A high-purity material melt settling centrifugal preparation device

Abstract

The application provides a high-purity material melting sedimentation centrifugal preparation device, which comprises a frame and a rotating mechanism, a distributed temperature control mechanism installed on the frame and the rotating mechanism, and a centrifugal tube installed in the distributed temperature control mechanism; the frame and the rotating mechanism comprise a base, a motor is installed in the base, the motor is connected with a rotating shaft, a plurality of supporting arms are arranged on the rotating shaft, and the supporting arms are connected with the distributed temperature control mechanism; a bottom heating row is arranged at the bottom of the distributed temperature control mechanism, a heating sleeve is arranged above the bottom heating row, a top temperature zone measurement and control unit and a bottom temperature zone measurement and control unit are arranged above and below the heating sleeve respectively, the centrifugal tube is arranged in the distributed temperature control mechanism, and limit blocks one, two and three are arranged around the centrifugal tube in the distributed temperature control mechanism. The application utilizes the density difference between impurities and main elements, realizes the preparation of high-purity materials through high-speed centrifugation, has a wide application range, low raw material requirement, simple structure, easy operation and high production benefit.

Description

Technical Field

[0001] This invention belongs to the field of high-purity material equipment, and specifically relates to a high-purity material melting, sedimentation, and centrifugal preparation device. Background Technology

[0002] Currently, in the field of high-purity material preparation, the widely used production processes are mainly divided into chemical methods and physical methods.

[0003] Chemical methods mainly include electrolytic refining, ion exchange, and solvent extraction, which are techniques that use chemical reactions to separate impurities. However, since they often require the introduction of other reagents, this causes two problems: firstly, the introduced reagents also need to be of high purity and are often expensive, which is not conducive to reducing costs; secondly, the introduction of reagents will inevitably cause pollution to some extent. Due to this limitation, the application of chemical methods in the field of high-purity material preparation is mostly limited to 5N.

[0004] Physical methods mainly include vacuum distillation, zone melting, Czochralski method, and directional solidification. These methods utilize the differences in physical properties between the main element and the impurity element, and employ physical processes such as evaporation, solidification, crystallization, diffusion, and electromigration to remove impurities, thereby achieving high purification of the main element material.

[0005] Methods such as zone melting and Czochralski single crystal pulling can prepare high-purity materials of 6N and above, but they often have relatively long production cycles and high costs; and they have high requirements for the quality of raw materials (generally requiring 5N and above). They are mainly used at the end of the high-purity material preparation process.

[0006] Vacuum distillation can process relatively low-quality raw materials and has a short production cycle; however, it is greatly limited by the physical properties of the main elements in high-purity materials. It is mostly used in the early stages of high-purity material preparation processes.

[0007] Industrial centrifuges can be classified into three categories based on their structure and separation requirements: filtration centrifuges, sedimentation centrifuges, and separators. Separators include disc separators, tubular separators, and chamber separators.

[0008] Centrifugal filtration involves applying centrifugal pressure generated by a suspension under a centrifugal force field to a filter medium, causing the liquid to pass through the filter medium to become filtrate, while solid particles are retained on the surface of the filter medium, thus achieving liquid-solid separation.

[0009] Centrifugal sedimentation utilizes the principle that components of a suspension (or emulsion) with different densities rapidly settle and separate into layers in a centrifugal force field, thereby achieving liquid-solid (or liquid-liquid) separation.

[0010] A separator has a cylindrical drum that rotates at high speed around its own axis, usually driven by an electric motor. When the suspension (or emulsion) is added to the drum, it is quickly driven to rotate at the same speed as the drum. Under centrifugal force, the components separate and are discharged separately. Generally, the higher the drum speed, the better the separation effect.

[0011] For example, the paper "Removal of Fe from molten Al by filtration in a centrifuge," published in Volume 906 of the Journal of Alloys and Compounds in 2022, proposes a process for removing iron from molten aluminum using centrifugal induction combined with an alumina foam ceramic filter (Al2O3 CFF). The equipment involved is a filtration centrifuge, and it requires the use of a special filter media—the alumina foam ceramic filter (Al2O3 CFF)—resulting in relatively high production costs.

[0012] For example, Chinese patent CN 113403487 A, "A High-Purity Aluminum Purification Device and Purification Method Thereof," discloses a device similar to a tubular separator, which purifies molten aluminum using normal segregation and gravity segregation through a rotating crucible. It should be noted that this device is an open-system production system under atmospheric pressure, and is clearly unsuitable for preparing high-purity materials with high vapor pressures, such as high-purity zinc, or high-purity materials with significant environmental hazards, such as high-purity arsenic and cadmium. The overall structure of this device is quite complex.

[0013] The equipment disclosed in Chinese patents CN 212732599 U "Vertical Molten Metal Centrifugal Separation Test Machine" and CN 113042222 A "Method for Centrifugal Separation of Molten Metal and its Vertical Centrifugal Separator" should be classified as a separator. It is applied in traditional metal smelting, secondary resources, and other fields. It separates the target metal from impurities by subjecting two or more molten metals with different specific gravities to high centrifugal force. Impurities, upon contact with the enrichment cone plate, are thrown into the tailings trough, while the target metal mineral is collected in the enrichment trough. However, it should be noted that the core of this equipment—the graphite separation mechanism—has a complex internal structure and low overall production efficiency.

[0014] The above three items are the currently published patents and papers in China related to the purification of molten metal using centrifugation methods. Among them, Chinese patent CN 212732599 U does not yet belong to the field of high-purity material preparation, and one of the remaining two is a filtration centrifuge, while the other is close to a tubular separator.

[0015] The equipment disclosed in Chinese Patent CN 115305358 A, "A Low-Oxygen Ultra-High Purity Arsenic Rod Forming Device," is applied in the field of high-purity material preparation. It integrates vacuum deoxidation, high-pressure melting, horizontal rotation degassing, and directional solidification into a single device, thereby producing high-density, smooth-surfaced high-purity arsenic rods suitable for molecular beam epitaxy. This effectively avoids problems such as uneven ingot surfaces, shrinkage cavities, and high oxygen content found in conventional ingot forming. However, it should be noted that this equipment does not essentially employ centrifugal sedimentation to further purify high-purity arsenic; rather, it removes air bubbles through horizontal rotation, serving only the purpose of achieving the desired arsenic rod forming effect.

[0016] In the field of high-purity material preparation, there is currently no publicly available information showing the application of similar sedimentation centrifuges. That is, a process and equipment for preparing high-purity materials that utilizes the density difference between impurities and the main elements to enrich light and heavy impurities at the head and tail ends of a closed centrifuge tube through high-speed centrifugation. Summary of the Invention

[0017] To overcome the technological bottlenecks in the industrial production of various high-purity and ultra-high-purity materials with relatively low melting points, this invention provides a high-purity material melting sedimentation centrifugation preparation device. Compared to existing technologies, this device heats and melts the material to be purified into a liquid state in a closed centrifuge tube. Utilizing the density difference between impurities and the main elements, high-speed centrifugation concentrates light and heavy impurities at the head and tail ends of the closed centrifuge tube, respectively, achieving further purification. This equipment provides a universal device applicable to the industrial production of various high-purity and ultra-high-purity materials with relatively low melting points; it also boasts advantages such as simple structure, ease of operation, and low operating costs.

[0018] The technical solution of the present invention is implemented as follows: a high-purity material melting sedimentation centrifugation preparation device, comprising a frame and a rotating mechanism, a distributed temperature control mechanism installed on the frame and the rotating mechanism, and a centrifuge tube installed in the distributed temperature control mechanism;

[0019] Furthermore, the frame and rotating mechanism include a base, a motor is installed inside the base, the motor is connected to a rotating shaft, and a plurality of support arms are provided on the rotating shaft, the support arms being connected to a distributed temperature control mechanism;

[0020] Furthermore, the distributed temperature control mechanism is provided with a bottom heating element at the bottom, a heating sleeve above the bottom heating element, a top temperature zone measurement and control unit and a bottom temperature zone measurement and control unit above and below the heating sleeve, respectively, and the centrifuge tube is located inside the distributed temperature control mechanism. Limiting block one, limiting block two and limiting block three are provided around the centrifuge tube inside the distributed temperature control mechanism. Limiting block one, limiting block two and limiting block three limit the spatial position and tilt angle of the centrifuge tube.

[0021] Furthermore, the centrifuge tube includes a centrifuge tube body, and a flange cover is provided on the top of the centrifuge tube body by fixing bolts. The flange cover is provided with a sealing valve to achieve medium and low pressure oxygen-free process conditions.

[0022] Furthermore, the limiting block one, limiting block two, and limiting block three are made of aluminum silicate, and each limiting block is evenly and densely perforated.

[0023] Furthermore, the centrifuge tube is made of high-purity quartz, high-purity titanium, high-purity graphite, or high-purity boron nitride.

[0024] The beneficial effects of this invention are:

[0025] 1) Compared with the prior art, the present invention utilizes the density difference between impurities and main elements to enrich light and heavy impurities at the head and tail ends of a closed centrifuge tube through high-speed centrifugation to prepare high-purity materials. At the same time, it also achieves ingot casting using directional solidification under medium-pressure oxygen-free conditions, solving the production problem of preparing high-density, smooth and flat high-purity arsenic rods for molecular beam epitaxy.

[0026] 2) This equipment has a wide range of applications. In addition to being used to prepare high-purity arsenic rods for molecular beam epitaxy, it can also be used to prepare high-purity oxygen-free selenium rods and other high-purity rods.

[0027] 3) Because this equipment has purification capabilities, the requirements for raw material quality can be appropriately relaxed, thereby further improving production efficiency.

[0028] 4) This equipment has a simple structure, is easy to operate, and has low operating costs. Attached Figure Description

[0029] Figure 1 This is the front view of the present invention;

[0030] Figure 2 This is a top view of the present invention;

[0031] Figure 3 This is a cross-sectional view of the distributed heater of the present invention.

[0032] In the diagram: 1. Frame and rotating mechanism; 101. Base; 102. Motor; 103. Support arm; 104. Rotating shaft; 2. Distributed temperature control mechanism; 201. Bottom heating element; 202. Bottom temperature zone measuring unit; 203. Heating jacket; 204. Limiting block one; 205. Top temperature zone measuring unit; 206. Limiting block two; 207. Limiting block three; 3. Centrifuge tube; 301. Centrifuge tube body; 302. Fixing bolts; 303. Flange cover; 304. Cover valve. Implementation

[0033] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0034] In the description of this invention, it should be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. 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. Therefore, they should not be construed as limitations on this invention.

[0035] See attached document Figure 1-3 A high-purity material melting sedimentation centrifugation preparation device includes: a frame and a rotating mechanism 1, a distributed temperature control mechanism 2 installed on the frame and rotating mechanism 1, and a centrifuge tube 3 installed in the distributed temperature control mechanism 2. The frame and rotating mechanism 1 includes a base 101, a motor 102 installed in the base 101, the motor 102 being connected to a rotating shaft 104, and three support arms 103 connected to the rotating shaft 104. The support arms 103 are connected to the distributed temperature control mechanism 2.

[0036] The distributed temperature control mechanism 2 has a bottom heating element 201 at the bottom and a heating sleeve 203 above the bottom heating element 201. A top temperature zone measurement and control unit 205 and a bottom temperature zone measurement and control unit 202 are respectively provided above and below the heating sleeve 203. The heating sleeve 203 passes through the bottom temperature measurement unit 202 and the top temperature measurement unit 205 from top to bottom. The centrifuge tube 3 is located inside the distributed temperature control mechanism 2. Limiting blocks 1 204, 206, and 3 207 are provided around the centrifuge tube 3 inside the distributed temperature control mechanism 2. Limiting blocks 1 204, 206, and 3 207 limit the spatial position and tilt angle of the centrifuge tube 3. The limiting blocks 1 204, 206, and 3 207 are made of aluminum silicate and are densely perforated.

[0037] The centrifuge tube 3 includes a centrifuge tube body 301, and a flange cover 303 is provided on the top of the centrifuge tube body 301 by fixing bolts 302. The flange cover 303 is provided with a cover valve 304. The centrifuge tube 3 is made of high-purity quartz, high-purity titanium, high-purity graphite, or high-purity boron nitride.

[0038] Centrifuge tubes 3 include low-pressure centrifuge tubes (0.1MPa~1.6 MPa) and medium-pressure centrifuge tubes (1.6MPa~7.5 MPa) according to their operating conditions.

[0039] The specific preparation process is as follows:

[0040] Example 1

[0041] This application example uses a melt sedimentation centrifugal high-purity material preparation apparatus from the previous embodiment to prepare ultra-high purity arsenic rods for molecular beam epitaxy through the following steps:

[0042] S1. Place 8 kg of raw material 6N high-purity arsenic into three high-purity quartz medium-pressure centrifuge tubes (hereinafter referred to as medium-pressure centrifuge tubes) in the glove box, tighten the fixing bolts, and secure the flange cover of the medium-pressure centrifuge tube to the high-purity quartz medium-pressure centrifuge tube. Then remove it from the glove box.

[0043] S2. Connect the medium-pressure centrifuge tube to the gas pressurization pipeline, open the valve of the medium-pressure centrifuge tube cap, and pressurize it to 3.8MPa with high-purity inert gas.

[0044] S3. Weigh the three centrifuge tubes separately and attach counterweights to ensure that the mass difference between the three is less than 0.1g.

[0045] S4. Place the three centrifuge tubes into the heating jacket and place the limiting block. Seal the heating jacket, turn on the temperature control system, and slowly raise the two temperature zones to 850℃ simultaneously and keep them at that temperature for 2 hours.

[0046] S5. Turn on the power system and slowly increase the speed to 6000r / min, and maintain this speed for 3 hours.

[0047] S6. Control the bottom temperature zone to cool down to 750℃, then simultaneously and slowly cool down the two temperature zones to 150℃ and 50℃ respectively and stop heating. Slowly reduce the rotation speed to 0r / min.

[0048] S7. After the system cools to room temperature, open the heating jacket, remove the medium-pressure centrifuge tubes, connect them to the gas relief line, open the medium-pressure centrifuge tube cap valve to release the pressure to 0.01 MPa, and close the cap valve. Clean the surfaces of the three medium-pressure centrifuge tubes and transfer them to the discharge glove box.

[0049] S8. Remove the fastening bolts of the medium-pressure centrifuge tube cap in the discharge glove box, remove the cap, and pour the high-purity arsenic rod into the discharge trough.

[0050] S9. Transfer the discharge chute to the packaging glove box, cut off the 4cm from the head end and the 5cm from the tail end for recycling, and you will get 7N5 ultra-high purity arsenic rods with a smooth and dense surface and an oxygen content of less than 1ppm.

[0051] Example 2

[0052] This example uses a melt sedimentation centrifugal high-purity material preparation apparatus from the previous embodiment to prepare high-purity oxygen-free selenium rods through the following steps:

[0053] S1. Place 8 kg of 5N high-purity selenium raw material into three high-purity quartz low-pressure centrifuge tubes (hereinafter referred to as low-pressure centrifuge tubes), tighten the fixing bolts, and secure the flange cover of the low-pressure centrifuge tube to the high-purity quartz low-pressure centrifuge tube.

[0054] S2. Connect the low-pressure centrifuge tube to the gas replacement pipeline, open the valve of the low-pressure centrifuge tube cap, evacuate to 10Pa, and fill with high-purity inert gas to 0.09 MPa. Perform gas replacement three times in total.

[0055] S3. Weigh the three centrifuge tubes separately and attach counterweights to ensure that the mass difference between the three is less than 0.1g.

[0056] S4. Place the three centrifuge tubes into the heating jacket and place the limiting block. Seal the heating jacket, turn on the temperature control system, and slowly raise the temperature of the two temperature zones to 250℃ simultaneously and keep the temperature constant for 2 hours.

[0057] S5. Turn on the power system and slowly increase the speed to 2000r / min, and maintain this speed for 2 hours.

[0058] S6. Control the bottom temperature zone to cool down to 200℃, then simultaneously and slowly cool down the two temperature zones to 100℃ and 50℃ respectively and stop heating. Slowly reduce the rotation speed to 0r / min.

[0059] S7. After the system cools to room temperature, open the heating jacket, remove the medium-pressure centrifuge tubes, connect them to the gas replacement pipeline, open the sealing valve of the medium-pressure centrifuge tubes, balance the pressure inside the centrifuge tubes, and then close the sealing valve. Clean the surfaces of the three medium-pressure centrifuge tubes and transfer them to the discharge glove box.

[0060] S8. In the discharge glove box, remove the fastening bolts of the low-pressure centrifuge tube cap, remove the cap, and pour the high-purity oxygen-free selenium rod into the discharge trough.

[0061] S9. Transfer the discharge trough to the packaging glove box, cut off 3cm from the head end and 4cm from the tail end to obtain 6N high-purity oxygen-free selenium rods.

[0062] The above description, in conjunction with specific preferred embodiments, provides a further detailed explanation of the present invention. It should not be construed that the specific implementation of the present invention is limited to these descriptions. For those skilled in the art, various simple deductions or substitutions can be made without departing from the concept of the present invention, and all such modifications and substitutions should be considered within the scope of protection of the present invention.

Claims

1. A high purity material melt settling centrifuge preparation apparatus, characterized by The utility model relates to a high purity material preparation device, including frame and rotating mechanism (1), install distributed temperature control mechanism (2) on frame and rotating mechanism (1), centrifugal tube (3) is installed in distributed temperature control mechanism (2), frame and rotating mechanism (1) including base (101), motor (102) is installed in base (101), motor (102) is connected with rotating shaft (104), a plurality of support arms (103) are equipped on rotating shaft (104), support arm (103) is connected with distributed temperature control mechanism (2);Distributed temperature control mechanism (2) bottom is equipped with bottom heating row (201), bottom heating row (201) top is equipped with heating cover (203), heating cover (203) top and bottom are equipped with top temperature zone measurement and control unit (205) and bottom temperature zone measurement and control unit (202) respectively, centrifugal tube (3) is located in distributed temperature control mechanism (2), and the surrounding of centrifugal tube (3) in distributed temperature control mechanism (2) is equipped with limit block one (204), limit block two (206) and limit block three (207), and limit block one (204), limit block two (206) and limit block three (207) limit the spatial position and inclination angle of centrifugal tube (3);Centrifugal tube (3) including centrifugal tube main part (301), centrifugal tube main part (301) top is equipped with flange cover (303) through fixed bolt (302), and flange cover (303) is equipped with cover valve (304);Utilize the density difference of impurity and main body element, and through high speed centrifugation, light, heavy impurities are enriched in the head, tail two ends of closed centrifugal tube respectively to prepare high purity material, and directional solidification process ingot casting is carried out under the condition of medium pressure oxygenless simultaneously.

2. The apparatus for producing high purity material by melt settling centrifugation according to claim 1, wherein Limit block one (204), limit block two (206) and limit block three (207) material is aluminium silicate, and each limit block is uniformly densely clothed and is punched.

3. The device for preparing high purity material by melt settling centrifugation according to claim 1 or 2, characterized in that Centrifugal tube (3) material is high purity quartz or high purity titanium or high purity graphite or high purity boron nitride.

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