Stirring device and crystallization purification system

Abstract

The utility model discloses a stirring device and a crystallization purification system, and solves the technical problems of insufficient impurity diffusion and low segregation purification efficiency in the purification process of a crystallization method in the prior art. A stirring device comprises a support, two lifting mechanisms, a stirring mechanism, a water bath mechanism and a driving mechanism, and the stirring mechanism comprises a stirring column and a spiral piece arranged on the stirring column; the water bath mechanism is correspondingly communicated with the water bath inlet and the water bath outlet; the driving end of the driving mechanism is connected with the stirring column to drive the stirring column to rotate; under the condition that the lifting mechanism drives the stirring mechanism to ascend, the driving mechanism drives the stirring mechanism to rotate in a first direction; and under the condition that the lifting mechanism drives the stirring mechanism to descend, the driving mechanism drives the stirring mechanism to rotate in a second direction opposite to the first direction. According to the stirring column, under the combined action of the lifting mechanism and the driving mechanism, the vertical stirring speed and the rotating speed of the stirring column are controlled, and the stirring efficiency and the segregation effect are improved.

Description

Technical Field

[0001] This application belongs to the field of crystallization technology, specifically relating to a stirring device and a crystallization purification system. Background Technology

[0002] Gallium (Ga) is a rare dispersed metal with a low melting point and a high boiling point. Its melting point is only 29.76°C, while its boiling point is as high as 2403°C. It has an extremely wide liquid temperature range, making it suitable for high-temperature applications. The density of liquid gallium is approximately 6.1 g / cm³. 3 Gallium has a high surface tension and easily wets materials such as glass. There are no independent gallium deposits; it is mainly extracted or recovered from bauxite (a byproduct of the aluminum industry), sphalerite (from zinc smelting), and gallium-based waste.

[0003] Gallium metal is primarily used in semiconductor materials, alloys, medical applications, and liquid metals. In recent years, gallium-based semiconductor materials, led by gallium arsenide (GaAs) and gallium nitride (GaN), have seen rapid development in applications such as 5G communications, fast charging, LEDs, and radar. However, due to the specific requirements of the semiconductor field, the purity of gallium must reach 7N or higher. Impurities such as iron (Fe), copper (Cu), and silicon (Si) must be controlled at the ppb level; otherwise, the electron mobility of the semiconductor material or the lifespan of the device will be affected.

[0004] Traditional high-purity gallium purification processes include electrolysis, chemical methods, zone melting, and crystallization. Electrolysis suffers from drawbacks such as high energy consumption, numerous electrolysis cycles, and susceptibility to impurity contamination. Chemical methods are cumbersome and prone to reagent residue. Zone melting is ineffective at removing some impurities (such as sulfur and oxygen), requiring multiple repetitions and resulting in low purification efficiency. Both crystallization and zone melting utilize the segregation mechanism of metal impurities to purify gallium. Crystallization is simple to implement, has a simple equipment structure, and high output. However, crystallization suffers from insufficient impurity diffusion and low segregation purification efficiency, posing challenges to quality control in the industrial production of high-purity gallium. Summary of the Invention

[0005] To address the technical problems of insufficient impurity diffusion and low purification efficiency due to segregation in current crystallization methods, this application provides a stirring device and a crystallization purification system.

[0006] In a first aspect of this application, a stirring apparatus is provided, comprising:

[0007] The support frame consists of two vertical bars and one horizontal bar.

[0008] Two sets of lifting mechanisms, one set of which is located on one of the vertical bars and the other set of which is located on another vertical bar, to jointly drive the horizontal bar to rise or fall;

[0009] A stirring mechanism includes a stirring column and a spiral component disposed on the stirring column. The stirring column has a cavity and a water bath inlet and a water bath outlet communicating with the cavity. The stirring column is used for stirring materials.

[0010] The water bath mechanism is connected to the water bath inlet and the water bath outlet respectively;

[0011] A driving mechanism, wherein the fixed end of the driving mechanism is disposed on the crossbar, and the driving end of the driving mechanism is connected to the stirring column to drive the stirring column to rotate;

[0012] Specifically, when the lifting mechanism drives the stirring mechanism to rise, the driving mechanism drives the stirring mechanism to rotate in a first direction; when the lifting mechanism drives the stirring mechanism to fall, the driving mechanism drives the stirring mechanism to rotate in a second direction, wherein the first direction and the second direction are opposite.

[0013] In some embodiments, the spiral component is a spiral collar, which is sleeved on and connected to the stirring column.

[0014] In some embodiments, the stirring column has a groove on the side near the drive mechanism, and the auger at least partially engages with the groove.

[0015] In some embodiments, the spiral component is integrally formed with the stirring column, and the spiral component protrudes from the stirring column.

[0016] In some embodiments, the lifting mechanism is an electric lifting mechanism or a hydraulic lifting mechanism, with the fixed end of the lifting mechanism connected to the vertical rod and the telescopic end of the lifting mechanism connected to the horizontal rod.

[0017] In some embodiments, the drive mechanism includes a motor, the fixed end of which is connected to the crossbar, and the drive end of which is connected to the stirring column.

[0018] In some embodiments, both the water bath inlet and the water bath outlet are fixedly connected to a flange, and a sealing ring is provided at the flange.

[0019] In some embodiments, the stirring column and / or the spiral collar are made of polytetrafluoroethylene or enamel.

[0020] The bracket, the housing of the lifting mechanism, and / or the housing of the drive mechanism are made of stainless steel.

[0021] In a second aspect of this application, a crystallization purification system is provided, comprising:

[0022] A crystallization and purification container, equipped with a receiving cavity for containing materials;

[0023] The aforementioned stirring device is mounted on the crystallization and purification container, and the stirring mechanism is located in the receiving cavity.

[0024] In some embodiments, the stirring column is provided with a slot on the side near the drive mechanism, and when the lifting mechanism drives the stirring mechanism to descend, the slot is located above the material in the receiving cavity.

[0025] A stirring device and a crystallization purification system are provided according to one or more embodiments of this application. The stirring device includes a support frame, two sets of lifting mechanisms, a stirring mechanism, a water bath mechanism, and a drive mechanism. The support frame includes two vertical rods and a horizontal rod. One set of lifting mechanisms is located on one vertical rod, and the other set of lifting mechanisms is located on the other vertical rod, jointly driving the horizontal rod to rise or fall. The stirring mechanism includes a stirring column and a spiral component located on the stirring column. The stirring column has a cavity and a water bath inlet and outlet communicating with the cavity. The stirring column is used for stirring materials. The water bath mechanism is correspondingly connected to the water bath inlet and outlet. The fixed end of the drive mechanism is located on the horizontal rod, and the driving end of the drive mechanism is connected to the stirring column to drive the stirring column to rotate. When the lifting mechanism drives the stirring mechanism to rise, the drive mechanism drives the stirring mechanism to rotate in a first direction. When the lifting mechanism drives the stirring mechanism to fall, the drive mechanism drives the stirring mechanism to rotate in a second direction, the first direction being opposite to the second direction.

[0026] The stirring column of this application can achieve temperature control by regulating the flow rate and temperature of the circulating water in the water bath mechanism. This temperature control is stable and efficient, while the water circulation heating system is clean and safe. It provides a stable reverse control heat source to suppress supercooled crystallization of gallium, achieving stable crystallization and purification of gallium. A spiral collar is provided at the lower end of the stirring column, allowing for sufficient flow of liquid gallium during stirring. This also makes heating the liquid gallium more efficient, contributing to improved segregation efficiency of impurities during the liquid solidification process. Furthermore, the stirring column, through the combined action of the lifting and driving mechanisms, controls the up-and-down stirring speed and amplitude, as well as the rotation speed, improving stirring efficiency and segregation effect. Attached Figure Description

[0027] Figure 1 A schematic diagram of the crystallization purification system in one or more embodiments of this application is shown.

[0028] Figure 2 A schematic diagram of the stirring device in one or more embodiments of this application is shown.

[0029] Explanation of reference numerals in the attached drawings: 100-stirring device, 110-support, 111-vertical rod, 112-horizontal rod, 120-lifting mechanism, 130-stirring mechanism, 131-stirring column, 1311-cavity, 1312-water bath inlet, 1313-water bath outlet, 132-spiral component, 140-drive mechanism, 200-crystallization and purification system, 210-crystallization and purification container. Detailed Implementation

[0030] To enable those skilled in the art to more clearly understand this application, the technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of the embodiments. Based on the embodiments of this application, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of this application.

[0031] Please see Figure 1 and Figure 2 According to a first aspect of this application, a stirring device 100 is provided, including a support 110, two sets of lifting mechanisms 120, a stirring mechanism 130, a water bath mechanism, and a drive mechanism 140. The support 110 includes two vertical rods 111 and a horizontal rod 112. One set of lifting mechanisms 120 is disposed on one vertical rod 111, and the other set of lifting mechanisms 120 is disposed on the other vertical rod 111, so as to jointly drive the horizontal rod 112 to rise or fall. The stirring mechanism 130 includes a stirring column 131 and a spiral component 132 disposed on the stirring column 131. The stirring column 131 is provided with a cavity 1311, and the stirring column 131 is also provided with a water bath inlet communicating with the cavity 1311. 1312 and water bath outlet 1313, stirring column 131 is used for stirring materials; water bath mechanism is connected to water bath inlet 1312 and water bath outlet 1313 respectively; fixed end of drive mechanism 140 is provided on crossbar 112, drive end of drive mechanism 140 is connected to stirring column 131 to drive stirring column 131 to rotate; wherein, when lifting mechanism 120 drives stirring mechanism 130 to rise, drive mechanism 140 drives stirring mechanism 130 to rotate in a first direction; when lifting mechanism 120 drives stirring mechanism 130 to fall, drive mechanism 140 drives stirring mechanism to rotate in a second direction, the first direction and the second direction are opposite.

[0032] The stirring device 100 of this application can be applied to the stirring of various materials. Taking metallic gallium crystal as an example, the material in this application is gallium crystal.

[0033] The lifting mechanism 120 of the vertical bar 111 on one side and the lifting mechanism 120 of the vertical bar 111 on the other side are symmetrically arranged. The two lifting mechanisms 120 rise or fall synchronously, thereby jointly driving the horizontal bar 112 to rise or fall, that is, driving the stirring mechanism 130 connected to the horizontal bar 112 to rise or fall.

[0034] The water bath mechanism (not shown in the figure) is connected to the corresponding water bath inlet 1312 and water bath outlet 1313 via pipelines to achieve hot water circulation. The pipelines are flexible hoses. When the lifting mechanism 120 drives the stirring mechanism 130 to rise, the drive mechanism 140 drives the stirring mechanism 130 to rotate in a first direction; when the lifting mechanism 120 drives the stirring mechanism 130 to fall, the drive mechanism 140 drives the stirring mechanism to rotate in a second direction. The first and second directions are opposite, meaning the flexible hose of the water bath mechanism rotates in the first direction and then in the second direction to reset, preventing the hose from tangling and ensuring the stability of the overall structure. Furthermore, the stirring column 131 rotates in the first direction during ascent and in the second direction during descent. Under the combined action of the lifting mechanism 120 and the drive mechanism 140, controlling the up-and-down stirring speed and amplitude, as well as the rotation speed of the stirring column 131, can improve stirring efficiency and segregation effect. This application does not limit the specific structure of the water bath mechanism.

[0035] In some embodiments, the temperature of the circulating water introduced into the water bath is controlled between 30 and 38°C, for example, 30°C, 32°C, 34°C, or 38°C. By adjusting the heating efficiency of the stirring column 131 through the water bath, the supercooled crystallization process can be adjusted and controlled, thereby stabilizing the gallium crystallization and purification process.

[0036] Therefore, the stirring column 131 of this application can achieve temperature control by controlling the flow rate and temperature of the circulating water in the water bath mechanism. The temperature control is stable and efficient, and the water circulation heating system is clean and safe, providing a stable reverse control heat source to suppress the supercooling crystallization of metallic gallium, thus achieving stable crystallization and purification of metallic gallium. A spiral collar is provided at the lower end of the stirring column 131, which allows for sufficient flow of liquid metallic gallium during stirring. Simultaneously, the stirring column 131 heats the liquid metallic gallium more efficiently, contributing to improved segregation efficiency of impurities during the liquid solidification process. Furthermore, under the combined action of the lifting mechanism 120 and the driving mechanism 140, the up-and-down stirring speed and amplitude, as well as the rotation speed of the stirring column 131, are controlled, improving stirring efficiency and segregation effect.

[0037] In some embodiments, the spiral member 132 is a spiral collar, which is sleeved on and connected to the stirring column 131. During stirring, the liquid gallium metal flows more fully along the spiral track of the spiral member 132, which helps to improve the segregation efficiency of impurities during the liquid phase solidification process and reduce the impurity content in the liquid gallium metal.

[0038] In some embodiments, the stirring column 131 is provided with a slot on the side near the drive mechanism 140, and the spiral component 132 is at least partially engaged with the slot, that is, the side of the spiral component 132 near the drive mechanism 140 is engaged with the slot, which facilitates quick disassembly and assembly of the spiral component 132 and facilitates cleaning before and after use of the device.

[0039] In some embodiments, the spiral component 132 is integrally formed with the stirring column 131, and the spiral component 132 protrudes from the stirring column 131. The integral design reduces the connection points between the spiral component 132 and the stirring column 131, thereby improving the overall structural stability.

[0040] In some embodiments, the lifting mechanism 120 is an electric lifting mechanism or a hydraulic lifting mechanism. The fixed end of the lifting mechanism 120 is connected to the vertical rod 111, and the telescopic end of the lifting mechanism 120 is connected to the horizontal rod 112. The lifting mechanisms 120 on one side of the vertical rod 111 and the lifting mechanisms 120 on the other side of the vertical rod 111 are symmetrically arranged. The two lifting mechanisms 120 rise or fall synchronously, thereby jointly driving the horizontal rod 112 to rise or fall, that is, driving the stirring mechanism 130 connected to the horizontal rod 112 to rise or fall.

[0041] In some embodiments, the drive mechanism 140 includes a motor, with the fixed end of the motor connected to the crossbar 112 and the drive end of the motor connected to the stirring column 131. That is, by driving the motor to rotate forward or backward, the rotation direction of the stirring column 131 can be adjusted, thereby improving the segregation efficiency of impurities during the liquid phase solidification process.

[0042] In some embodiments, both the water bath inlet 1312 and the water bath outlet 1313 are fixedly connected to a flange, and a sealing ring is fixedly connected to the outside of the flange. This ensures the airtight connection between the water bath mechanism and the cavity 1311 of the stirring column 131.

[0043] In some embodiments, the stirring column 131 and / or the spiral collar are made of polytetrafluoroethylene or enamel material; polytetrafluoroethylene and enamel material have acid and alkali resistance and high temperature resistance, and can be cleaned with strong acid and high-purity water to avoid contamination of the product during the crystallization process.

[0044] In other embodiments, the housings of the support 110, the lifting mechanism 120, and / or the drive mechanism 140 are made of stainless steel, which ensures that the entire device will not rust when operating in an acidic environment, thus ensuring safety and stability during the experiment.

[0045] In the second aspect of this application, as Figure 1 As shown, a crystallization purification system 200 is provided, including a crystallization purification container 210 and the aforementioned stirring device 100. The crystallization purification container 210 is provided with a receiving cavity for containing materials; the aforementioned stirring device 100 is mounted on the crystallization purification container 210, and the stirring mechanism 130 is located in the receiving cavity. In some embodiments, the stirring column 131 is coaxially arranged with the receiving cavity, which ensures that the stirring column 131 partially extends into the receiving cavity and is located in the middle of the receiving cavity. During the rotation and lifting of the stirring column 131, the contact range between the stirring column 131 and the metallic gallium liquid is increased, thereby improving the segregation efficiency of impurities during the liquid phase solidification process.

[0046] In some embodiments, the stirring column 131 is provided with a slot on the side near the drive mechanism 140. When the lifting mechanism 120 drives the stirring mechanism 130 to rise or fall, the slot is located above the material in the receiving cavity. That is, when the stirring column 131 and the slot are not integrally formed, the spiral member 132 engages with the slot to fix the spiral member 132 to the stirring column 131. During the stirring and purification process of the stirring column 131 with the material, the slot is always above the material, preventing the material from flowing into the slot during stirring. This ensures the connection stability between the stirring column 131 and the spiral member 132, and also ensures that the liquid high-purity gallium can flow with the spiral shape of the spiral member 132, which helps the liquid phase gallium to flow fully and allows impurity elements to diffuse fully between the solid and liquid phases of gallium.

[0047] The operation steps of the crystallization purification system 200 of this application are as follows: Metallic gallium (99.99%) is melted and poured into a crystallization purification container 210 for crystallization. A stirring column 131 is immersed in the liquid gallium in the purification container. The temperature of the circulating water in the stirring column 131 is adjusted to maintain a heating temperature range of 30–38°C, thus suppressing excessively rapid crystallization caused by an undercooled crystallization temperature field. The single-cycle crystallization purification time is between 6 and 12 hours, and the crystallization rate during a single-cycle crystallization process is 80–95%. A spiral component 132 is fixed to the lower end of the stirring column 131. The lifting stroke and speed of the lifting mechanism 120 and the rotation speed of the drive mechanism 140 are adjusted. The lifting speed of the stirring column 131 is 1–20 mm / s, and the lifting stroke range is 1–150 mm. The rotation speed is 10–20 rpm. The stirring column 131, with a spiral component 132 fixed at its lower end, stirs back and forth on the liquid gallium metal, thereby achieving sufficient segregation and diffusion of impurity elements during the gallium crystallization and purification process. After completing a single-cycle crystallization, the liquid gallium metal is transferred out of the crystallization container, and the remaining solid gallium is used as raw material to continue the purification of the next crystallization cycle. Depending on the impurity content in the raw material, the above steps can be repeated 2 to 7 times to obtain purified gallium metal.

[0048] In this application, unless otherwise expressly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature being directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature being directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0049] In the description of this application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", and "counterclockwise" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this application.

[0050] In this application, unless otherwise expressly specified and limited, the terms "connection," "fixed," etc., should be interpreted broadly. For example, "fixed" can mean a fixed connection, a detachable connection, or an integral part; it can mean a mechanical connection or an electrical connection; it can mean a direct connection or an indirect connection through an intermediate medium; it can mean the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.

[0051] Furthermore, the use of terms such as "first" and "second" in this application is for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Therefore, features defined with "first" or "second" may explicitly or implicitly include one or more features. In the description of this application, "multiple" means two or more, unless otherwise explicitly specified.

[0052] Although embodiments of this application have been shown and described, those skilled in the art will understand that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of this application, the scope of which is defined by the claims and their equivalents.

Claims

1. A stirring device, characterized in that, include: The support frame consists of two vertical bars and one horizontal bar. Two sets of lifting mechanisms, one set of which is located on one of the vertical bars and the other set of which is located on another vertical bar, to jointly drive the horizontal bar to rise or fall; A stirring mechanism includes a stirring column and a spiral component disposed on the stirring column. The stirring column has a cavity and a water bath inlet and a water bath outlet communicating with the cavity. The stirring column is used for stirring materials. The water bath mechanism is connected to the water bath inlet and the water bath outlet respectively; A driving mechanism, wherein the fixed end of the driving mechanism is disposed on the crossbar, and the driving end of the driving mechanism is connected to the stirring column to drive the stirring column to rotate; Specifically, when the lifting mechanism drives the stirring mechanism to rise, the driving mechanism drives the stirring mechanism to rotate in a first direction; when the lifting mechanism drives the stirring mechanism to fall, the driving mechanism drives the stirring mechanism to rotate in a second direction, wherein the first direction and the second direction are opposite.

2. The stirring device according to claim 1, characterized in that The spiral component is a spiral-shaped collar, which is sleeved on and connected to the stirring column.

3. The stirring device of claim 2, wherein The stirring column is provided with a slot on the side near the driving mechanism, and the spiral component at least partially engages with the slot.

4. The stirring device of claim 1, wherein The spiral component is integrally formed with the stirring column, and the spiral component protrudes from the stirring column.

5. A stirring device according to any one of claims 1-4, characterized in that The lifting mechanism is an electric lifting mechanism or a hydraulic lifting mechanism. The fixed end of the lifting mechanism is connected to the vertical rod, and the telescopic end of the lifting mechanism is connected to the horizontal rod.

6. A stirring device according to any one of claims 1-4, characterized in that The driving mechanism includes a motor, the fixed end of which is connected to the crossbar, and the driving end of which is connected to the stirring column.

7. A stirring device according to any one of claims 1-4, characterized in that Both the water bath inlet and the water bath outlet are fixedly connected to a flange, and a sealing ring is provided at the flange.

8. The stirring device according to any one of claims 1 to 4, characterized in that The stirring column and / or the spiral component are made of polytetrafluoroethylene or enamel material; The bracket, the housing of the lifting mechanism, and / or the housing of the drive mechanism are made of stainless steel.

9. A crystallization purification system characterized by, include: A crystallization and purification container, equipped with a receiving cavity for containing materials; The stirring device according to any one of claims 1-8 is mounted on the crystallization and purification container, and the stirring mechanism is located in the receiving cavity.

10. The crystallization purification system of claim 9, wherein, The stirring column is provided with a slot on the side near the driving mechanism. When the lifting mechanism drives the stirring mechanism to descend, the slot is located above the material in the receiving cavity.

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