High-purity arsenic sublimation device

Abstract

The utility model relates to the technical field of high-purity arsenic preparation, and provides a high-purity arsenic sublimation device which comprises a sublimation barrel, a barrel cover, a crucible, a collecting cover and a negative pressure machine, the crucible is arranged at the inner bottom of the sublimation barrel, and a heating sleeve is arranged on the outer wall of the crucible; a threaded bottom is arranged on the lower wall of the barrel cover, a sealing brim is fixedly connected to the outer wall of the sublimation barrel, and the threaded bottom is in threaded connection to the inner wall of the sealing brim; a mounting table is arranged on the inner wall of the sublimation barrel, the collecting cover is arranged above the mounting table, and a spiral pipeline is arranged in the collecting cover. By arranging the collecting cover and the conveying pipe, when arsenic is sublimated, sublimated impurities can be discharged firstly, the phenomenon that when arsenic steam is condensed, the impurities and the arsenic steam are condensed at the same time due to the fact that too many impurities are contained in the barrel, and the purity is reduced is avoided, the crucible is directly heated by the heating sleeve through the semi-embedded arrangement of the communicating pipe crucible, and therefore the purity of the arsenic is improved. And the influence on equipment is avoided.

Description

Technical Field

[0001] This utility model belongs to the field of high-purity arsenic preparation technology, specifically relating to a high-purity arsenic sublimation device. Background Technology

[0002] High-purity arsenic refers to elemental arsenic with a purity of 99.999% (5N) or higher. It has a silvery-gray metallic luster and is primarily used in the preparation of III-V compound semiconductors such as gallium arsenide. It is a core raw material for LEDs, lasers, solar cells, and 5G communication devices. Its preparation requires a combination of chemical purification (such as reduction methods) and physical refining (zone melting), and the production process must strictly control the risk of extreme toxicity. Global annual production capacity is approximately several hundred tons, making it a key basic raw material in the field of strategic emerging materials.

[0003] A known authorized patent with application number 201921748534.7 discloses a high-purity arsenic sublimation device, comprising a cooling system, a heating system, a sublimation furnace, a deposition system, and a vacuum system. The sublimation furnace includes a furnace body, a condensing inner liner, and a melting chamber. The melting chamber is located at the bottom of the furnace body with its opening facing upwards. The condensing inner liner has its opening facing downwards, and its lower opening is detachably sealed to the upper opening of the melting chamber. The condensing inner liner has a top opening and is fitted with an inner liner cover that mates with the top opening. Both the condensing inner liner and the melting chamber are located within the furnace body. The top of the furnace body is connected to the deposition system via a pipeline, and the vacuum system is connected to the deposition system via a pipeline. The temperature of the heating system is adjustable. This utility model's high-purity arsenic sublimation device also has the advantages of high production capacity, stable operation, low safety risk, low cost, ease of large-scale production, and simple operation.

[0004] However, the following problems were found in the implementation of the above technical solutions: it is difficult to remove the condenser liner during use, making it difficult to quickly remove the high-purity arsenic, and directly heating the sublimation tank will interfere with equipment that is close to the tank.

[0005] Therefore, a high-purity arsenic sublimation device is proposed to solve the above problems. Utility Model Content

[0006] This invention proposes a high-purity arsenic sublimation device, which solves the problems in related technologies where it is difficult to remove the condenser liner during use, making it difficult to quickly remove high-purity arsenic, and that directly heating the sublimation tank can interfere with equipment that is close to the tank.

[0007] The technical solution of this utility model is as follows: a high-purity arsenic sublimation device, comprising: a sublimation tank, a tank lid, a crucible, a collection lid and a negative pressure machine, wherein the crucible is disposed at the inner bottom of the sublimation tank and a heating jacket is provided on the outer wall of the crucible;

[0008] The lower wall of the barrel lid is provided with a threaded bottom, and the outer wall of the sublimation barrel is fixedly connected with a sealing eave, and the threaded bottom is threadedly connected to the inner wall of the sealing eave;

[0009] The inner wall of the sublimation tank is provided with an installation platform, the collection cover is located above the installation platform, the inside of the collection cover is provided with a spiral pipe, the inside of the installation platform is provided with a cooling pipe, and the spiral pipe inside the collection cover is interlocked with the cooling pipe.

[0010] Preferably, the top of the collection cover is provided with a conveying pipe, the end of the conveying pipe is provided with a retaining ring, the inside of the sublimation tank is provided with a sliding groove, the retaining ring is sleeved on the inner wall of the sliding groove, the outer wall of the sublimation tank is provided with an output pipe, the conveying pipe is connected to the output pipe, and the inside of the output pipe is provided with a solenoid valve.

[0011] Preferably, the output end of the negative pressure machine is fixedly connected to a connecting pipe, the inside of the connecting pipe is provided with a vacuum valve, and the outer wall of the connecting pipe is provided with a filter block.

[0012] Preferably, the connecting pipe is connected to the sublimation tank, and a connecting pipe is provided on the outside of the sublimation tank, the connecting pipe spanning the mounting platform.

[0013] Preferably, the outer wall of the sublimation tank is provided with a circulating cooling module, and the other end of the cooling pipe is connected to the circulating cooling module.

[0014] Preferably, a sealing ring is provided on the lower wall of the threaded bottom, and a vacuum gauge is provided on the upper wall of the bucket lid.

[0015] The working principle and beneficial effects of this utility model are as follows:

[0016] By using a collection cover and conveying pipe, impurities from the sublimation of arsenic can be discharged first, preventing excessive impurities from remaining in the container. This would cause impurities to condense simultaneously with the arsenic vapor during condensation, resulting in a decrease in purity. The semi-embedded design of the crucible via the connecting pipe allows the heating jacket to directly heat the crucible without affecting the equipment. Attached Figure Description

[0017] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments.

[0018] Figure 1 This is a three-dimensional structural diagram of the present invention;

[0019] Figure 2 This is a rear-view three-dimensional structural diagram of the present invention;

[0020] Figure 3 This is a cross-sectional structural diagram of the sublimation tank of this utility model;

[0021] Figure 4 This is a top view of the sliding groove structure of this utility model.

[0022] In the diagram: 1. Sublimation tank; 2. Tank lid; 3. Crucible; 4. Heating jacket; 5. Collection cover; 6. Delivery pipe; 7. Snap ring; 8. Sliding groove; 9. Solenoid valve; 10. Output pipe; 11. Negative pressure unit; 12. Connecting pipe; 13. Vacuum valve; 14. Filter block; 15. Connecting pipe; 16. Cooling pipe; 17. Circulating cooling module; 18. Sealing rim; 19. Sealing ring; 20. Vacuum gauge; 21. Threaded bottom; 22. Mounting platform. Detailed Implementation

[0023] The technical solutions of this utility model will be clearly and completely described below with reference to the embodiments of this utility model. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of this utility model.

[0024] Implementation

[0025] Please see Figure 1 -4. A high-purity arsenic sublimation device, comprising: a sublimation tank 1, a tank cover 2, a crucible 3, a collection cover 5, and a negative pressure machine 11. The crucible 3 is located at the inner bottom of the sublimation tank 1, and a heating jacket 4 is provided on the outer wall of the crucible 3.

[0026] The lower wall of the barrel lid 2 is provided with a threaded bottom 21, and the outer wall of the sublimation barrel 1 is fixedly connected with a sealing eave 18, and the threaded bottom 21 is threadedly connected to the inner wall of the sealing eave 18.

[0027] The inner wall of the sublimation tank 1 is provided with an installation platform 22, and the collection cover 5 is located above the installation platform 22. The inside of the collection cover 5 is provided with a spiral pipe, and the inside of the installation platform 22 is provided with a cooling pipe 16. The spiral pipe inside the collection cover 5 is engaged with the cooling pipe 16.

[0028] The technical solution provided in this embodiment is as follows: First, material is placed in crucible 3, and then collection cover 5 is installed. During installation, the retaining ring 7 is first inserted into the sliding groove 8, and then placed above the mounting platform 22. Then, the circulating cooling module 17 is turned on to check whether the cooling channel inside the collection cover 5 is connected to the cooling pipe 16. After the check is completed, the circulating cooling module 17 is turned off. Then, the sealing ring 17 is installed inside the sealing eaves 18, and then the barrel cover 2 is installed. In use, the negative pressure machine 11 is turned on to evacuate the inside of the sublimation barrel 1. The filter block 14 prevents impurities inside from entering the negative pressure machine 11. At this time, the connecting pipe 15 outputs negative pressure to the bottom of the collection cover 5 to avoid uneven pressure inside the barrel. After reaching the preset negative pressure value, the heating jacket 4 is started to heat the crucible. The crucible 3 is heated. During the heating process, substances with lower boiling points evaporate rapidly and are then transported to the output pipe 10 via the conveying pipe 6 after passing through the collection cover 5. When the temperature reaches the boiling point of arsenic at the current pressure, the solenoid valve 10 is closed, and then the circulating cooling module 17 is activated. Coolant enters the cooling channel inside the collection cover 5 through the cooling pipe 16 and circulates to cool the collection cover 5. When the arsenic vapor comes into contact with the cool surface of the collection cover 5, it sublimates due to the rapid temperature drop. After the arsenic sublimates completely inside the crucible 3, the heating jacket 4 and the negative pressure machine 11 are turned off. When the internal pressure is consistent with the atmospheric pressure, the lid 2 is removed and the cooling circulation module 17 is turned off. Then the collection cover 5 is removed, and the solidified arsenic is collected.

[0029] Furthermore, a conveying pipe 6 is provided at the top of the collection cover 5, and a retaining ring 7 is provided at the end of the conveying pipe 6. A sliding groove 8 is provided inside the sublimation tank 1, and the retaining ring 7 is sleeved on the inner wall of the sliding groove 8. An output pipe 10 is provided on the outer wall of the sublimation tank 1. The conveying pipe 6 is connected to the output pipe 10, and a solenoid valve 9 is provided inside the output pipe 10.

[0030] Specifically, the setting of the retaining ring 7 provides an effective constraint for the installation of the collection cover 5, preventing the collection cover 5 from not being installed properly during installation.

[0031] Furthermore, the output end of the negative pressure machine 11 is fixedly connected to a connecting pipe 12, a vacuum valve 13 is installed inside the connecting pipe 12, a filter block 14 is installed on the outer wall of the connecting pipe 12, and the connecting pipe 12 is connected to the sublimation tank 1.

[0032] Specifically, by setting up the filter block 12, impurities in the tank are prevented from entering the negative pressure machine 11 during operation, thus preventing damage to the negative pressure machine 11.

[0033] Furthermore, a connecting pipe 15 is provided on the outside of the sublimation tank 1, and the connecting pipe 15 spans the mounting platform 22.

[0034] Specifically, the connecting pipe 15 connects the upper and lower parts of the collection cover 5 to avoid uneven air pressure inside the negative pressure tank 1 when vacuuming is performed due to the installation of the collection cover 5.

[0035] Furthermore, a circulating cooling module 17 is provided on the outer wall of the sublimation tank 1, and the other end of the cooling pipe 16 is connected to the circulating cooling module 17.

[0036] Specifically, the cooling circulation module 17 can quickly cool down the collection cover 5, and can effectively and quickly condense and liquefy arsenic vapor.

[0037] Furthermore, a sealing ring 19 is provided on the lower wall of the threaded bottom 21, and a vacuum gauge 20 is provided on the upper wall of the barrel cover 2.

[0038] Specifically, the sealing ring 19 is designed to prevent air leakage between the sublimation tank 1 and the tank cover 2 after installation, thus ensuring the airtightness of the device.

[0039] The above are merely preferred embodiments of the present utility model and are not intended to limit the present utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model shall be included within the protection scope of the present utility model.

Claims

1. A high-purity arsenic sublimation apparatus, comprising: Sublimation barrel (1), barrel lid (2), crucible (3), collection lid (5) and negative pressure machine (11), characterized in that the crucible (3) is set at the inner bottom of the sublimation barrel (1), and the outer wall of the crucible (3) is provided with a heating jacket (4); The lower wall of the barrel lid (2) is provided with a threaded bottom (21), and the outer wall of the sublimation barrel (1) is fixedly connected with a sealing eave (18), and the threaded bottom (21) is threadedly connected to the inner wall of the sealing eave (18). The inner wall of the sublimation tank (1) is provided with an installation platform (22), and the collection cover (5) is located above the installation platform (22). The inside of the collection cover (5) is provided with a spiral pipe, and the inside of the installation platform (22) is provided with a cooling pipe (16). The spiral pipe inside the collection cover (5) is engaged with the cooling pipe (16).

2. The high-purity arsenic sublimation apparatus according to claim 1, characterized in that: The top of the collection cover (5) is provided with a conveying pipe (6), and the end of the conveying pipe (6) is provided with a retaining ring (7). The inside of the sublimation tank (1) is provided with a sliding groove (8), and the retaining ring (7) is sleeved on the inner wall of the sliding groove (8). The outer wall of the sublimation tank (1) is provided with an output pipe (10), and the conveying pipe (6) is connected to the output pipe (10). The inside of the output pipe (10) is provided with a solenoid valve (9).

3. The high-purity arsenic sublimation apparatus according to claim 1, characterized in that: The output end of the negative pressure machine (11) is fixedly connected to a connecting pipe (12), a vacuum valve (13) is provided inside the connecting pipe (12), and a filter block (14) is provided on the outer wall of the connecting pipe (12).

4. The high-purity arsenic sublimation apparatus according to claim 3, characterized in that: The connecting pipe (12) is connected to the sublimation tank (1), and a connecting pipe (15) is provided on the outside of the sublimation tank (1), which spans the mounting platform (22).

5. The high-purity arsenic sublimation apparatus according to claim 1, characterized in that: The outer wall of the sublimation tank (1) is provided with a circulating cooling module (17), and the other end of the cooling pipe (16) is connected to the circulating cooling module (17).

6. The high-purity arsenic sublimation apparatus according to claim 1, characterized in that: A sealing ring (19) is provided on the lower wall of the threaded bottom (21), and a vacuum gauge (20) is provided on the upper wall of the bucket lid (2).

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