CN120905762A - Solution-based crystal growth systems and methods - Google Patents
Solution-based crystal growth systems and methodsInfo
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- CN120905762A CN120905762A CN202511101990.2A CN202511101990A CN120905762A CN 120905762 A CN120905762 A CN 120905762A CN 202511101990 A CN202511101990 A CN 202511101990A CN 120905762 A CN120905762 A CN 120905762A
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Abstract
本发明涉及晶体生长技术领域，公开了一种溶液法晶体生长系统及晶体生长方法，溶液法晶体生长系统包括溶解装置、第一连接装置、第二连接装置、结晶装置、第一温控单元、第二温控单元和第三温控单元；溶解装置的出液口、第一连接装置、结晶装置、第二连接装置和溶解装置的回液口依次连通形成封闭的循环回路，溶解装置的出液口、第一连接装置和结晶装置之间流通结晶溶液，结晶装置、第二连接装置和溶解装置的回液口之间流通回流液；溶解装置和第一温控单元导热连接，第一连接装置和第二连接装置和第二温控单元导热连接，结晶装置和第三温控单元导热连接；第一温控单元的温度、第二温控单元的温度、第三温控单元的温度依次升高或依次下降。
This invention relates to the field of crystal growth technology, and discloses a solution-based crystal growth system and method. The solution-based crystal growth system includes a dissolving device, a first connecting device, a second connecting device, a crystallization 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 crystallization device, the second connecting device, and the return port of the dissolving device are sequentially connected to form a closed loop. A crystallization solution flows between the outlet of the dissolving device, the first connecting device, and the crystallization device, and a reflux liquid flows between the crystallization device, the second connecting device, and the return port of the dissolving device. The dissolving device and the first temperature control unit are thermally connected, as are the first and second connecting devices and the second temperature control unit, and the crystallization device and the third temperature control unit. The temperatures of the first, second, and third temperature control units increase or decrease sequentially.
Description
Technical Field
The invention relates to the technical field of crystal growth, in particular to a solution method crystal growth system and a crystal growth method.
Background
The solution method is a technique for forming an ordered crystal structure by controlling the slow precipitation of solutes from a supersaturated solution. At present, a solution method is generally adopted for growing crystals, and the static solution system method has the following problems that the growth rate of crystals is unstable due to uneven local concentration of the solution, the temperature gradient is single, the preferred orientation growth of crystals is not facilitated, solutes cannot be timely supplemented, and the growth time and the size are limited.
Disclosure of Invention
The embodiment of the invention aims to provide a solution method crystal growth system and a solution method crystal growth method, which are used for solving the technical problem of single temperature gradient in the prior art.
The technical scheme adopted by the embodiment of the invention for solving the technical problems is as follows:
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;
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, crystallization 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 port of the dissolving device;
The dissolving device is in heat conduction connection with the first temperature control unit, the first connecting device is in heat conduction connection with the second connecting device and the second temperature control unit, and the crystallization device is in heat conduction 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.
Optionally, the second temperature control unit includes a first temperature control module and a second temperature control module, the first connection device is in heat conduction connection with the first temperature control module, and the second connection device is in heat conduction 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;
Or 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 reduced, 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 reduced.
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 are in one-to-one correspondence respectively, and each second temperature control unit is in heat conduction connection with a corresponding one of the first connecting devices and a corresponding one of the second connecting devices;
and along the flowing direction of the crystallization solution, the temperature of each second temperature control unit is sequentially increased or sequentially decreased.
Optionally, the first temperature control unit comprises a first container and a first temperature control component, the first container is used for containing a first temperature control liquid, the first temperature control component is used for controlling the temperature of the first temperature control liquid, and the dissolving device is soaked 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 second temperature control liquid, 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 soaked 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 third temperature control liquid, the third temperature control assembly is used for controlling the temperature of the third temperature control liquid, and the crystallization device is soaked 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.
Optionally, the dissolving device comprises a supplementing bin and a peristaltic pump, and the supplementing bin is soaked 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 port of the material supplementing bin, the liquid outlet of the material supplementing bin and the liquid return port of the peristaltic pump are sequentially communicated to form a closed circulation loop.
Optionally, the dissolving device further comprises a first filter, and the first filter is arranged in the supplementing bin.
Optionally, the crystallization device includes growth container and crystal growth platform, the growth container is soaked in the third temperature control unit, the top of growth container is equipped with the inlet, the bottom of growth container is equipped with the liquid outlet, the inlet with first connecting device intercommunication, the liquid outlet with second connecting device intercommunication, the crystal growth platform is established in the growth container, the crystal growth platform is located the below of inlet.
Optionally, the crystallization device further comprises a second filter, and the second filter is arranged at the liquid outlet.
Optionally, the first connection means comprises a first helical tube and the second connection means comprises a second helical tube;
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;
the first spiral tube and the second spiral tube are soaked in the second temperature control unit.
The invention also provides a crystal growth method using the solution method crystal growth system, which comprises the following steps:
providing a crystallization solution by a dissolution device;
The crystallization solution in the dissolution device flows to the crystallization device through a first connection device;
After the crystallization solution flows through the crystallization device, crystal seed crystals at the crystallization device grow, and reflux liquid is formed;
the reflux liquid flows to the dissolving device through the second connecting device;
Repeating the steps until the crystallization seed crystal at the crystallization device grows into a crystallization target product.
Compared with the prior art, in the solution method crystal growth system, the crystallization raw material is dissolved in the dissolution device to form the crystallization solution, the crystallization solution flows to the crystallization device through the first connecting device, the crystallization device is provided with the crystallization seed crystal, the crystallization seed crystal continuously grows in the crystallization solution, and finally, the crystallization target product can be grown. 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, and when the crystallization solution sequentially passes through the dissolving device, the first connecting device and the crystallization device, the contact temperature is in gradient change, so that the crystallization solution can be slowly crystallized, the preferred orientation growth of crystals is facilitated, and the crystallization quality can be improved.
The crystal growth method of the present invention also has the above advantages and will not be described in detail herein.
Drawings
One or more embodiments are illustrated by way of example and not limitation in the figures of the accompanying drawings, in which like references indicate similar elements, and in which the figures of the drawings are not to be taken in a limiting sense, unless otherwise indicated.
FIG. 1 is a schematic diagram of a solution crystal growth system according to an embodiment of the present invention;
FIG. 2 is a cross-sectional view of a solution-process crystal growth system in accordance with one embodiment of the present invention;
FIG. 3 is another cross-sectional view of a solution-process crystal growth system according to one embodiment of the present invention;
FIG. 4 is a schematic view of a first connector assembly according to an embodiment of the present invention;
Fig. 5 is a schematic structural view of a third joint assembly according to an embodiment of the invention.
Reference numerals:
100. Solution-process crystal growth system 10, dissolution device 12, replenishment bin 14, peristaltic pump 16, first filter 17, fourth joint assembly 18, fifth joint assembly 20, first connection device 22, first spiral tube 24, first joint assembly 242, first hose 2422, first pipe segment 2424, second pipe segment 244, first buckle 246, second buckle 248, third filter 30, second connection device 32, second spiral tube 40, crystallization device 42, growth container 44, crystal growth stage 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
In order that the invention may be readily understood, a more particular description thereof will be rendered by reference to specific embodiments that are illustrated in the appended drawings. It will be understood that when an element is referred to as being "connected" to another element, it can be directly on the other element or one or more intervening elements may be present therebetween. The terms "upper," "lower," "left," "right," "upper," "lower," "top," and "bottom," and the like, as used herein, refer to an orientation or positional relationship based on that shown in the drawings, merely for convenience in describing the present invention and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Unless defined otherwise, 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 invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Referring to fig. 1, a solution crystal growth system 100 according to an embodiment of the invention includes a dissolution device 10, a first connection device 20, a second connection device 30, a crystallization device 40, a first temperature control unit 50, a second temperature control unit 60 and a third temperature control unit 70, wherein a liquid outlet of the dissolution device 10, the first connection device 20, the crystallization device 40, the second connection device 30 and a liquid return port of the dissolution device 10 are sequentially communicated to form a closed circulation loop, crystallization solution is circulated between the liquid outlet of the dissolution device 10, the first connection device 20 and the crystallization device 40, reflux liquid is circulated between the crystallization device 40, the second connection device 30 and the liquid return port of the dissolution device 10, the dissolution device 10 is in heat conduction connection with the first temperature control unit 50, the first connection device 20 is in heat conduction connection with the second connection device 30 and the second temperature control unit 60, the crystallization device 40 is in heat conduction connection with the third temperature control unit 70, and 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.
In the embodiment, the dissolving device 10 is in heat conduction connection with the first temperature control unit 50, the first connecting device 20 is in heat conduction connection with the second connecting device 30 and the second temperature control unit 60, and the crystallizing device 40 is in heat conduction connection with the third temperature control unit 70, wherein the dissolving device 10 is soaked in the first temperature control unit 50, the first connecting device 20 is soaked in the second temperature control unit 60, and the crystallizing device 40 is soaked in the third temperature control unit 70.
The solution crystal growth system 100 of this embodiment works on the principle that a crystallization raw material is dissolved in a dissolution device 10 to form a crystallization solution, the crystallization solution flows to a crystallization device 40 through a first connection device 20, a crystallization seed crystal is placed in the crystallization device 40, and the crystallization seed crystal continuously grows in the crystallization solution, and can finally grow into a crystallization target product. The source of the crystallization seed can be added from outside or can be generated by crystallization solution. The crystallization solution is used to form crystallization seeds by forming crystallization particles at the crystallization device 40 when the crystallization solution passes through the crystallization device 40, and selecting better crystallization particles as crystallization seeds. The crystallization solution flows through the crystallization device 40 to form a reflux liquid, and the reflux liquid flows back to the dissolution device 10 through the second connection device 30, and the dissolution device 10 supplements the reflux liquid with the crystallization raw material to form a new crystallization solution. When the characteristic of the crystallization raw material is temperature-rising 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 characteristic of the crystallization raw material is cooling 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.
In a specific embodiment, the raw materials for the temperature-rising crystallization can be lead bromide (PbBr 2) and methyl ammonium bromide (MABr), and the crystal target product is methyl amine lead bromide (MAPbBr 3).
Lead bromide (PbBr 2) and methyl ammonium bromide (MABr) were ultrasonically dissolved in the thf (N, N-dimethylformamide) solution by the dissolution device 10 and then injected into the first connection device 20. Wherein the temperature of the first temperature control unit 50 is 50 ℃, the temperature of the second temperature control unit 60 is 70 ℃, and the temperature of the third temperature control unit 70 is 90 ℃. After fine crystal particles are grown in the crystallization device 40 from the crystallization solution, better crystal particles are selected as crystal seeds, and the crystal seeds continuously grow in the crystallization solution to form a crystallization target product.
In a specific embodiment, the source material for the reduced temperature crystallization may be methylamine iodide (MAI), lead acetate trihydrate (Pb (CH 3COO)2.3H2 O), and the crystalline target product is lead methylamine iodide (MAPbI 3).
Methylamine iodide (MAI) and lead acetate trihydrate (Pb (CH 3COO)2.3H2 O) are dissolved in HI (hydrogen iodide) solution by a dissolving device 10 and then flow into a circulation loop at a first connecting device 20, wherein the temperature of the first temperature control unit 50 is 90 ℃, the temperature of the second temperature control unit 60 is 70 ℃, and the temperature of the third temperature control unit 70 is 50 ℃.
In the solution 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 dissolution device 10, the first connection device 20, and the crystallization device 40, the contact temperature thereof is changed in a gradient manner, so that the crystallization solution can be slowly crystallized, which is beneficial to the growth of the preferred crystal orientation, thereby improving the quality of the crystallization.
When the first and second connection means 20 and 30 and the second temperature control unit 60 are thermally connected, the temperature of the crystallization solution in the first connection means 20 and the temperature of the reflux liquid in the second connection means 30 may be the same or different. However, in order to meet the needs of different users, in an embodiment, the second temperature control unit 60 includes a first temperature control module 62 and a second temperature control module 64, the first connection device 20 is in heat conduction connection with the first temperature control module 62, the second connection device 30 is in heat conduction connection with the second temperature control module 64, the temperature of the first temperature control unit 50, the temperature of the first temperature control module 62, the temperature of the third temperature control unit 70 sequentially increase, 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 sequentially increase, 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 sequentially decrease, 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 sequentially decrease. The temperature of the first temperature control module 62 and the temperature of the second temperature control module 64 may 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 is different from the temperature of the second temperature control module 64, 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 that the temperature of the crystallization solution and the temperature of the reflux liquid can be finely adjusted, the temperature changes of the crystallization solution and the reflux liquid can be accurately controlled, and the growth quality of the crystallization target product can be further improved.
In an embodiment, the number of the first connection devices 20, the number of the second connection devices 30 and the number of the second temperature control units 60 are at least two and correspond to each other one by one, each of the second temperature control units 60 is in heat conduction connection with a corresponding one of the first connection devices 20 and a corresponding one of the second connection devices 30, and the temperatures of the second temperature control units 60 are sequentially increased or sequentially decreased along the flowing direction of the crystallization solution. That is, the number of the second temperature control units 60 may be plural, and each of the second temperature control units 60 is provided with one first connecting device 20 and one second connecting device 30, respectively, and the temperatures of the respective second temperature control units 60 are also sequentially increased or sequentially decreased along the flowing direction of the crystallization solution. This arrangement allows the crystallization solution to be slowly increased or decreased in temperature as it passes through each of the first connecting means 20. The temperature of the crystallization solution is slowly increased or decreased while passing the reflux liquid through each of the second connecting means 30. The growth quality of the crystallization target product can be further improved.
In a specific embodiment, when the crystallization raw material is temperature-raised crystallization, the number of the second temperature control units 60 is 4. The temperature of the first temperature control unit 50 is 50C, the temperature of each second temperature control unit 60 is 60C, 65C, 70C, 75C, respectively, and the temperature of the third temperature control unit 70 is 90C, along the flow direction of the crystallization solution. The arrangement is such that the crystallization solution, as it flows from dissolution apparatus 10 to crystallization apparatus 40, slowly increases in temperature to achieve slow crystallization.
In another specific embodiment, when the crystallization starting material is cooled down crystallization, the number of the second temperature control units 60 is 4. The temperature of the first temperature control unit 50 is 90 ℃, the temperature of each second temperature control unit 60 is 75 ℃, 70 ℃, 65 ℃ and 60 ℃ along the flowing direction of the crystallization solution, and the temperature of the third temperature control unit 70 is 50 ℃. The arrangement is such that the crystallization solution is slowly cooled as it flows from dissolution apparatus 10 to crystallization apparatus 40 to achieve slow crystallization.
In an embodiment, each of the second temperature control units 60 includes a first temperature control module 62 and a second temperature control module 64, respectively. In a specific embodiment, as shown in fig. 1, the number of the second temperature control units 60 is four, and each second temperature control unit 60 includes a first temperature control module 62 and a second temperature control module 64.
In one embodiment, the first temperature control unit 50 includes 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, the dissolution device 10 is immersed in the first temperature control liquid, the second temperature control unit 60 includes 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, the first connection device 20 and the second connection device 30 are immersed in the second temperature control liquid, and the third temperature control unit 70 includes 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 respectively. The first temperature control assembly, the second temperature control assembly and the third temperature control assembly respectively comprise a temperature detection rod and a heating coil, wherein the temperature detection rod is respectively arranged in the first container, the second container and the third container, the heating coil is wound around the peripheral surfaces of the first container, the second container and the third container, or the heating coil is arranged at the bottom ends of the first container, the second container and the third container. The heating coil is used for heating the first container, the second container and the third container, and controlling the temperature of the first temperature control liquid, the second temperature control liquid and the third temperature control liquid according to the temperature indication of the temperature detection rod.
When the second temperature control unit 60 includes the first temperature control module 62 and the second temperature control module 64, the second container is partitioned by a partition to form a first accommodating groove and a second accommodating groove, and the first accommodating groove and the second accommodating groove are respectively provided with a temperature detecting rod. The first temperature control module 62 includes a first accommodating groove and a temperature detecting rod, and the second temperature control module 64 includes a second accommodating groove and another temperature detecting rod.
Through setting up above-mentioned structure, can carry out accurate control to the temperature in first container, second container and the three container, make the temperature of first temperature control liquid, the temperature of second temperature control liquid, the temperature of third temperature control liquid can slowly rise in proper order or descend in proper order to can further improve the growth quality of crystallization target product.
Referring to fig. 2 and 3, when the reflux liquid is refluxed to the crystallization device 40 through the second connection device 30, the solution concentration of the reflux liquid is reduced to maintain the saturation degree of the crystallization solution. In an embodiment, the dissolving device 10 comprises a feeding bin 12 and a peristaltic pump 14, wherein the feeding bin 12 is soaked in a first temperature control liquid of the first temperature control unit 50, and a liquid outlet of the peristaltic pump 14, the first connecting device 20, the crystallization device 40, the second connecting device 30, a liquid return port of the feeding bin 12, a liquid outlet of the feeding bin 12 and a liquid return port of the peristaltic pump 14 are sequentially communicated to form a closed circulation loop.
The crystallization raw material is dissolved and added into the reflux liquid through the supplementing bin 12, a new crystallization solution is formed, solute is timely supplemented, and the saturation of the crystallization solution is ensured. Specifically, the solute may be dosed via a syringe. Under the driving of the peristaltic pump 14, the flow rates of the crystallization solution and the reflux liquid are 5-20 ml/min, so that the situation that the material supplementing bin 12 and the peristaltic pump 14 are respectively and fully contacted with the first temperature control unit 50, the first connecting device 20 and the second connecting device 30 are respectively and fully contacted with the second temperature control unit 60, and the crystallization device 40 and the third temperature control unit 70 are fully contacted is ensured, so that the temperature of the crystallization solution and the temperature of the reflux liquid are both in gradient change, and the crystallization solution can be slowly crystallized.
In one embodiment, peristaltic pump 14, heating coil and temperature probe are cooperatively controlled by a PLC controller, through which temperature and flow are monitored.
When the crystal raw material is dissolved in the replenishing bin 12, if the crystal raw material is not sufficiently dissolved, raw material particles are easily formed in the crystal raw material, so that the influence of the raw material particles on the crystallization process is avoided. In one embodiment, the dissolving apparatus 10 further comprises a first filter 16, the first filter 16 being disposed in the replenishment cartridge 12, wherein a filtration membrane having a pore size of 0.22 μm is disposed in the first filter 16. By providing the first filter 16, the material particles can be filtered out, and the crystallization material in the crystallization solution can be sufficiently dissolved, so that the quality of the crystallization target product can be further improved.
In one embodiment, the crystallization device 40 includes a growth container 42 and a crystal growth stage 44, the growth container 42 is immersed in the third temperature control liquid of the third temperature control unit 70, a liquid inlet is disposed at the top of the growth container 42, a liquid outlet is disposed at the bottom end of the growth container 42, the liquid inlet is communicated with the first connecting device 20, the liquid outlet is communicated with the second connecting device 30, the crystal growth stage 44 is disposed in the growth container 42, and the crystal growth stage 44 is located below the liquid inlet. The growth container 42 may be made of quartz material, and the upper end of the growth container 42 may be an opening, which is a liquid inlet, and the bottom end of the growth container 42 forms a liquid outlet. The crystal growth stage 44 is located above the liquid outlet and below the liquid inlet, and the crystallization solution flowing out of the liquid inlet drips or drips onto the crystal growth stage 44, and the crystal growth stage 44 is placed with a crystallization seed crystal thereon. The crystallization seed crystal grows into a crystallization target product under the action of the crystallization solution. By the above structure, the crystallization solution and the crystallization seed are brought into sufficient contact, and when the crystallization solution is crystallized with the crystallization impurity, the crystallization impurity can be separated.
In order to separate the crystallized impurities, in one embodiment, the crystallization device 40 further includes a second filter 46, and the second filter 46 is disposed at the liquid outlet. The second filter 46 may be funnel-shaped, and specifically, a filtering membrane having a pore size of 0.22 μm is disposed 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 by the hook. The crystal growing stage 44 is also secured to the growth vessel 42 by a securing structure and is positioned above the second filter 46.
In one embodiment, the first connecting device 20 comprises a first spiral pipe 22, the second connecting device 30 comprises a second spiral pipe 32, the liquid 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, and the first spiral pipe 22 and the second spiral pipe 32 are soaked in the second temperature control liquid of the second temperature control unit 60.
Wherein the first spiral tube 22 and the second spiral tube 32 are respectively made of quartz materials. The first spiral pipe 22 and the second spiral pipe 32 are disposed in the vertical direction, respectively. By this arrangement, the contact area and the contact length of the first spiral pipe 22, the second spiral pipe 32, and the second temperature-controlled liquid can be increased, so that the flow path of the crystallization solution in the first spiral pipe 22 can be increased, the flow path of the reflux liquid in the second spiral pipe 32 can be increased, and the second temperature-controlled liquid can sufficiently transfer heat to the crystallization solution and the reflux liquid, respectively.
Referring to fig. 4 and fig. 5 together, in an embodiment, when the number of the first spiral pipes 22 and the second spiral pipes 32 is plural, each of the first spiral pipes 22 is sequentially connected in series, each of the second spiral pipes 32 is sequentially connected in series, and the first connecting device 20 further includes a first joint assembly 24, and any two adjacent first spiral pipes 22 are connected by the first joint assembly 24. Specifically, the first connector assembly 24 includes a first hose 242 and two first clamps 244, one end of the first hose 242 is connected to one first coil 22 by one first clamp 244, and the other end of the first hose 242 is connected to the other first coil 22 by the other first clamp 244.
Wherein the first hose 242 is a corrosion resistant hose. With the above structure, the arrangement of the first spiral pipe 22 is facilitated, making the first spiral pipe 22 more convenient to install.
In one embodiment, the first joint assembly 24 further includes a second clasp 246 and a third filter 248, the first hose 242 includes a first pipe section 2422 and a second pipe section 2424, one end of the first pipe section 2422 is connected to a first coil 22 through a first clasp 244, the other end of the first pipe section 2422 is connected to one end of the third filter 248 through a second clasp 246, one end of the second pipe section 2424 is connected to the other first coil 22 through the other first clasp 244, the other end of the second pipe section 2424 is connected to the other end of the third filter 248 through the other second clasp 246, i.e., the third filter 248 is mounted between the two second clasps 246.
Wherein a filter membrane having a pore size of 0.22 μm is provided in the third filter 248. By providing 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.
In an embodiment, the second connecting device 30 further includes a second joint assembly 34, and any two adjacent second spiral pipes 32 are connected by the second joint assembly 34, and the structure of the second joint assembly 34 is the same as or similar to that of the first joint assembly 24, which is not described herein.
In one embodiment, crystallization apparatus 40 further includes a third joint assembly 48, and first coil 22 adjacent growth container 42 is connected to growth container 42 by third joint assembly 48. Specifically, the third joint assembly 48 includes a third hose 482 and a third clasp 484, one end of the third hose 482 is connected to the first coil 22 by the third clasp 484, and the other end of the third hose 482 extends into the growth container 42. The crystallization solution is contained in the growth container 42, and the third hose 482 extends into the crystallization solution, so that the fluctuation of the liquid level of the crystallization solution in the growth container 42 is prevented from being large. By providing the first connector assembly 24, the second connector assembly 34, and the third connector assembly 48, the joints are more convenient to attach the first container, the second container, and the third container, and the tightness is ensured.
The first buckle 244, the second buckle 246 and the third buckle 484 are respectively of a clamp structure, the clamp structure comprises two semicircular connecting rings and screws, one ends of the two connecting rings are hinged and connected, the other ends of the two connecting rings are detachably connected through the screws, and the other ends of the two connecting rings are connected to form a circular ring.
In one embodiment, the dissolution apparatus 10 further includes a fourth connector assembly 17, and the fourth connector assembly 17 may be disposed between a second coil 32 adjacent the first container and the first container.
In an embodiment, the dissolving device 10 further includes a fifth joint assembly 18, and the fifth joint assembly 18 may be disposed between a first spiral tube 22 adjacent to the first container and the first container, wherein the structures of the fourth joint assembly 17 and the fifth joint assembly 18 may be the same as or similar to the third joint assembly 48, and will not be described herein.
The embodiment of the invention also provides a crystal growth method using the solution method crystal growth system 100, which comprises the following steps:
S1, providing a crystallization solution through a dissolving device 10;
S2, the crystallization solution in the dissolving device 10 flows to the crystallization device 40 through the first connecting device 20;
S3, after the crystallization solution flows through the crystallization device 40, crystal seeds at the crystallization device 40 grow, and reflux liquid is formed;
s4, flowing the reflux liquid to the dissolving device 10 through the second connecting device 30;
S5, repeating the steps from S1 to S4 until the crystal seed crystal at the crystallization device 40 grows into a crystallization target product.
The crystal growth method of the present embodiment also has the above advantages, and will not be described here again.
It should finally be noted that the above embodiments are only intended to illustrate the technical solution of the present invention and not to limit it, that the technical features of the above embodiments or of the different embodiments may be combined in any order, and that many other variations in the different aspects of the present invention as described above exist, which are not provided in details for the sake of brevity, and that, although the present invention is described in the detailed description with reference to the foregoing embodiments, it should be understood by those skilled in the art that modifications may be carried out to the technical solution described in the foregoing embodiments or to the equivalent substitution of some of the technical features thereof, where these modifications or substitutions do not depart from the essence of the corresponding technical solution from the scope of the technical solution of the embodiments of the present invention.
Claims (10)
1. The solution method crystal growth system is characterized by 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;
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, crystallization 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 port of the dissolving device;
The dissolving device is in heat conduction connection with the first temperature control unit, the first connecting device is in heat conduction connection with the second connecting device and the second temperature control unit, and the crystallization device is in heat conduction 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 crystal growth system of claim 1, wherein the second temperature control unit comprises a first temperature control module and a second temperature control module, the first connection device and the first temperature control module are in thermally conductive connection, and the second connection device and the second temperature control module are in thermally conductive connection;
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;
Or 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 reduced, 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 reduced.
3. The solution crystal growth system according to claim 1, wherein the number of the first connection devices, the number of the second connection devices, and the number of the second temperature control units are at least two and correspond one to one, respectively, each of the second temperature control units being thermally connected to a corresponding one of the first connection devices and a corresponding one of the second connection devices;
and along the flowing direction of the crystallization solution, the temperature of each second temperature control unit is sequentially increased or sequentially decreased.
4. The solution-process crystal growth system of claim 1, wherein the first temperature-control unit includes a first container for holding a first temperature-control liquid and a first temperature-control assembly for controlling a temperature of the first temperature-control liquid, the dissolution device being 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 second temperature control liquid, 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 soaked 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 third temperature control liquid, the third temperature control assembly is used for controlling the temperature of the third temperature control liquid, and the crystallization device is soaked 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 crystal growth system of claim 4, wherein the dissolution device comprises a replenishment bin and a peristaltic pump, the replenishment bin being 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 port of the material supplementing bin, the liquid outlet of the material supplementing bin and the liquid return port of the peristaltic pump are sequentially communicated to form a closed circulation loop.
6. The solution crystal growth system of claim 5, wherein the dissolving apparatus further comprises a first filter disposed within the replenishment cartridge.
7. The solution crystal growth system according to claim 1, wherein the crystallization device comprises a growth container and a crystal growth stage, the growth container is immersed in the third temperature control unit, a liquid inlet is formed in the top of the growth container, a liquid outlet is formed in 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 stage is arranged in the growth container, and the crystal growth stage is located below the liquid inlet.
8. The solution crystal growth system of claim 7, wherein the crystallization device further comprises a second filter, the second filter being disposed at the liquid outlet.
9. The solution crystal growth system of claim 1, wherein the first connection means comprises a first coil and the second connection means comprises a second coil;
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;
the first spiral tube and the second spiral tube are soaked in the second temperature control unit.
10. A crystal growth method using the solution-process crystal growth system of claim 1, comprising:
providing a crystallization solution by a dissolution device;
The crystallization solution in the dissolution device flows to the crystallization device through a first connection device;
After the crystallization solution flows through the crystallization device, crystal seed crystals at the crystallization device grow, and reflux liquid is formed;
the reflux liquid flows to the dissolving device through the second connecting device;
Repeating the steps until the crystallization seed crystal at the crystallization device grows into a crystallization target product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202511101990.2A CN120905762A (en) | 2025-08-07 | 2025-08-07 | Solution-based crystal growth systems and methods |
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| CN202511101990.2A CN120905762A (en) | 2025-08-07 | 2025-08-07 | Solution-based crystal growth systems and methods |
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- 2025-08-07 CN CN202511101990.2A patent/CN120905762A/en active Pending
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