A zone refining purification apparatus and method
By combining a heater and a slag puller with a vibrator inside a quartz tube, the problem of difficult separation of the surface slag phase in zone melting is solved, achieving efficient and low-cost metal purification, which is suitable for industrial production.
Patent Information
- Application Number
- CN202410540684.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-30
- Publication Date
- 2026-11-06
- Estimated Expiration
- 2044-04-30
AI Technical Summary
In existing zone melting technologies, the surface slag phase is difficult to separate efficiently, which affects the purification effect and quality of the product. Moreover, existing equipment is costly and inefficient, making it unsuitable for large-scale mass production.
The design employs a heater and a scum traction device inside a quartz tube, combined with a vibrator. The heater moves along the length of the quartz tube, the scum traction device moves the surface scum to the tail of the ingot, and the vibrator stirs the molten ingot, thereby improving the efficiency of impurity separation.
It achieves efficient removal of surface impurities, improves product purity, reduces production costs, increases production capacity, and is suitable for industrial-scale production.
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Figure CN118441155B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of metal smelting and purification, and more specifically, to a zone smelting and purification apparatus and method. Background Technology
[0002] Methods for purifying high-purity rare and dispersed metals are broadly classified into physical purification methods and chemical purification methods. Zone melting is one of the most commonly used physical purification methods for high-purity / ultra-high-purity metals. It utilizes the phenomenon of segregation to locally melt the material, forming a narrow molten zone, and then slowly moves it along the length of the ingot from one end to the other. This process is repeated multiple times to concentrate impurities at the head or tail, thereby purifying the material in the middle. Essentially, it utilizes the difference in solubility of impurities in the solidified and molten states of the metal to cause impurities to precipitate or alter their distribution.
[0003] The inventors discovered that existing smelting technologies struggle to efficiently separate surface slag phases. For example, easily oxidized metals like Bi tend to form large slag patches on the surface during zone melting, significantly impacting product purification and quality. Furthermore, current zone melting equipment lacks a device specifically designed for surface slag treatment during this process, leading to difficult and inefficient subsequent processing. This results in high production costs and low capacity for high-purity products, making it unsuitable for large-scale mass production. Additionally, zone melting involves stirring the molten ingots to improve purification. Existing technologies typically employ external magnetic or electric fields, but these methods are ineffective, inefficient, costly, and difficult to separate impurities with separation coefficients close to 1. Summary of the Invention
[0004] The purpose of this invention is to provide a zone melting and purification apparatus and method that can efficiently remove surface impurities and concentrate the impurities at both ends of the ingot, thereby improving the purity of the product.
[0005] The embodiments of the present invention are implemented as follows: In a first aspect, the present invention provides a zone melting and purification apparatus, comprising: A quartz tube, wherein an evaporating dish is disposed inside the quartz tube; A heater for heating the quartz tube to melt the ingot in the evaporating dish, and the heater is movable along the length of the quartz tube; A scum traction device, one end of which is connected to the heater, and the other end is inserted from the end of the quartz tube and located inside the evaporating dish; A vibrator for vibrating the quartz tube; As the heater heats the quartz tube and moves along the quartz tube, the scum puller moves with the heater, and the end of the scum puller located inside the evaporating dish moves the scum on the surface of the molten ingot to the end.
[0006] In an optional embodiment, the scum puller includes a U-shaped rod and a scum scraper. One end of the U-shaped rod is connected to the heater, and the other end is located inside the quartz tube and connected to the scum scraper, which is located inside the evaporating dish.
[0007] In an optional embodiment, the U-shaped rod is threadedly connected to the scraper spoon.
[0008] In an optional embodiment, a flange is provided on the end face of the quartz tube, and an elongated hole is provided on the flange for the U-shaped rod to pass through, and the U-shaped rod can move in the elongated hole.
[0009] In an optional embodiment, the zone melting and purification apparatus further includes bolts and washers, the bolts connecting the washers and the two being located on opposite sides of the elongated hole; The bolt has a through hole in the middle, and the U-shaped rod passes through the through hole.
[0010] In an optional embodiment, the zone melting and purification apparatus further includes a stand, on which the quartz tube is disposed, and on which the heater is movably disposed.
[0011] In an optional embodiment, the zone melting and purification apparatus further includes an outlet pipe and an inlet pipe, which are respectively connected to the two ends of the quartz tube.
[0012] Secondly, the present invention provides a zone melting purification method, based on a zone melting purification apparatus according to any of the foregoing embodiments, comprising: Step S1: Place the metal ingot in an evaporating dish, then place the evaporating dish into a quartz tube, seal both ends with flanges and connect the inlet and outlet pipes respectively, and then introduce nitrogen gas into the quartz tube. Step S2: After ventilating for 2 hours, move the heater to the beginning of the evaporating dish (near the gas inlet of the quartz tube) and turn on the heater to begin melting the metal ingot in the starting area; Step S3: After the ingot has completely melted, adjust the position of the scum puller and turn on the vibrator. Adjust the vibration frequency to slightly stir the liquid surface, and then start moving the heater. The scum puller and the heater move synchronously. The surface scum will move from the head to the tail of the ingot with the scum puller and eventually gather at the tail end of the ingot. When the heater moves from the head to the tail end of the evaporating dish, it is one zone melting purification. Repeat this process many times. After that, most of the scum will be enriched at the tail end of the ingot. Then adjust the height of the scum puller so that it is suspended above the ingot. Step S4: After multiple zone meltings are completed, the metal ingot is taken out, and the head and tail are removed. It is then used as raw material for the next zone melting cycle. Steps S2 and S3 are repeated to obtain a high-purity metal product.
[0013] In an optional implementation, in step S4, the head is removed at 5%-10% of the whole, and the tail is removed at 15%-20% of the whole.
[0014] The beneficial effects of the embodiments of the present invention are: This invention provides a zone melting and purification apparatus, comprising a quartz tube, a heater, a vibrator, and a scum drawer; an evaporating dish is disposed inside the quartz tube; the heater is used to heat the quartz tube to melt the ingot in the evaporating dish, and the heater can move along the length of the quartz tube; one end of the scum drawer is connected to the heater, and the other end is inserted from the end of the quartz tube and located inside the evaporating dish; the vibrator is used to vibrate the quartz tube; when the heater heats the quartz tube and moves along the quartz tube, the scum drawer moves with the heater, and the end of the scum drawer located inside the evaporating dish moves the scum on the surface of the molten ingot to the end.
[0015] This invention features a heater that moves along the length of the quartz tube, allowing the ingot to be gradually melted as the heater moves. Because the heater is connected to a scum traction device that moves with it, when the heater is melting an ingot at a certain position, the scum traction device can move the surface scum at that position to the top of the beam. This design provides advantages such as low cost, high capacity, high purity, and fewer melting cycles for the ingot, which is beneficial for large-scale industrial production. Furthermore, this invention uses a vibrator to vibrate the quartz tube, thereby externally stirring the molten ingot. This accelerates the transport of impurities accumulated in the diffusion layer to the entire melt, reducing the thickness of the diffusion layer and improving the purification effect. Attached Figure Description
[0016] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.
[0017] Figure 1 This is a schematic diagram of a zone melting and purification device provided in an embodiment of the present invention; Figure 2 This is a schematic diagram showing that the ingot is divided into five parts from the beginning to the end after the zone melting is completed, according to an embodiment of the present invention.
[0018] icon: 10-Quartz tube; 20-Evaporating dish; 30-Heater; 40-Scum puller; 41-U-shaped rod; 42-Scum scraper; 50-Flange; 51-Elongated hole; 60-Bolt; 61-Through hole; 70-Gasket; 80-Vibrator; 90-Frame; 100-Inlet pipe; 110-Outlet pipe. Detailed Implementation
[0019] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.
[0020] Therefore, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the invention without inventive effort are within the scope of protection of the invention.
[0021] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.
[0022] In the description of this invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product of this invention is in use. They are only for the convenience of describing this invention 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, and therefore should not be construed as a limitation of this invention. In addition, the terms "first," "second," "third," etc., are only used to distinguish descriptions and should not be construed as indicating or implying relative importance.
[0023] Furthermore, terms such as "horizontal" and "vertical" do not imply that components must be absolutely horizontal or suspended, but rather that they can be slightly tilted. For example, "horizontal" simply means that its direction is more horizontal than "vertical," and does not mean that the structure must be completely horizontal, but can be slightly tilted.
[0024] In the description of this invention, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.
[0025] This embodiment provides a zone melting purification apparatus and method, mainly used to solve the problem that impurities on the surface of ingots cannot be removed during melting, which greatly affects the product purification effect and product quality, as detailed below.
[0026] like Figure 1 As shown, this embodiment provides a zone melting and purification apparatus, including a quartz tube 10, a heater 30, a vibrator 80, and a scum puller 40; an evaporating dish 20 is disposed inside the quartz tube 10; the heater 30 is used to heat the quartz tube 10 to melt the ingot in the evaporating dish 20, and the heater 30 can move along the length of the quartz tube 10; one end of the scum puller 40 is connected to the heater 30, and the other end is inserted from the end of the quartz tube 10 and located inside the evaporating dish 20; the vibrator 80 is used to vibrate the quartz tube 10; when the heater 30 heats the quartz tube 10 and moves along the quartz tube 10, the scum puller 40 moves with the heater 30, and the end of the scum puller 40 located inside the evaporating dish 20 moves the scum on the surface of the molten ingot to the end.
[0027] Specifically, the slag scraping direction of the slag puller 40 is from the air inlet end of the quartz tube 10 to the air outlet end of the quartz tube 10. In detail, during zone melting, the equilibrium distribution coefficient K0 of impurities is the key factor determining their migration. K0 refers to the concentration C of impurities in the solid phase under solid-liquid equilibrium at a certain temperature. S The concentration C of impurities in the liquid phase L The ratio of the two. However, in reality, non-equilibrium solidification often occurs, and the equilibrium distribution coefficient is not constant. Therefore, an effective distribution coefficient K is introduced. eff Its relationship with the equilibrium distribution coefficient is as follows:
[0028] In the formula, K0 is the equilibrium segregation coefficient, f is the melting zone velocity, δ is the diffusion layer thickness, and D is the diffusion coefficient of the impurity element in the material. When fδ / D→0, K eff →K0.
[0029] In actual production, external forces such as rotation, stirring, applying an external magnetic field, and oscillation can be used to accelerate the transport of impurities accumulated in the diffusion layer into the entire melt, thereby reducing the thickness of the diffusion layer and contributing to K eff Approaching K0, it solves the problem of removing impurities with a separation coefficient close to 1.
[0030] It is understood that this embodiment uses a heater 30 that can move along the length of the quartz tube 10 to gradually melt the ingot as the heater 30 moves. Since the present invention has a scum traction device 40 connected to the heater 30 that can move with the heater 30, when the heater 30 melts the ingot at a certain position, the scum traction device 40 can move the surface scum at that position to the end of the beam top. Through the above configuration, the ingot melting has advantages such as low cost, high capacity, high purity, and fewer regional melting times, which is conducive to industrial-scale production.
[0031] It is worth noting that the vibrator 80 in this embodiment provides external force to stir the molten ingot, thereby accelerating the transport of impurities accumulated in the diffusion layer to the entire melt, reducing the thickness of the diffusion layer, and contributing to K eff It tends towards K0, thereby improving the purification effect.
[0032] In a preferred embodiment, the scum puller 40 includes a U-shaped rod 41 and a scum scraper 42. One end of the U-shaped rod 41 is connected to the heater 30, and the other end is located inside the quartz tube 10 and connected to the scum scraper 42, which is located inside the evaporating dish 20. Specifically, the U-shaped rod 41 is made of a rigid material that is not easily deformed and is resistant to high temperatures. The scum scraper 42 is made of quartz material, and its shape is the same as the cross-sectional shape of the evaporating dish 20.
[0033] Furthermore, the U-shaped rod 41 is threadedly connected to the scraper spoon 42. Understandably, the threaded connection facilitates disassembly.
[0034] In a preferred embodiment, a flange 50 is provided on the end face of the quartz tube 10, and an elongated hole 51 is provided on the flange 50 for the U-shaped rod 41 to pass through, allowing the U-shaped rod 41 to move within the elongated hole 51. Specifically, the flange 50 is made of stainless steel and primarily serves to seal the quartz tube 10, while also facilitating the opening of holes for connecting gas pipelines, etc. It is worth noting that the elongated hole 51 on the flange 50 in this embodiment is mainly intended to facilitate the vertical movement of the U-shaped rod 41. Since the height of the scraper 42 varies depending on the volume of the ingot, the elongated hole 51 facilitates height adjustment of the scraper 42.
[0035] In a preferred embodiment, the zone melting and purification device further includes a bolt 60 and a washer 70, the bolt 60 connecting the washer 70, and the two being located on opposite sides of the elongated hole 51; a through hole 61 is provided in the middle of the bolt 60, through which the U-shaped rod 41 passes.
[0036] It is understandable that the purpose of setting the gasket 70 and the bolt 60 is to fix the U-shaped rod 41. When it is necessary to move the U-shaped rod 41, simply loosen the bolt 60. At the same time, the gasket 70 can also provide a certain degree of sealing for the elongated hole 51.
[0037] Because traditional zone melting has difficulty separating impurities with a separation coefficient close to 1, existing technologies typically employ external magnetic or electric fields to reduce the diffusion layer thickness and promote impurity diffusion and migration. However, these methods generally suffer from high equipment costs and high energy consumption. In a preferred embodiment, the zone melting and purification apparatus further includes a frame 90, on which a quartz tube 10 is mounted, and a heater 30 is movably mounted. Specifically, the frame 90 includes a base and two supports, which are arranged parallel to each other on the frame 90. The quartz tube 10 is mounted on the two supports, and a track (not shown in the figure) for movement is also provided on the frame 90, on which the heater 30 is mounted.
[0038] Furthermore, the zone melting and purification apparatus provided in this embodiment also includes an outlet pipe 110 and an inlet pipe 100, which are respectively connected to the two ends of the quartz tube 10. Specifically, the main function of the inlet pipe 100 is to introduce high-purity nitrogen gas, while the outlet pipe 110 is mainly used to discharge waste gas from the quartz tube 10.
[0039] This embodiment also provides a zone melting purification method, based on the above-mentioned zone melting purification apparatus, as follows: Step S1: Place the metal ingot in the evaporating dish 20, then place the evaporating dish 20 into the quartz tube 10, seal both ends with flanges 50 and connect the inlet pipe 100 and outlet pipe 110 respectively, and then introduce nitrogen into the quartz tube 10. Step S2: After ventilating for 2 hours, move the heater 30 to the beginning of the evaporating dish 20 (near the air inlet of the quartz tube 10) and turn on the heater 30 to begin regional melting of the metal ingot; Step S3: After the ingot has completely melted, adjust the position of the scum puller and turn on the vibrator. Adjust the vibration frequency to slightly stir the liquid surface, and then start moving the heater. The scum puller and the heater move synchronously. The surface scum will move from the head to the tail of the ingot with the scum puller and eventually gather at the tail end of the ingot. When the heater moves from the head to the tail end of the evaporating dish, it is one zone melting purification. Repeat this process many times. After that, most of the scum will be enriched at the tail end of the ingot. Then adjust the height of the scum puller so that it is suspended above the ingot. Step S4: After multiple zone meltings are completed, the metal ingot is taken out, and the head and tail are removed. It is then used as raw material for the next zone melting cycle. Steps S2 and S3 are repeated to obtain a high-purity metal product.
[0040] In detail, in step S4, 5%-10% of the head is removed and 15%-20% of the tail is removed.
[0041] To more clearly illustrate the technical solution provided in this embodiment, examples are provided for explanation, as follows: Example 1 Based on this apparatus, a method for preparing high-purity metallic bismuth by zone melting includes the following steps: Step S1: Place 5 kg of 5N bismuth into evaporating dish 20, then place evaporating dish 20 into quartz tube 10, seal both ends with flange 50 to connect to gas pipeline, and introduce high-purity nitrogen gas at a flow rate of 300 ml / min. Step S2: After ventilating for 2 hours, move the heater 30 to the beginning (air inlet) of the evaporating dish 20, turn on the heater 30, and set the material temperature to 550℃; Step S3: After the bismuth ingot in the evaporating dish 20 melts, adjust the position of the slag traction device 40, turn on the high-frequency vibrator, and the heater 30 begins to move towards the tail end of the evaporating dish 20 at a displacement speed of 180 mm / h, and perform zone melting twice; then adjust the temperature to 500℃, reduce the displacement speed to 150 mm / h, and perform zone melting 10 times consecutively; then adjust the temperature to 480℃, reduce the displacement speed to 100 mm / h, and perform zone melting 5 times consecutively.
[0042] Step S4: After zone melting, remove the bismuth ingot, discard 5%-10% from the head and 15%-20% from the tail, and use it as raw material for the next zone melting cycle. Repeat steps S2 and S3 to obtain 6N high-purity bismuth. The test results are shown in Table 1 below.
[0043] Table 1 High-purity bismuth test report
[0044] Sampling: The product ingots are then... Figure 2 The sample was divided into five parts from the beginning to the end. The first part was about 5%-10% of the total length, and the fifth part was about 15%-20% of the total length. The samples were taken and tested in segments. The test results are shown in Table 2 below.
[0045] Table 2 High-purity bismuth test report
[0046] The data above shows that after zone melting, impurities in the raw bismuth concentrate at both ends, with most impurities accumulating at the tail end, while the middle portion has the lowest impurity content. Therefore, 5%-10% of the impurities at the head and 15%-20% at the tail need to be removed from the product.
[0047] Comparative Example 1: Compared to Example 1, the device is identical except for the removal of the scum traction device 40.
[0048] Based on this apparatus, a method for preparing high-purity metallic bismuth by zone melting includes the following steps: Step S1: Place 5 kg of 5N bismuth into evaporating dish 20, then place evaporating dish 20 into quartz tube 10, seal both ends with flange 50 to connect to gas pipeline, and introduce high-purity nitrogen gas at a flow rate of 300 ml / min. Step S2: After ventilating for 2 hours, move the heater 30 to the beginning (air inlet) of the evaporating dish 20, turn on the heater 30, and set the material temperature to 550℃; Step S3: After the bismuth ingot in the evaporating dish 20 melts, turn on the high-frequency vibrator and the heater 30 begins to move towards the tail end of the evaporating dish 20 at a displacement speed of 180 mm / h, and perform zone melting twice; then adjust the temperature to 500℃, reduce the displacement speed to 150 mm / h, and perform zone melting 10 times consecutively; then adjust the temperature to 480℃, reduce the displacement speed to 100 mm / h, and perform zone melting 5 times consecutively.
[0049] Step S4: After zone melting, remove the bismuth ingot, discard 5%-10% from the head and 15%-20% from the tail, and use it as raw material for the next zone melting cycle. Repeat steps S2 and S3 to obtain high-purity bismuth. The test results are shown in Table 3 below.
[0050] Table 3 High-purity bismuth test report
[0051] Therefore, the bismuth purity obtained in Comparative Example 1 is lower than that in Example 1.
[0052] Comparative Example 2: Compared to Example 1, this device eliminates the high-frequency vibrator 80.
[0053] Based on this apparatus, a method for preparing high-purity metallic bismuth by zone melting includes the following steps: Step S1: Place 5 kg of 5N bismuth into evaporating dish 20, then place evaporating dish 20 into quartz tube 10, seal both ends with flange 50 to connect to gas pipeline, and introduce high-purity nitrogen gas at a flow rate of 300 ml / min. Step S2: After ventilating for 2 hours, move the heater 30 to the beginning (air inlet) of the evaporating dish 20, turn on the heater 30, and set the material temperature to 550℃; Step S3: After the bismuth ingot in the evaporating dish 20 melts, adjust the position of the slag puller 40, and the heater 30 begins to move towards the tail end of the evaporating dish 20 at a displacement speed of 180 mm / h, performing zone melting twice; then adjust the temperature to 500℃, reduce the displacement speed to 150 mm / h, and perform zone melting 10 times consecutively; then adjust the temperature to 480℃, reduce the displacement speed to 100 mm / h, and perform zone melting 5 times consecutively. Step S4: After zone melting, remove the bismuth ingot, discard 5%-10% from the head and 15%-20% from the tail, and use it as raw material for the next zone melting cycle. Repeat steps S2 and S3 to obtain high-purity bismuth. The test results are shown in Table 4 below.
[0054] Table 4 High-purity bismuth test report
[0055] Therefore, compared with Example 1, Comparative Example 2 yielded bismuth with a higher total amount of impurities and lower purity.
[0056] Comparative Example 3: Compared with Example 1, this device eliminates the scum traction device 40 and the high-frequency vibrator 80.
[0057] Based on this apparatus, a method for preparing high-purity metallic bismuth by zone melting includes the following steps: Step S1: Place 5 kg of 5N bismuth into evaporating dish 20, then place evaporating dish 20 into quartz tube 10, seal both ends with flange 50 to connect to gas pipeline, and introduce high-purity nitrogen gas at a flow rate of 300 ml / min. Step S2: After ventilating for 2 hours, move the heater 30 to the beginning (air inlet) of the evaporating dish 20, turn on the heater 30, and set the material temperature to 550℃; Step S3: After the bismuth ingot in the evaporating dish 20 melts, the heater 30 begins to move towards the tail end of the evaporating dish 20 at a displacement speed of 180 mm / h, and performs zone melting twice; then the temperature is adjusted to 500℃, the displacement speed is reduced to 150 mm / h, and zone melting is performed 10 times consecutively; then the temperature is adjusted to 480℃, the displacement speed is reduced to 100 mm / h, and zone melting is performed 5 times consecutively. Step S4: After zone melting, remove the bismuth ingot, discard 5%-10% from the head and 15%-20% from the tail, and use it as raw material for the next zone melting cycle. Repeat steps S2 and S3 to obtain high-purity bismuth. The test results are shown in Table 5 below.
[0058] Table 5 High-purity bismuth test report
[0059] Therefore, the bismuth purity obtained in Comparative Example 3 was lower than that in Example 1.
[0060] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.
Claims
1. A zone smelting and purification apparatus, characterized in that, include: A quartz tube, wherein an evaporating dish is disposed inside the quartz tube; A heater for heating the quartz tube to melt the ingot in the evaporating dish, and the heater is movable along the length of the quartz tube; A scum traction device, one end of which is connected to the heater, and the other end is inserted from the end of the quartz tube and located inside the evaporating dish; A vibrator for vibrating the quartz tube; As the heater heats the quartz tube and moves along the quartz tube, the scum puller moves with the heater, and the scum puller at one end inside the evaporating dish moves the scum on the surface of the molten ingot to the end. The scum puller includes a U-shaped rod and a scum scraper. One end of the U-shaped rod is connected to the heater, and the other end is located inside the quartz tube and connected to the scum scraper. The scum scraper is located inside the evaporating dish. A flange is provided on the end face of the quartz tube, and an elongated hole is provided on the flange for the U-shaped rod to pass through, and the U-shaped rod can move in the elongated hole.
2. The zone smelting and purification apparatus according to claim 1, characterized in that, The U-shaped rod is threadedly connected to the slag scraper.
3. The zone smelting and purification apparatus according to claim 1, characterized in that, The zone smelting and purification device also includes bolts and washers, the bolts connecting the washers and the two being located on opposite sides of the elongated hole; The bolt has a through hole in the middle, and the U-shaped rod passes through the through hole.
4. The zone smelting and purification apparatus according to claim 1, characterized in that, The zone smelting and purification apparatus also includes a frame, on which the quartz tube is mounted, and on which the heater is movably mounted.
5. The zone smelting and purification apparatus according to claim 1, characterized in that, The zone smelting and purification device also includes an outlet pipe and an inlet pipe, which are respectively connected to the two ends of the quartz tube.
6. A zone melting purification method, based on the zone melting purification apparatus according to any one of claims 1 to 5, characterized in that, include: Step S1: Place the metal ingot in an evaporating dish, then place the evaporating dish into a quartz tube, seal both ends with flanges and connect the inlet and outlet pipes respectively, and then introduce nitrogen gas into the quartz tube. Step S2: After ventilating for 2 hours, move the heater to the beginning of the evaporating dish and turn on the heater to begin melting the metal ingot in the starting area; Step S3: After the ingot has completely melted, adjust the position of the scum puller and turn on the vibrator. Adjust the vibration frequency to slightly stir the liquid surface, and then start moving the heater. The scum puller and the heater move synchronously. The surface scum will move from the head to the tail of the ingot with the scum puller and eventually gather at the tail end of the ingot. When the heater moves from the head to the tail end of the evaporating dish, it is one zone melting purification. Repeat this process many times. After that, most of the scum will be enriched at the tail end of the ingot. Then adjust the height of the scum puller so that it is suspended above the ingot. Step S4: After multiple zone meltings are completed, the metal ingot is taken out, and the head and tail are removed. It is then used as raw material for the next zone melting cycle. Steps S2 and S3 are repeated to obtain a high-purity metal product.
7. The zone smelting purification method according to claim 6, characterized in that, In step S4, 5%-10% of the head is removed and 15%-20% of the tail is removed.
Citation Information
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