Solution method crystal growth system and crystal growth method

Abstract

The invention relates to the technical field of crystal growth, and discloses a solution-method crystal growth system and a solution-method crystal growth method.The solution-method crystal growth system comprises a dissolving device, a first connecting device, a second connecting device, a crystallizing device, a first temperature control unit, a second temperature control unit and a third temperature control unit; a liquid outlet of the dissolving device, the first connecting device, the crystallizing device, the second connecting device and a liquid return opening of the dissolving device are sequentially communicated to form a closed circulation loop, a crystallizing solution circulates among the liquid outlet of the dissolving device, the first connecting device and the crystallizing device, and reflux liquid circulates among the crystallizing device, the second connecting device and the liquid return opening of the dissolving device; the dissolving device is in heat-conducting connection with the first temperature control unit, the first connecting device and the second connecting device are in heat-conducting connection with the second temperature control unit, and the crystallizing device is in heat-conducting connection with the third temperature control unit; the temperature of the first temperature control unit, the temperature of the second temperature control unit and the temperature of the third temperature control unit are sequentially increased or decreased.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of crystal growth, in particular to a solution method crystal growth system and a crystal growth method. BACKGROUND

[0002] Solution method crystal growth technology is a technology of forming an ordered crystal structure by controlling the slow precipitation of solute from a supersaturated solution. At present, the solution method crystal growth technology usually adopts a static solution system method, which has the following problems: local concentration of the solution is uneven, resulting in unstable crystal growth rate; the temperature gradient is single, which is not conducive to the preferred orientation growth of the crystal; and the solute cannot be supplemented in time, which limits the growth time and size. SUMMARY

[0003] Embodiments of the present application aim to provide a solution method crystal growth system and a crystal growth method to solve the technical problem of a single temperature gradient in the prior art.

[0004] Embodiments of the present application solve the technical problem by adopting the following technical solution:

[0005] A solution method crystal growth system is provided, comprising a dissolving device, a first connecting device, a second connecting device, a crystallizing device, a first temperature control unit, a second temperature control unit and a third temperature control unit;

[0006] The liquid outlet of the dissolving device, the first connecting device, the crystallizing device, the second connecting device and the liquid return port of the dissolving device are sequentially communicated to form a closed circulation loop, the crystallizing solution flows through the liquid outlet of the dissolving device, the first connecting device and the crystallizing device, and the backflow liquid flows through the crystallizing device, the second connecting device and the liquid return port of the dissolving device;

[0007] The dissolving device and the first temperature control unit are thermally connected, the first connecting device and the second connecting device are thermally connected to the second temperature control unit, and the crystallizing device is thermally connected to the third temperature control unit;

[0008] The temperature of the first temperature control unit, the temperature of the second temperature control unit and the temperature of the third temperature control unit are sequentially increased or sequentially decreased.

[0009] Optionally, the second temperature control unit comprises a first temperature control module and a second temperature control module, the first connecting device and the first temperature control module are thermally connected, and the second connecting device and the second temperature control module are thermally connected;

[0010] The temperature of the first temperature control unit, the temperature of the first temperature control module, and the temperature of the third temperature control unit are sequentially increased, and the temperature of the first temperature control unit, the temperature of the second temperature control module, and the temperature of the third temperature control unit are sequentially increased.

[0011] Alternatively, the temperature of the first temperature control unit, the temperature of the first temperature control module, and the temperature of the third temperature control unit are sequentially decreased, and the temperature of the first temperature control unit, the temperature of the second temperature control module, and the temperature of the third temperature control unit are sequentially decreased.

[0012] Optionally, the number of the first connecting devices, the number of the second connecting devices, and the number of the second temperature control units are at least two and one-to-one corresponding, respectively, and each second temperature control unit is in heat conduction connection with a corresponding first connecting device and a corresponding second connecting device.

[0013] In the flow direction of the crystallization solution, the temperature of each second temperature control unit is sequentially increased or sequentially decreased.

[0014] Optionally, the first temperature control unit comprises a first container and a first temperature control assembly, the first container is used to hold a first temperature control liquid, and the first temperature control assembly is used to control the temperature of the first temperature control liquid, and the dissolving device is immersed in the first temperature control liquid.

[0015] The second temperature control unit comprises a second container and a second temperature control assembly, the second container is used to hold a second temperature control liquid, and the second temperature control assembly is used to control the temperature of the second temperature control liquid, and the first connecting device and the second connecting device are immersed in the second temperature control liquid.

[0016] The third temperature control unit comprises a third container and a third temperature control assembly, the third container is used to hold a third temperature control liquid, and the third temperature control assembly is used to control the temperature of the third temperature control liquid, and the crystallization device is immersed in the third temperature control liquid.

[0017] The temperature of the first temperature control liquid, the temperature of the second temperature control liquid, and the temperature of the third temperature control liquid are sequentially increased or sequentially decreased.

[0018] Optionally, the dissolving device comprises a material supplement bin and a peristaltic pump, and the material supplement bin is immersed in the first temperature control unit.

[0019] The liquid outlet of the peristaltic pump, the first connecting device, the crystallization device, the second connecting device, the liquid return port of the material supplement bin, the liquid outlet of the material supplement bin, and the liquid return port of the peristaltic pump are sequentially communicated to form a closed circulation loop.

[0020] Optionally, the dissolving device further comprises a first filter arranged in the feeding bin.

[0021] Optionally, the crystallization device comprises a growth container and a crystal growth platform, the growth container is immersed in the third temperature control unit, a liquid inlet is arranged at the top of the growth container, a liquid outlet is arranged at the bottom end of the growth container, the liquid inlet is communicated with the first connecting device, the liquid outlet is communicated with the second connecting device, the crystal growth platform is arranged in the growth container and located below the liquid inlet.

[0022] Optionally, the crystallization device further comprises a second filter arranged in the liquid outlet.

[0023] Optionally, the first connecting device comprises a first spiral pipe, and the second connecting device comprises a second spiral pipe.

[0024] The liquid outlet of the dissolving device, the first spiral pipe, the crystallization device, the second spiral pipe and the liquid return port of the dissolving device are sequentially communicated to form a closed circulation loop.

[0025] The first spiral pipe and the second spiral pipe are immersed in the second temperature control unit.

[0026] The application further provides a crystal growth method using the solution method crystal growth system.

[0027] The crystallization solution is provided by the dissolving device;

[0028] The crystallization solution in the dissolving device flows to the crystallization device through the first connecting device;

[0029] The crystallization solution flows through the crystallization device to grow the crystallization seed crystal in the crystallization device and form a backflow liquid;

[0030] The backflow liquid flows to the dissolving device through the second connecting device;

[0031] The above steps are repeated until the crystallization seed crystal in the crystallization device is grown into a crystallization target product.

[0032] Compared with the prior art, in the solution method crystal growth system of the present application, the crystallization raw material is dissolved in the dissolving device to form a crystallization solution, the crystallization solution flows to the crystallization device through the first connecting device, the crystallization seed crystal is contained in the crystallization device, the crystallization seed crystal continuously grows in the crystallization solution, and finally can grow into the target product of crystallization. Since the temperature of the first temperature control unit, the temperature of the second temperature control unit and the temperature of the third temperature control unit are sequentially increased or sequentially decreased, when the crystallization solution sequentially passes through the dissolving device, the first connecting device and the crystallization device, the temperature it contacts is changed in a gradient, so that the crystallization solution can slowly crystallize, which is beneficial to the preferential orientation growth of the crystal, thereby improving the quality of the crystal.

[0033] The crystal growth method of the present application also has the above advantages, which will not be repeated here. BRIEF DESCRIPTION OF DRAWINGS

[0034] One or more embodiments are illustrated by way of example in the figures that form a part of this patent document, these illustrative examples do not limit the embodiments, and elements having the same reference numbers designate analogous elements throughout the specification, unless otherwise indicated, the figures in the drawings do not constitute a proportional limit.

[0035] Figure 1 is a structural schematic diagram of a solution method crystal growth system in an embodiment of the present application;

[0036] Figure 2 is a cross-sectional view of a solution method crystal growth system in an embodiment of the present application;

[0037] Figure 3 is another cross-sectional view of a solution method crystal growth system in an embodiment of the present application;

[0038] Figure 4 is a structural schematic diagram of a first joint assembly in an embodiment of the present application;

[0039] Figure 5 is a structural schematic diagram of a third joint assembly in an embodiment of the present application.

[0040] Reference signs:

[0041] 100, solution method crystal growth system; 10, dissolving device; 12, feeding bin; 14, peristaltic pump; 16, first filter; 17, fourth joint assembly; 18, fifth joint assembly; 20, first connecting device; 22, first spiral pipe; 24, first joint assembly; 242, first hose; 2422, first pipe section; 2424, second pipe section; 244, first buckle; 246, second buckle; 248, third filter; 30, second connecting device; 32, second spiral pipe; 40, crystallizing device; 42, growth vessel; 44, crystal growth platform; 46, second filter; 48, third joint assembly; 482, third hose; 484, third buckle; 50, first temperature control unit; 60, second temperature control unit; 62, first temperature control module; 64, second temperature control module; 70, third temperature control unit. DETAILED DESCRIPTION

[0042] For the purpose of promoting the understanding and facilitating appreciation of the invention, the disclosure hereinafter will describe in detail concrete embodiments thereof, in conjunction with the accompanying drawings. It is to be understood that when an element is referred to as being "connected to" another element, it can be directly connected to the other element, or intervening elements can be present therebetween. The terms "upper", "lower", "left", "right", "top", "bottom", "front", "rear", and the like as used herein are used for description only and are not to be construed as limiting the present invention in position or orientation. The terms "first", "second", etc. are used herein only to describe various elements, but do not connote any priority or importance of the elements over or relative to one another.

[0043] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description of the application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.

[0044] Reference will now be made to Figure 1In one of the embodiments of the present application, a solution method crystal growth system 100 is provided, which comprises a dissolving device 10, a first connecting device 20, a second connecting device 30, a crystallizing device 40, a first temperature control unit 50, a second temperature control unit 60 and a third temperature control unit 70. The liquid outlet of the dissolving device 10, the first connecting device 20, the crystallizing device 40, the second connecting device 30 and the liquid return port of the dissolving device 10 are sequentially communicated to form a closed circulation loop. The crystallizing solution flows through the liquid outlet of the dissolving device 10, the first connecting device 20 and the crystallizing device 40. The backflow liquid flows through the crystallizing device 40, the second connecting device 30 and the liquid return port of the dissolving device 10. The dissolving device 10 and the first temperature control unit 50 are in heat conduction connection. The first connecting device 20 and the second connecting device 30 are in heat conduction connection with the second temperature control unit 60. The crystallizing device 40 is in heat conduction connection with the third temperature control unit 70. The temperature of the first temperature control unit 50, the temperature of the second temperature control unit 60 and the temperature of the third temperature control unit 70 are sequentially increased or sequentially decreased.

[0045] In the present embodiment, the dissolving device 10 and the first temperature control unit 50 are in heat conduction connection. The first connecting device 20 and the second connecting device 30 are in heat conduction connection with the second temperature control unit 60. The crystallizing device 40 is in heat conduction connection with the third temperature control unit 70. The dissolving device 10 can be immersed in the first temperature control unit 50. The first connecting device 20 and the second connecting device 30 can be immersed in the second temperature control unit 60. The crystallizing device 40 can be immersed in the third temperature control unit 70.

[0046] The working principle of the solution method crystal growth system 100 of the present embodiment is as follows. The crystallization raw material is dissolved in the dissolving device 10 to form a crystallization solution. The crystallization solution flows to the crystallizing device 40 through the first connecting device 20. The crystallization seed crystal is contained in the crystallizing device 40. The crystallization seed crystal continuously grows in the crystallization solution and finally grows into the target product. The source of the crystallization seed crystal can be externally added or generated by the crystallization solution. The method for generating the crystallization seed crystal by the crystallization solution is as follows. When the crystallization solution passes through the crystallizing device 40, the crystallization particles can be formed in the crystallizing device 40. The high-quality crystallization particles can be selected as the crystallization seed crystal. The crystallization solution becomes the backflow liquid after flowing through the crystallizing device 40. The backflow liquid flows back to the dissolving device 10 through the second connecting device 30. The dissolving device 10 supplements the crystallization raw material in the backflow liquid to form a new crystallization solution. When the property of the crystallization raw material is temperature increasing crystallization, the temperature of the first temperature control unit 50, the temperature of the second temperature control unit 60 and the temperature of the third temperature control unit 70 are sequentially increased. When the property of the crystallization raw material is temperature decreasing crystallization, the temperature of the first temperature control unit 50, the temperature of the second temperature control unit 60 and the temperature of the third temperature control unit 70 are sequentially decreased.

[0047] In a specific embodiment, the raw material for temperature-increasing crystallization can be lead bromide (PbBr2) and methylammonium bromide (MABr), and the target product of crystallization is methylammonium lead bromide (MAPbBr3).

[0048] After the lead bromide (PbBr2) and the methylammonium bromide (MABr) are ultrasonically dissolved in a dmf (N,N-dimethylformamide) solution by the dissolving device 10, they are injected into the first connecting device 20. The temperature of the first temperature control unit 50 is 50°C, the temperature of the second temperature control unit 60 is 70°C, and the temperature of the third temperature control unit 70 is 90°C. After the crystallization solution grows fine crystalline particles at the crystallization device 40, the high-quality crystalline particles are selected as the crystallization seeds, and the crystallization seeds grow into the target product of crystallization in the crystallization solution.

[0049] In a specific embodiment, the raw material for temperature-decreasing crystallization can be methylammonium iodide (MAI) and lead acetate trihydrate (Pb(CH3COO)2.3H2O), and the target product of crystallization is methylammonium lead iodide (MAPbI3).

[0050] After the methylammonium iodide (MAI) and the lead acetate trihydrate (Pb(CH3COO)2.3H2O) are dissolved in a HI (hydrogen iodide) solution by the dissolving device 10, they are then made to flow into the circulation loop by the first connecting device 20. The temperature of the first temperature control unit 50 is 90°C, the temperature of the second temperature control unit 60 is 70°C, and the temperature of the third temperature control unit 70 is 50°C. After the crystallization solution grows fine crystalline particles at the crystallization device 40, the high-quality crystalline particles are selected as the crystallization seeds, and the crystallization seeds grow into the target product of crystallization in the crystallization solution.

[0051] In the solution method crystal growth system 100 of the present embodiment, since the temperature of the first temperature control unit 50, the temperature of the second temperature control unit 60, and the temperature of the third temperature control unit 70 are sequentially increased or sequentially decreased, when the crystallization solution sequentially passes through the dissolving device 10, the first connecting device 20, and the crystallization device 40, the temperature it contacts is changed in a gradient, which allows the crystallization solution to slowly crystallize, is conducive to the preferred orientation growth of the crystal, and thus can improve the quality of the crystal.

[0052] When the first connecting device 20 and the second connecting device 30 and the second temperature control unit 60 are in thermal connection, the temperature of the crystallization solution in the first connecting device 20 and the temperature of the reflux liquid in the second connecting device 30 can be the same or different. In order to meet the needs of different users, in an embodiment, the second temperature control unit 60 comprises a first temperature control module 62 and a second temperature control module 64, the first connecting device 20 and the first temperature control module 62 are in thermal connection, the second connecting device 30 and the second temperature control module 64 are in thermal connection; the temperature of the first temperature control unit 50, the temperature of the first temperature control module 62, and the temperature of the third temperature control unit 70 are sequentially increased, and the temperature of the first temperature control unit 50, the temperature of the second temperature control module 64, and the temperature of the third temperature control unit 70 are sequentially increased; or, the temperature of the first temperature control unit 50, the temperature of the first temperature control module 62, and the temperature of the third temperature control unit 70 are sequentially decreased, and the temperature of the first temperature control unit 50, the temperature of the second temperature control module 64, and the temperature of the third temperature control unit 70 are sequentially decreased. The temperature of the first temperature control module 62 and the temperature of the second temperature control module 64 can be the same or different. Since the first temperature control module 62 and the second temperature control module 64 are independent of each other. When the temperature of the first temperature control module 62 and the temperature of the second temperature control module 64 are different, the user can adjust the temperature of the first temperature control module 62 and the temperature of the second temperature control module 64 according to the actual situation, so as to fine-tune the temperature of the crystallization solution and the temperature of the reflux liquid, accurately control the temperature change of the crystallization solution and the reflux liquid, and further improve the growth quality of the crystallization target product.

[0053] In an embodiment, the number of first connecting devices 20, the number of second connecting devices 30, and the number of second temperature control units 60 are at least two respectively and one-to-one correspondence, each second temperature control unit 60 is in thermal connection with a corresponding first connecting device 20 and a corresponding second connecting device 30; along the flow direction of the crystallization solution, the temperature of each second temperature control unit 60 is sequentially increased or sequentially decreased. That is, the number of second temperature control units 60 can be multiple, each second temperature control unit 60 is provided with a first connecting device 20 and a second connecting device 30 respectively, and along the flow direction of the crystallization solution, the temperature of each second temperature control unit 60 is also sequentially increased or sequentially decreased. In this way, when the crystallization solution passes through each first connecting device 20, the temperature of the crystallization solution is slowly increased or decreased. When the reflux liquid passes through each second connecting device 30, the temperature of the crystallization solution is slowly increased or decreased. This can further improve the growth quality of the crystallization target product.

[0054] In a specific embodiment, when the crystallization raw material is temperature-increasing crystallization, the number of the second temperature control units 60 is four. The temperature of the first temperature control unit 50 is 50°C, and the temperatures of the second temperature control units 60 are 60°C, 65°C, 70°C and 75°C respectively along the flow direction of the crystallization solution, and the temperature of the third temperature control unit 70 is 90°C. In this way, the temperature of the crystallization solution slowly increases when it flows from the dissolving device 10 to the crystallization device 40, so as to realize slow crystallization.

[0055] In another specific embodiment, when the crystallization raw material is temperature-decreasing crystallization, the number of the second temperature control units 60 is four. The temperature of the first temperature control unit 50 is 90°C, and the temperatures of the second temperature control units 60 are 75°C, 70°C, 65°C and 60°C respectively along the flow direction of the crystallization solution, and the temperature of the third temperature control unit 70 is 50°C. In this way, the temperature of the crystallization solution slowly decreases when it flows from the dissolving device 10 to the crystallization device 40, so as to realize slow crystallization.

[0056] In an embodiment, each of the second temperature control units 60 comprises a first temperature control module 62 and a second temperature control module 64. Figure 1 As shown in FIG. 4, the number of the second temperature control units 60 is four, and each of the second temperature control units 60 comprises a first temperature control module 62 and a second temperature control module 64.

[0057] In an embodiment, the first temperature control unit 50 comprises a first container for containing a first temperature control liquid and a first temperature control assembly for controlling the temperature of the first temperature control liquid, and the dissolving device 10 is immersed in the first temperature control liquid; the second temperature control unit 60 comprises a second container for containing a second temperature control liquid and a second temperature control assembly for controlling the temperature of the second temperature control liquid, and the first connecting device 20 and the second connecting device 30 are immersed in the second temperature control liquid; the third temperature control unit 70 comprises a third container for containing a third temperature control liquid and a third temperature control assembly for controlling the temperature of the third temperature control liquid, and the crystallization device 40 is immersed in the third temperature control liquid. The first temperature control liquid, the second temperature control liquid and the third temperature control liquid can be water or dimethyl silicone oil. The first temperature control assembly, the second temperature control assembly and the third temperature control assembly each comprise a temperature probe and a heating coil, wherein the first container, the second container and the third container are each provided with a temperature probe, the circumferential surface of the first container, the second container and the third container is surrounded by a heating coil, or the bottom end of the first container, the second container and the third container is provided with a heating coil. The heating coil is used for heating the first container, the second container and the third container, and the temperature of the first temperature control liquid, the second temperature control liquid and the third temperature control liquid is controlled according to the temperature indication of the temperature probe.

[0058] When the second temperature control unit 60 comprises the first temperature control module 62 and the second temperature control module 64, the second container is separated by the partition plate to form the first containing groove and the second containing groove, and the first containing groove and the second containing groove are respectively provided with the temperature sensing rod. The first temperature control module 62 comprises the first containing groove and a temperature sensing rod, and the second temperature control module 64 comprises the second containing groove and another temperature sensing rod.

[0059] Through the above structure, the temperature in the first container, the second container and the third container can be accurately controlled, the temperature of the first temperature control liquid, the temperature of the second temperature control liquid and the temperature of the third temperature control liquid can be slowly increased or decreased in turn, so that the growth quality of the target product of crystallization can be further improved.

[0060] Please refer to Figure 2 and Figure 3 When the reflux liquid flows back to the crystallization device 40 through the second connecting device 30, the solution concentration of the reflux liquid has been reduced, and in order to maintain the saturation of the crystallization solution, in an embodiment, the dissolving device 10 comprises a feeding bin 12 and a peristaltic pump 14, the feeding bin 12 is soaked in the first temperature control liquid of the first temperature control unit 50; the liquid outlet of the peristaltic pump 14, the first connecting device 20, the crystallization device 40, the second connecting device 30, the liquid inlet of the feeding bin 12, the liquid outlet of the feeding bin 12 and the liquid inlet of the peristaltic pump 14 are sequentially communicated to form a closed circulation loop.

[0061] The crystallization raw material is dissolved and added to the reflux liquid through the feeding bin 12 to form a new crystallization solution, and the solute is supplemented in time to ensure the saturation of the crystallization solution. Specifically, the solute can be added quantitatively by a syringe. Under the driving of the peristaltic pump 14, the flow rate of the crystallization solution and the reflux liquid is 5-20 ml / min. By setting this way, it is ensured that the feeding bin 12, the peristaltic pump 14 and the first temperature control unit 50 are in full contact, the first connecting device 20, the second connecting device 30 and the second temperature control unit 60 are in full contact, and the crystallization device 40 and the third temperature control unit 70 are in full contact, so that the temperature of the crystallization solution and the temperature of the reflux liquid are both changed in a gradient, and the crystallization solution can be slowly crystallized.

[0062] In an embodiment, the peristaltic pump 14, the heating coil and the temperature sensing rod are uniformly and coordinately controlled by a PLC controller, and the temperature and the flow rate are monitored by the PLC controller.

[0063] When the crystallization raw material is dissolved in the replenishment tank 12, if the crystallization raw material is not dissolved sufficiently, the crystallization raw material is easy to form raw material particles, in order to avoid the influence of the raw material particles on the crystallization process. In an embodiment, the dissolving device 10 further comprises a first filter 16 arranged in the replenishment tank 12, wherein a filter membrane with a pore size of 0.22 μm is arranged in the first filter 16. By arranging the first filter 16, the raw material particles can be filtered out, and it is ensured that the crystallization raw material in the crystallization solution is sufficiently dissolved, so that the quality of the crystallization target product can be further improved.

[0064] In an embodiment, the crystallization device 40 comprises a growth container 42 and a crystal growth platform 44, the growth container 42 is immersed in the third temperature control liquid of the third temperature control unit 70, the top of the growth container 42 is provided with an inlet, the bottom end of the growth container 42 is provided with an outlet, the inlet is communicated with the first connecting device 20, and the outlet is communicated with the second connecting device 30, the crystal growth platform 44 is arranged in the growth container 42, and the crystal growth platform 44 is located below the inlet. The growth container 42 can be made of quartz material, the upper end of the growth container 42 can be an open top, which is the inlet, and the bottom end of the growth container 42 forms the outlet. The crystal growth platform 44 is located above the outlet and below the inlet, the crystallization solution flowing out of the inlet falls or drips onto the crystal growth platform 44, and the crystal growth platform 44 is placed with a crystallization seed crystal. The crystallization seed crystal grows into a crystallization target product under the action of the crystallization solution. Through the above structure, the crystallization solution and the crystallization seed crystal are in sufficient contact, and when the crystallization solution crystallizes with crystallization impurities, the crystallization impurities can be separated.

[0065] In order to separate the crystallization impurities, in an embodiment, the crystallization device 40 further comprises a second filter 46 arranged at the outlet. The second filter 46 can be in the shape of a funnel, and specifically, a filter membrane with a pore size of 0.22 μm is arranged in the second filter 46. One end of the second filter 46 is provided with a hook, and the second filter 46 is hung on the growth container 42 through the hook. The crystal growth platform 44 is also fixed on the growth container 42 through a fixing structure and located above the second filter 46.

[0066] In an embodiment, the first connecting device 20 comprises a first spiral pipe 22, and the second connecting device 30 comprises a second spiral pipe 32; the outlet of the dissolving device 10, the first spiral pipe 22, the crystallization device 40, the second spiral pipe 32 and the liquid return port of the dissolving device 10 are sequentially communicated to form a closed circulation loop; the first spiral pipe 22 and the second spiral pipe 32 are immersed in the second temperature control liquid of the second temperature control unit 60.

[0067] The first spiral pipe 22 and the second spiral pipe 32 are made of quartz. The first spiral pipe 22 and the second spiral pipe 32 are arranged along the vertical direction. In this way, the contact area and the contact length of the first spiral pipe 22, the second spiral pipe 32 and the second temperature control liquid are increased, so that the flow path of the crystallization solution in the first spiral pipe 22 and the flow path of the reflux liquid in the second spiral pipe 32 are increased, and the second temperature control liquid can fully heat the crystallization solution and the reflux liquid, respectively.

[0068] Please refer to Figure 4 and Figure 5 In an embodiment, when the number of the first spiral pipe 22 and the second spiral pipe 32 is multiple, the first spiral pipes 22 are connected in series, the second spiral pipes 32 are connected in series, and the first connecting device 20 further comprises a first joint assembly 24. Any two adjacent first spiral pipes 22 are connected through the first joint assembly 24. Specifically, the first joint assembly 24 comprises a first hose 242 and two first buckles 244. One end of the first hose 242 is connected to one first spiral pipe 22 through one first buckle 244, and the other end of the first hose 242 is connected to another first spiral pipe 22 through another first buckle 244.

[0069] The first hose 242 is a corrosion-resistant hose. Through the above structure, the first spiral pipe 22 is arranged conveniently, and the first spiral pipe 22 is more convenient to install.

[0070] In an embodiment, the first joint assembly 24 further comprises a second buckle 246 and a third filter 248. The first hose 242 comprises a first pipe segment 2422 and a second pipe segment 2424. One end of the first pipe segment 2422 is connected to one first spiral pipe 22 through one first buckle 244, and the other end of the first pipe segment 2422 is connected to one end of the third filter 248 through one second buckle 246. One end of the second pipe segment 2424 is connected to another first spiral pipe 22 through another first buckle 244, and the other end of the second pipe segment 2424 is connected to the other end of the third filter 248 through another second buckle 246. That is, the third filter 248 is installed between the two second buckles 246.

[0071] The third filter 248 is provided with a filter membrane with a pore size of 0.22 μm. Through the third filter 248, impurities in the crystallization solution can be filtered out, and the quality of the crystallization target product can be further improved.

[0072] In an embodiment, the second connecting device 30 further comprises a second joint assembly 34. Any two adjacent second spiral pipes 32 are connected through the second joint assembly 34. The structure of the second joint assembly 34 is the same as or similar to that of the first joint assembly 24, and details are not repeated here.

[0073] In an embodiment, the crystallization device 40 further comprises a third joint assembly 48, the first spiral pipe 22 adjacent to the growth container 42 is connected to the growth container 42 through the third joint assembly 48. Specifically, the third joint assembly 48 comprises a third hose 482 and a third buckle 484, one end of the third hose 482 is connected to the first spiral pipe 22 through the third buckle 484, and the other end of the third hose 482 extends into the growth container 42. The growth container 42 contains a crystallization solution, and the third hose 482 extends into the crystallization solution to avoid large fluctuations in the liquid level of the crystallization solution in the growth container 42. By providing the first joint assembly 24, the second joint assembly 34, and the third joint assembly 48, the connection between each of the first container, the second container, and the third container is more convenient, and the sealing performance is guaranteed.

[0074] The first buckle 244, the second buckle 246, and the third buckle 484 are all in the form of a clamp structure, which comprises two semicircular connecting rings and a screw. One end of each of the two connecting rings is hingedly connected, and the other end of each of the two connecting rings is detachably connected through the screw. After the other ends of the two connecting rings are connected, a circular ring is formed.

[0075] In an embodiment, the dissolving device 10 further comprises a fourth joint assembly 17, which is arranged between a second spiral pipe 32 adjacent to the first container and the first container.

[0076] In an embodiment, the dissolving device 10 further comprises a fifth joint assembly 18, which is arranged between a first spiral pipe 22 adjacent to the first container and the first container. The fourth joint assembly 17 and the fifth joint assembly 18 can have the same or similar structure as the third joint assembly 48, and thus will not be described here.

[0077] Embodiments of the present application also provide a crystal growth method using the solution method crystal growth system 100 described above, which comprises the following steps:

[0078] S1, providing a crystallization solution by the dissolving device 10;

[0079] S2, flowing the crystallization solution in the dissolving device 10 to the crystallization device 40 through the first connecting device 20;

[0080] S3, growing a crystallization seed in the crystallization device 40 by flowing the crystallization solution through the crystallization device 40, and forming a reflux liquid;

[0081] S4, flowing the reflux liquid to the dissolving device 10 through the second connecting device 30;

[0082] S5, repeating the above steps, i.e., repeating steps S1 to S4, until the crystallization seed in the crystallization device 40 grows into a target crystal product.

[0083] The crystal growth method of the embodiment also has the above advantages, which are not described herein again.

[0084] Finally, it should be noted that: the above examples are only used to illustrate the technical solutions of the present application, but not to limit them; under the idea of the present application, the technical features of the above examples or different examples can also be combined, the steps can be implemented in any order, and there are many other changes of different aspects of the present application as described above, which are not provided in details for simplicity; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that: the technical solutions recorded in the foregoing examples can still be modified, or some technical features can be replaced by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A solution crystal growth system, characterized by, The device comprises a dissolving device, a first connecting device, a second connecting device, a crystallizing device, a first temperature control unit, a second temperature control unit and a third temperature control unit; The outlet of the dissolving device, the first connecting device, the crystallizing device, the second connecting device and the return liquid outlet of the dissolving device are sequentially communicated to form a closed circulation loop, the crystallizing solution flows through the outlet of the dissolving device, the first connecting device and the crystallizing device, and the return liquid flows through the crystallizing device, the second connecting device and the return liquid outlet of the dissolving device; The dissolving device and the first temperature control unit are in thermal connection, the first connecting device and the second connecting device are in thermal connection with the second temperature control unit, and the crystallizing device is in thermal connection with the third temperature control unit; The temperature of the first temperature control unit, the temperature of the second temperature control unit and the temperature of the third temperature control unit are sequentially increased or sequentially decreased.

2. The solution method crystal growth system according to claim 1, characterized by, The second temperature control unit comprises a first temperature control module and a second temperature control module, the first connecting device is in thermal connection with the first temperature control module, and the second connecting device is in thermal connection with the second temperature control module; The temperature of the first temperature control unit, the temperature of the first temperature control module and the temperature of the third temperature control unit are sequentially increased, and the temperature of the first temperature control unit, the temperature of the second temperature control module and the temperature of the third temperature control unit are sequentially increased. Alternatively, the temperature of the first temperature control unit, the temperature of the first temperature control module and the temperature of the third temperature control unit are sequentially decreased, and the temperature of the first temperature control unit, the temperature of the second temperature control module and the temperature of the third temperature control unit are sequentially decreased.

3. The solution method crystal growth system according to claim 1, wherein, The number of the first connecting devices, the number of the second connecting devices and the number of the second temperature control units are at least two respectively and one-to-one corresponding, each second temperature control unit is in thermal connection with a corresponding first connecting device and a corresponding second connecting device; In the flow direction of the crystallizing solution, the temperature of each second temperature control unit is sequentially increased or sequentially decreased.

4. The solution method crystal growth system according to claim 1, wherein The first temperature control unit comprises a first container and a first temperature control assembly, the first container is used for containing a first temperature control liquid, and the first temperature control assembly is used for controlling the temperature of the first temperature control liquid, and the dissolving device is immersed in the first temperature control liquid; The second temperature control unit comprises a second container and a second temperature control assembly, the second container is used for containing a second temperature control liquid, and the second temperature control assembly is used for controlling the temperature of the second temperature control liquid, and the first connecting device and the second connecting device are immersed in the second temperature control liquid; The third temperature control unit comprises a third container and a third temperature control assembly, the third container is used for containing a third temperature control liquid, and the third temperature control assembly is used for controlling the temperature of the third temperature control liquid, and the crystallizing device is immersed in the third temperature control liquid; The temperature of the first temperature control liquid, the temperature of the second temperature control liquid and the temperature of the third temperature control liquid are sequentially increased or sequentially decreased.

5. The solution method crystal growth system according to claim 4, wherein The dissolving device comprises a feeding bin and a peristaltic pump, and the feeding bin is immersed in the first temperature control unit; The liquid outlet of the peristaltic pump, the first connecting device, the crystallization device, the second connecting device, the liquid return outlet of the feeding bin, the liquid outlet of the feeding bin and the liquid return outlet of the peristaltic pump are sequentially communicated to form a closed circulation loop.

6. The solution method crystal growth system according to claim 5, wherein The dissolving device further comprises a first filter arranged in the feeding bin.

7. The solution method crystal growth system according to claim 1, wherein The crystallization device comprises a growth container and a crystal growth platform, the growth container is immersed in the third temperature control unit, the top of the growth container is provided with a liquid inlet, the bottom of the growth container is provided with a liquid outlet, the liquid inlet is communicated with the first connecting device, the liquid outlet is communicated with the second connecting device, and the crystal growth platform is arranged in the growth container and located below the liquid inlet.

8. The solution method crystal growth system according to claim 7, wherein, The crystallization device further comprises a second filter arranged in the liquid outlet.

9. The solution method crystal growth system according to claim 1, wherein, The first connecting device comprises a first spiral pipe, and the second connecting device comprises a second spiral pipe. The liquid outlet of the dissolving device, the first spiral pipe, the crystallization device, the second spiral pipe and the liquid return outlet of the dissolving device are sequentially communicated to form a closed circulation loop. The first spiral pipe and the second spiral pipe are immersed in the second temperature control unit.

10. A crystal growth method using the solution method crystal growth system according to claim 1, characterized by Comprise: A crystallization solution is provided by a dissolving device; The crystallization solution in the dissolving device flows to the crystallization device through a first connecting device; The crystallization solution flows through the crystallization device to grow a crystallization seed crystal at the crystallization device and form a backflow liquid; The backflow liquid flows to the dissolving device through the second connecting device; The above steps are repeated until the crystallization seed crystal at the crystallization device is grown into a crystallization target product.

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