passes through the inner wall of the annular cover and is fixedly connected to a push plate, the side wall of the lifting plate is fixedly connected to a fixing frame, the upper end of the T-shaped rod is fixedly connected to a third rod, the side wall of the fixing frame is rotatably connected to a connecting rod, and the other end of the connecting rod is rotatably connected to the third rod.

[0012] Preferably, a mounting groove is provided in the top of the reaction furnace, and a plurality of fan blades are fixedly connected to the side wall of the rotating shaft located in the mounting groove.

[0013] Preferably, a first annular cavity is provided in the reaction furnace, a plurality of first exhaust holes are provided at the bottom of the first annular cavity, one end of the first exhaust hole is connected to the mounting groove, a first solenoid valve is installed on the inner wall of the first exhaust hole, an air supply pipe is fixedly connected to the inner wall of the first annular cavity, and the other end of the air supply pipe is connected to an external air pump.

[0014] Preferably, a cooling mechanism is installed on the reactor, and the cooling mechanism includes a second annular cavity opened in the reactor, two second exhaust holes are opened in the bottom of the second annular cavity, the other end of the second exhaust hole is connected with the mounting groove, a pressure relief valve is installed on the inner wall of the second exhaust hole, the first annular cavity is connected with the second annular cavity through a plurality of one-way air inlet holes, a second solenoid valve is installed on the inner wall of the one-way air inlet hole, an installation cavity is opened in the side wall of the reactor, a temperature sensor is installed on the inner wall of the installation cavity, and the temperature sensor is connected with the first solenoid valve and the second solenoid valve through a PLC control circuit.

[0015] Preferably, a feed pipe is fixedly connected to the upper end of the reaction furnace, a discharge pipe is fixedly connected to the lower end of the reaction furnace, and a valve is installed at the lower end of the discharge pipe.

[0016] The present invention has the following beneficial effects: 1. Compared with the traditional hot injection method, solid phase sintering can be used for industrial mass production, and AlO (OH) is used as the matrix. At high temperature, AlO (OH) is limited by its own pore size, making CsPbX 3 The size of the nanoparticles cannot grow with increasing temperature, the quantum confinement effect is retained, and the participation of surface ligands is not required. Dry solid powders can be synthesized, reducing the harm to the environment. 2. By setting up the lifting mechanism and driving mechanism, during the reaction process, as the sintering temperature increases, CsBr and PbBr 2 The material melts and vaporizes to form gaseous CsBr and PbBr 2 , while gaseous CsBr and PbBr 2 It will flow upward in the reactor, and the AlO (OH) at the bottom will not be able to fully react with the gaseous CsBr and PbBr 2 contact, and then CsBr and PbBr 2 Therefore, during the sintering process, the motor is started so that the lifting plate can scoop up the AlO (OH) at the bottom of the reactor and then lift it to the middle of the reactor, so that AlO (OH) can fully react with the gaseous CsBr and PbBr 2 contact, so that the gaseous CsBr and PbBr 2Dispersed in the pores of AlO(OH), forming perovskite quantum dots; 3. When the reciprocating screw rotates, the two mounting frames will be driven to rotate synchronously through the two driving rods, and then the two lifting plates can make circular motion, so that AlO (OH) at different positions can be lifted, so that all AlO (OH) and CsBr and PbBr can be separated to the maximum extent. 2 Contact, and then the reaction is more complete, without causing waste; 4. By setting up a material gathering mechanism, the lifting plate will drive the fixed frame to rotate repeatedly when it rotates repeatedly, and then the fixed frame will drive the T-bar to move back and forth through the connecting rod and the third rod, thereby driving the push plate to move back and forth. When the lifting plate rotates away from the inner wall of the reactor, the push plate will move toward the center of the reactor, and then push the AlO (OH) at the edge of the annular cover into the center of the reactor for accumulation. At this time, the lifting plate can shovel up more AlO (OH), and then more AlO (OH) will react with gaseous CsBr and PbBr each time. 2 Contact, thereby improving the efficiency of the reaction and accelerating the production process; 5. By setting the installation slot and the fan blades, the rotating shaft will drive the multiple fan blades to rotate. Under the action of the fan blades, on the one hand, the nitrogen discharged through the first exhaust hole can flow downward quickly and contact with the lower material to form a protective and air-isolating effect. On the other hand, when the nitrogen flows downward, it can well inhibit the gaseous CsBr and PbBr 2 Flow upward, so that the gaseous CsBr and PbBr 2 Stay in the middle and lower part of the reactor as much as possible, and cooperate with the lifting plate to make AlO (OH) as much as possible with more CsBr and PbBr 2 Full contact; 6. By setting a cooling mechanism, when the temperature in the reactor 1 exceeds 650 degrees Celsius, the temperature sensor will sense a signal, and the first solenoid valve and the second solenoid valve will be energized through the PLC control circuit, the first solenoid valve will be energized to close, and the second solenoid valve will be energized to open, and then the nitrogen entering the first annular cavity will enter the second annular cavity through the one-way air inlet hole, and the nitrogen will accumulate in the second annular cavity, and then the pressure in the second annular cavity will gradually increase, and then the nitrogen will gradually increase in pressure. When the pressure in the second annular cavity exceeds the threshold of the pressure relief valve, the pressure relief valve will open, and the nitrogen will instantly enter the reactor through the second exhaust hole. According to the nitrogen expansion refrigeration principle, nitrogen is released after being pressurized. Its pressure will decrease during the expansion process, and then the molecular energy change causes the temperature to drop. Therefore, the nitrogen released after pressurization can achieve the purpose of refrigeration and reduce the temperature in the reactor. When the temperature drops to 650 degrees Celsius, the temperature sensor will cut off the power supply through the PLC control circuit, and then the first solenoid valve will be powered off and opened, and the second solenoid valve will be powered off and closed, so as to carry out normal nitrogen supply. Therefore, the temperature can be automatically lowered according to the temperature changes in the reactor, so that the temperature in the reactor is always maintained at the optimal reaction temperature of about 650 degrees Celsius. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 A schematic diagram of the three-dimensional structure of a perovskite quantum dot and composite production device proposed by the present invention; Figure 2 for Figure 1 A schematic cross-sectional view of the structure; Figure 3 for Figure 2 Structural diagram of the middle lifting mechanism; Figure 4 for Figure 2 A schematic diagram of the structure enlargement at point A; Figure 5 for Figure 2 A schematic diagram of the structure at B in FIG. Figure 6 for Figure 2 Schematic diagram of the enlarged structure at position C in FIG.

[0018] In the figure: 1, reactor; 2, annular groove; 3, mounting frame; 4, first rod; 5, lifting plate; 6, limiting rod; 7, slider; 8, limiting groove; 9, L-shaped rod; 10, mounting rod; 11, L-shaped frame; 12, second rod; 13, slide; 14, rotating shaft; 15, reciprocating screw; 16, motor; 17, annular cover; 18, T-shaped rod; 19, push plate; 20, fixing rod; 21, fixing frame; 22, third Rod; 23, connecting rod; 24, first annular cavity; 25, first exhaust hole; 26, first solenoid valve; 27, air supply pipe; 28, mounting groove; 29, fan blade; 30, second annular cavity; 31, second exhaust hole; 32, pressure relief valve; 33, one-way air inlet hole; 34, second solenoid valve; 35, mounting cavity; 36, temperature sensor; 37, feed pipe; 38, discharge pipe; 39, drive rod; 40, vertical groove. DETAILED DESCRIPTION

[0019] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without violating the connotation of the present invention, so the present invention is not limited by the specific implementation disclosed below.

[0020] A method for preparing perovskite quantum dots and their composites comprises the following steps: S1. First, weigh appropriate amounts of CsBr and PbBr according to the ratio. 2 and AlO(OH), (CsBr: PbBr 2 The feed ratio of ) and AlO(OH) is 0.082 mmol and 2.46 mmol; S2, weigh the CsBr and PbBr 2 Grind AlO(OH) into powder for 30 min to make it fully mixed; S3, then the powdered CsBr, PbBr 2 and AlO(OH) are placed in the equipment for sintering. The sintering temperature is controlled at 650 degrees Celsius, and nitrogen is introduced during the sintering process for protection. S4. After sintering, perovskite quantum dots of blue, green and red quantum dot powders can be obtained.

[0021] Reference Figure 1 - Figure 6 , a production device for perovskite quantum dots and their composites, comprising: Reactor 1; Lifting mechanism, such as Figure 2 - Figure 3 As shown, the lifting mechanism includes an annular groove 2 provided on the inner wall of the reaction furnace 1, two mounting frames 3 are symmetrically slidably connected to the inner wall of the annular groove 2, the inner walls of the two mounting frames 3 are both rotatably connected to the first rod 4, the side walls of the first rod 4 are fixedly connected to the lifting plate 5, the inner wall of the reaction furnace 1 is symmetrically fixedly connected to two limiting rods 6, the side walls of the two limiting rods 6 are commonly slidably connected to a slider 7, the side wall of the slider 7 is provided with a limiting groove 8, the inner wall of the limiting groove 8 is symmetrically slidably connected to two L-shaped rods 9, the other ends of the two L-shaped rods 9 are fixedly connected to the mounting rod 10, the side wall of the mounting rod 10 is symmetrically fixedly connected to two L-shaped frames 11, the side wall of the lifting plate 5 is fixedly connected to the second rod 12, the side walls of the two L-shaped frames 11 are provided with two slide grooves 13, and the side wall of the second rod 12 is slidably connected to the inner walls of the two slide grooves 13; A driving mechanism is installed on the reaction furnace 1 .

[0022] like Figure 2 As shown, the driving mechanism includes a rotating shaft 14 rotatably connected to the top of the reactor 1, a reciprocating screw 15 is fixedly connected to the lower end of the rotating shaft 14, and the side wall of the reciprocating screw 15 is threadedly connected to the slider 7. A motor 16 is fixedly connected to the upper end of the reactor 1, and the output end of the motor 16 passes through the upper end of the reactor 1 and is fixedly connected to the rotating shaft 14.

[0023] Furthermore, as the sintering temperature increases during the reaction, CsBr and PbBr 2 The material melts and vaporizes to form gaseous CsBr and PbBr 2 , while gaseous CsBr and PbBr 2 will flow upward in the reactor 1, and the AlO(OH) at the bottom will not be able to fully react with the gaseous CsBr and PbBr 2 contact, and then CsBr and PbBr 2 It cannot be well dispersed in the holes of AlO (OH) to form perovskite quantum dots. Therefore, during the sintering process, the motor 16 is started to drive the rotating shaft 14 to rotate, and the rotation of the rotating shaft 14 will synchronously drive the reciprocating screw 15 to rotate, and then the slider 7 will quickly slide back and forth up and down, and the slider 7 will drive the mounting rod 10 to move back and forth up and down through the L-shaped rod 9, and then drive the L-shaped frame 11 to move back and forth up and down, thereby driving the lifting plate 5 to reciprocate around the center of the first rod 4, and then the lifting plate 5 can shovel up the AlO (OH) at the bottom of the reactor 1, and then lift it to the middle position of the reactor 1, so that AlO (OH) can fully react with the gaseous CsBr and PbBr 2 contact, so that the gaseous CsBr and PbBr 2 Dispersed in the pores of AlO(OH) to form perovskite quantum dots.

[0024] like Figure 2 - Figure 3As shown, the driving mechanism also includes two driving rods 39 symmetrically fixedly connected to the side walls of the reciprocating screw 15, the lower ends of the two driving rods 39 are respectively fixedly connected to the upper ends of the two mounting frames 3, a vertical groove 40 is opened on the side wall of the mounting rod 10, the vertical groove 40 penetrates the side wall of the mounting rod 10, and the side wall of the driving rod 39 is slidably connected to the inner wall of the vertical groove 40.

[0025] Furthermore, when the reciprocating screw 15 rotates, the two mounting frames 3 are synchronously driven to rotate through the two driving rods 39, thereby driving the two lifting plates 5 to make circular motion, thereby lifting AlO (OH) at different positions, maximizing the separation of all AlO (OH) with CsBr and PbBr. 2 Contact, thereby reacting more fully without causing waste.

[0026] Two fixing rods 20 are fixedly connected to the lower ends of the two mounting frames 3 , and an annular cover 17 is fixedly connected to the other ends of the two fixing rods 20 . The lower end of the annular cover 17 is arranged to fit the bottom of the reaction furnace 1 .

[0027] like Figure 2 and Figure 5 As shown, a material gathering mechanism is installed on the annular cover 17, and the material gathering mechanism includes two T-shaped rods 18 symmetrically slidably connected to the side wall of the annular cover 17, one end of the two T-shaped rods 18 passes through the inner wall of the annular cover 17 and is fixedly connected to a push plate 19, the side wall of the lifting plate 5 is fixedly connected to a fixing frame 21, the upper end of the T-shaped rod 18 is fixedly connected to a third rod 22, the side wall of the fixing frame 21 is rotatably connected to a connecting rod 23, and the other end of the connecting rod 23 is rotatably connected to the third rod 22.

[0028] Furthermore, when the lifting plate 5 rotates repeatedly, it will drive the fixing frame 21 to rotate repeatedly, and then the fixing frame 21 will drive the T-shaped rod 18 to move back and forth through the connecting rod 23 and the third rod 22, thereby driving the push plate 19 to move back and forth. When the lifting plate 5 rotates in a direction away from the inner wall of the reactor 1, the push plate 19 will move toward the center of the reactor 1, and then push the AlO (OH) at the edge of the annular cover 17 into the center of the reactor 1 for accumulation. At this time, the lifting plate 5 can shovel up more AlO (OH), and then more AlO (OH) will react with the gaseous CsBr and PbBr each time. 2 contact, thereby improving the efficiency of the reaction and accelerating the production process.

[0029] like Figure 2 and Figure 6 As shown, a mounting groove 28 is provided in the top of the reaction furnace 1 , and a plurality of fan blades 29 are fixedly connected to the side wall of the rotating shaft 14 located in the mounting groove 28 .

[0030] Furthermore, the rotating shaft 14 drives the plurality of blades 29 to rotate. Under the action of the blades 29, on the one hand, the nitrogen discharged through the first exhaust hole 25 can flow downward quickly and contact with the lower material to form a protective and air-isolating effect. On the other hand, when the nitrogen flows downward, it can well inhibit the gaseous CsBr and PbBr 2 Flow upward, so that the gaseous CsBr and PbBr 2 Stay in the middle and lower part of the reactor 1 as much as possible, and cooperate with the lifting plate 5 to make AlO (OH) as much as possible with more CsBr and PbBr 2 Full contact.

[0031] like Figure 2 and Figure 6 As shown, a first annular cavity 24 is provided in the reaction furnace 1, and a plurality of first exhaust holes 25 are provided at the bottom of the first annular cavity 24. One end of the first exhaust hole 25 is connected to the mounting groove 28, and a first solenoid valve 26 is installed on the inner wall of the first exhaust hole 25. The first solenoid valve 26 is closed when powered on and opened when powered off. An air supply pipe 27 is fixedly connected to the inner wall of the first annular cavity 24, and the other end of the air supply pipe 27 is connected to an external air pump.

[0032] Furthermore, during the sintering process, the external air pump is started to pump nitrogen into the first annular cavity 24 through the air supply pipe 27, and then the nitrogen enters the reaction furnace 1 through the multiple first exhaust holes 25 to protect and isolate the air.

[0033] The reaction furnace 1 is provided with a cooling mechanism, such as Figure 2 and Figure 6 As shown, the cooling mechanism includes a second annular cavity 30 provided in the reaction furnace 1, two second exhaust holes 31 are provided in the bottom of the second annular cavity 30, the other end of the second exhaust hole 31 is connected with the mounting groove 28, a pressure relief valve 32 is installed on the inner wall of the second exhaust hole 31, the first annular cavity 24 is connected with the second annular cavity 30 through a plurality of one-way air inlet holes 33, the one-way air inlet holes 33 only allow the nitrogen in the first annular cavity 24 to enter the second annular cavity 30, a second solenoid valve 34 is installed on the inner wall of the one-way air inlet hole 33, the second solenoid valve 34 is powered on and opened, and powered off and closed, an installation cavity 35 is provided in the side wall of the reaction furnace 1, a temperature sensor 36 is installed on the inner wall of the installation cavity 35, and the temperature sensor 36 is connected with the first solenoid valve 26 and the second solenoid valve 34 through a PLC control circuit.

[0034] Furthermore, when the temperature in the reactor 1 exceeds 650 degrees Celsius, the temperature sensor 36 will sense a signal, and the first solenoid valve 26 and the second solenoid valve 34 will be energized through the PLC control circuit, the first solenoid valve 26 will be energized to close, and the second solenoid valve 34 will be energized to open, and then the nitrogen entering the first annular cavity 24 will enter the second annular cavity 30 through the one-way air inlet 33, and the nitrogen will accumulate in the second annular cavity 30, and then the pressure in the second annular cavity 30 will gradually increase, and then the nitrogen will gradually increase in pressure. When the pressure in the second annular cavity 30 exceeds the threshold of the pressure relief valve 32, the pressure relief valve 32 will open, and the nitrogen will instantly pass through the second exhaust hole 31 After entering the reactor 1, according to the nitrogen expansion refrigeration principle, the nitrogen is released after being pressurized, and its pressure will decrease during the expansion process, and then the molecular energy change causes the temperature to drop. Therefore, the nitrogen released after pressurization can achieve the purpose of refrigeration and can reduce the temperature in the reactor 1. When the temperature drops to 650 degrees Celsius, the temperature sensor 36 will cut off the power supply through the PLC control circuit, and then the first solenoid valve 26 will be powered off and opened, and the second solenoid valve 34 will be powered off and closed, so as to carry out normal nitrogen supply. Therefore, the temperature can be automatically lowered according to the temperature change in the reactor 1, so that the temperature in the reactor 1 is always maintained at the optimal reaction temperature of about 650 degrees Celsius.

[0035] like Figure 2 As shown, a feed pipe 37 is fixedly connected to the upper end of the reaction furnace 1 , a discharge pipe 38 is fixedly connected to the lower end of the reaction furnace 1 , and a valve is installed at the lower end of the discharge pipe 38 .

[0036] In the present invention, firstly according to (CsBr: PbBr 2 The materials are weighed and then ground into powder and added into the reactor 1 through the feed pipe 37. The reactor 1 is started and the materials are sintered at a high temperature. The sintering temperature is controlled at 650 degrees Celsius.

[0037] During the sintering process, the external air pump is started to pump nitrogen into the first annular cavity 24 through the air supply pipe 27, and then the nitrogen enters the reaction furnace 1 through the multiple first exhaust holes 25 to protect and isolate the air.

[0038] As the sintering temperature increases during the reaction, CsBr and PbBr 2 The material melts and vaporizes to form gaseous CsBr and PbBr 2 , while gaseous CsBr and PbBr 2 will flow upward in the reactor 1, and the AlO(OH) at the bottom will not be able to fully react with the gaseous CsBr and PbBr 2 contact, and then CsBr and PbBr 2Therefore, during the sintering process, the motor 16 is started to drive the rotating shaft 14 to rotate, and the rotating shaft 14 drives the plurality of fan blades 29 to rotate. Under the action of the fan blades 29, on the one hand, the nitrogen discharged through the first exhaust hole 25 can flow downward quickly and contact with the lower material to form a protective and air-isolating effect. On the other hand, when the nitrogen flows downward, it can well inhibit the gaseous CsBr and PbBr 2 Flow upward, so that the gaseous CsBr and PbBr 2 The first rod 4 is used as the center of the first rod 4, and the first rod 4 is used as the center of the first rod 4. ... 2 contact, so that the gaseous CsBr and PbBr 2 Dispersed in the pores of AlO(OH) to form perovskite quantum dots.

[0039] When the lifting plate 5 rotates repeatedly, it will drive the fixing frame 21 to rotate repeatedly, and then the fixing frame 21 will drive the T-shaped rod 18 to move back and forth through the connecting rod 23 and the third rod 22, thereby driving the push plate 19 to move back and forth. When the lifting plate 5 rotates in the direction away from the inner wall of the reactor 1, the push plate 19 will move toward the center of the reactor 1, and then push the AlO (OH) at the edge of the annular cover 17 into the center of the reactor 1 for accumulation. At this time, the lifting plate 5 can shovel up more AlO (OH), and then more AlO (OH) will react with the gaseous CsBr and PbBr each time. 2 contact, thereby improving the efficiency of the reaction and accelerating the production process.

[0040] When the reciprocating screw 15 rotates, the two mounting frames 3 are synchronously driven to rotate through the two driving rods 39, thereby driving the two lifting plates 5 to make circular motion, thereby lifting AlO (OH) at different positions, maximizing the separation of all AlO (OH) with CsBr and PbBr. 2 When the mounting frame 3 rotates, the annular cover 17 is driven to rotate synchronously through the fixing rod 20, and then the push plate 19 is also driven to rotate synchronously to maintain the aggregation of AlO (OH) at the bottom.

[0041] When the temperature in the reactor 1 exceeds 650 degrees Celsius, the temperature sensor 36 will sense a signal, and the first solenoid valve 26 and the second solenoid valve 34 will be energized through the PLC control circuit. The first solenoid valve 26 will be energized to close, and the second solenoid valve 34 will be energized to open, and then the nitrogen entering the first annular cavity 24 will enter the second annular cavity 30 through the one-way air inlet 33, and the nitrogen will accumulate in the second annular cavity 30, and then the pressure in the second annular cavity 30 will gradually increase, and then the nitrogen will gradually increase in pressure. When the pressure in the second annular cavity 30 exceeds the threshold of the pressure relief valve 32, the pressure relief valve 32 will open, and the nitrogen will instantly enter through the second exhaust hole 31. In the reactor 1, according to the nitrogen expansion refrigeration principle, the nitrogen is released after being pressurized, and its pressure will decrease during the expansion process, and then the molecular energy change causes the temperature to drop. Therefore, the nitrogen released after pressurization can achieve the purpose of refrigeration and can reduce the temperature in the reactor 1. When the temperature drops to 650 degrees Celsius, the temperature sensor 36 will cut off the power supply through the PLC control circuit, and then the first solenoid valve 26 will be powered off and opened, and the second solenoid valve 34 will be powered off and closed, so as to carry out normal nitrogen supply. Therefore, the temperature can be automatically lowered according to the temperature change in the reactor 1, so that the temperature in the reactor 1 is always maintained at the optimal reaction temperature of about 650 degrees Celsius.

[0042] After sintering is completed, the valve on the discharge pipe 38 is opened, and the obtained perovskite quantum dots of the blue, green and red quantum dot powders will be discharged through the discharge pipe 38 and collected.

[0043] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for preparing perovskite quantum dots and their composites, characterized in that: The following steps are involved: S1. First, weigh appropriate amounts of CsBr, PbBr2 and AlO(OH) according to the ratio. The feeding ratio of (CsBr: PbBr2) and AlO(OH) is 0.082 mmol and 2.46 mmol; S2. Grind the weighed CsBr, PbBr2 and AlO(OH) into powder for 30 min to fully mix them; S3, then put the powdered CsBr, PbBr2 and AlO (OH) into the equipment for sintering, the sintering temperature is controlled at 650 degrees Celsius, and nitrogen is introduced during the sintering process for protection; S4. After sintering, blue, green and red perovskite quantum dots are obtained.

2. A production device for perovskite quantum dots and their composites, applied to the method for preparing perovskite quantum dots and their composites according to claim 1, characterized in that: include: Reactor (1); A material lifting mechanism, the material lifting mechanism comprising an annular groove (2) provided on the inner wall of a reaction furnace (1), the inner wall of the annular groove (2) being symmetrically slidably connected to two mounting frames (3), the inner walls of the two mounting frames (3) being rotatably connected to a first rod (4), the side walls of the first rod (4) being fixedly connected to a lifting plate (5), the inner wall of the reaction furnace (1) being symmetrically fixedly connected to two limiting rods (6), the side walls of the two limiting rods (6) being slidably connected to a slider (7), the side walls of the slider (7) being provided with a limiting groove (8), the inner wall of the limiting groove (8) being symmetrically slidably connected to two L-shaped rods (9), the other ends of the two L-shaped rods (9) being fixedly connected to a mounting rod (10), the side walls of the mounting rod (10) being symmetrically fixedly connected to two L-shaped frames (11), the side walls of the lifting plate (5) being fixedly connected to a second rod (12), the side walls of the two L-shaped frames (11) being provided with two sliding grooves (13), the side walls of the second rod (12) being slidably connected to the inner walls of the two sliding grooves (13); A driving mechanism is installed on the reaction furnace (1).

3. The production equipment of perovskite quantum dots and their composites according to claim 2, characterized in that: in: The driving mechanism comprises a rotating shaft (14) rotatably connected to the top of the reaction furnace (1); a reciprocating screw (15) is fixedly connected to the lower end of the rotating shaft (14); a side wall of the reciprocating screw (15) is threadedly connected to a slider (7); a motor (16) is fixedly connected to the upper end of the reaction furnace (1); an output end of the motor (16) passes through the upper end of the reaction furnace (1) and is fixedly connected to the rotating shaft (14).

4. The production equipment of perovskite quantum dots and their composites according to claim 3, characterized in that: in: The driving mechanism further comprises two driving rods (39) symmetrically fixedly connected to the side wall of the reciprocating screw (15), the lower ends of the two driving rods (39) being fixedly connected to the upper ends of the two mounting frames (3) respectively, the side wall of the mounting rod (10) being provided with a vertical groove (40), the vertical groove (40) penetrating the side wall of the mounting rod (10), and the side wall of the driving rod (39) being slidably connected to the inner wall of the vertical groove (40).

5. The production equipment of perovskite quantum dots and their composites according to claim 2, characterized in that: in: The lower ends of the two mounting frames (3) are fixedly connected to two fixing rods (20), and the other ends of the two fixing rods (20) are commonly fixedly connected to an annular cover (17), wherein the lower end of the annular cover (17) is arranged to fit the inner bottom of the reaction furnace (1).

6. The production equipment of perovskite quantum dots and their composites according to claim 5, characterized in that: in: A material gathering mechanism is installed on the annular cover (17), and the material gathering mechanism comprises two T-shaped rods (18) symmetrically slidably connected to the side wall of the annular cover (17), one end of each of the two T-shaped rods (18) passes through the inner wall of the annular cover (17) and is fixedly connected to a push plate (19), the side wall of the lifting plate (5) is fixedly connected to a fixing frame (21), the upper end of the T-shaped rod (18) is fixedly connected to a third rod (22), the side wall of the fixing frame (21) is rotatably connected to a connecting rod (23), and the other end of the connecting rod (23) is rotatably connected to the third rod (22).

7. The production equipment of perovskite quantum dots and their composites according to claim 4, characterized in that: in: A mounting groove (28) is provided at the top of the reaction furnace (1), and a plurality of fan blades (29) are fixedly connected to the side wall of the rotating shaft (14) located in the mounting groove (28).

8. The production equipment of perovskite quantum dots and their composites according to claim 7, characterized in that: in: A first annular cavity (24) is provided in the reaction furnace (1); a plurality of first exhaust holes (25) are provided at the bottom of the first annular cavity (24); one end of the first exhaust hole (25) is communicated with the mounting groove (28); a first solenoid valve (26) is installed on the inner wall of the first exhaust hole (25); an air supply pipe (27) is fixedly connected to the inner wall of the first annular cavity (24); the other end of the air supply pipe (27) is communicated with an external air pump.

9. The production equipment of perovskite quantum dots and their composites according to claim 8, characterized in that: in: The reaction furnace (1) is provided with a cooling mechanism, the cooling mechanism comprising a second annular cavity (30) provided in the reaction furnace (1), two second exhaust holes (31) provided at the bottom of the second annular cavity (30), the other end of the second exhaust hole (31) being in communication with the installation groove (28), a pressure relief valve (32) being provided on the inner wall of the second exhaust hole (31), the first annular cavity (24) being in communication with the second annular cavity (30) via a plurality of one-way air inlet holes (33), a second solenoid valve (34) being provided on the inner wall of the one-way air inlet hole (33), a mounting cavity (35) provided in the side wall of the reaction furnace (1), a temperature sensor (36) being provided on the inner wall of the mounting cavity (35), the temperature sensor (36) being connected to the first solenoid valve (26) and the second solenoid valve (34) via a PLC control circuit.

10. The production equipment of perovskite quantum dots and their composites according to claim 2, characterized in that: in: The upper end of the reaction furnace (1) is fixedly connected to a feed pipe (37), the lower end of the reaction furnace (1) is fixedly connected to a discharge pipe (38), and the lower end of the discharge pipe (38) is provided with a valve.

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