Vacuum sublimation furnace capable of rapidly cooling

Abstract

The utility model relates to the technical field of vacuum sublimation furnaces, in particular to a quick-cooling vacuum sublimation furnace which comprises a vacuum sublimation furnace body, a nitrogen filling pipe used for primary cooling is arranged at the bottom of the vacuum sublimation furnace body, and a first cooling pipeline and a second cooling pipeline used for secondary cooling are arranged on the outer wall of the vacuum sublimation furnace body. When the vacuum sublimation furnace is used and the temperature is reduced to below 400 DEG C, inert gas serving as a heat conducting medium is slowly filled into the vacuum sublimation furnace body through the nitrogen filling pipe until the pressure in the furnace body is close to the atmospheric pressure, and the inert gas in the furnace body can quickly transfer heat to the pipe wall of the furnace body to achieve the purpose of accelerating cooling; and cold water which circularly passes through is introduced into the first cooling pipeline and the second cooling pipeline, so that the cooling speed is high, and a relatively good cooling effect on the vacuum sublimation furnace body can be achieved.

Description

Technical Field

[0001] The utility model relates to the technical field of vacuum sublimation furnaces, in particular to a vacuum sublimation furnace with rapid cooling. Background Art

[0002] A vacuum sublimation furnace is a device that performs sublimation under vacuum conditions. It is primarily used to prepare high-purity materials, particularly solid substances with a relatively high vapor pressure at their melting point. A vacuum sublimation furnace can purify solid substances by converting them directly into a gaseous state through sublimation in the absence of oxygen or reduced pressure, and then condensing them back into a solid state. The low pressure and absence of oxygen in a vacuum environment lower the sublimation temperature, allowing solid substances to sublime at lower temperatures. The purified sublimated material can then be collected through condensation. This process prevents the presence of liquid substances, reduces the influx of impurities, and thus improves product purity.

[0003] The vacuum sublimation furnace sublimates the material at 1100-1400 degrees in an atmosphere with a vacuum degree of less than 100pa. The cooling method is to cool the material by introducing cooling water into the furnace jacket. In a vacuum environment, when the temperature in the vacuum sublimation furnace drops below 400°C, the furnace core in the furnace barrel of the vacuum sublimation furnace cools down slowly, making the cooling time as long as 30 hours or more. However, during the operation of the vacuum sublimation furnace, since the reaction material is in a high vacuum environment (less than 100kPa), there are very few molecular collisions under high vacuum, which makes it difficult to transfer heat and dissipate heat slowly. The material can only be cooled by thermal radiation, so the cooling is very slow, which will affect the cooling of the vacuum sublimation furnace. Therefore, a vacuum sublimation furnace with rapid cooling is now proposed. Utility Model Content

[0004] The purpose of the utility model is to solve the problem in the prior art that when the temperature in the vacuum sublimation furnace drops below 400°C, the furnace core in the furnace barrel of the vacuum sublimation furnace cools down slowly, resulting in a cooling time of more than 30 hours. However, during the operation of the vacuum sublimation furnace, since the reaction materials are in a high vacuum environment (less than 100kPa), there are very few molecular collisions under high vacuum, resulting in difficulty in heat transfer and slow heat dissipation. The materials can only be cooled by thermal radiation, so the cooling is very slow, which affects the cooling of the vacuum sublimation furnace. Therefore, a vacuum sublimation furnace with rapid cooling is proposed.

[0005] In order to achieve the above purpose, the present invention adopts the following technical solutions:

[0006] A rapid cooling vacuum sublimation furnace comprises a vacuum sublimation furnace body, the bottom of which is provided with a nitrogen flushing pipe for preliminary cooling, and an outer wall of which is provided with a first cooling pipe and a second cooling pipe for further cooling.

[0007] Preferably, a support plate for supporting the vacuum sublimation furnace body is symmetrically fixedly connected to the bottom of the vacuum sublimation furnace body.

[0008] Preferably, the first cooling pipe and the second cooling pipe are both in a snake shape, and the inner walls of the first cooling pipe and the second cooling pipe are in contact with the outer wall of the vacuum sublimation furnace body.

[0009] Preferably, the bottom of one end of each of the first cooling pipe and the second cooling pipe is fixedly connected to a water inlet pipe, and the bottom of the other end of each of the first cooling pipe and the second cooling pipe is fixedly connected to a water outlet pipe.

[0010] Preferably, a U-shaped connecting plate is inserted between the first cooling pipe and the second cooling pipe, a first threaded hole is provided on one outer wall of the connecting plate, and a second threaded hole is provided on the other outer wall of the connecting plate, a plurality of first connecting grooves coaxially arranged with the first threaded hole are provided on the first cooling pipe, a plurality of second connecting grooves coaxially arranged with the second threaded hole are provided on the second cooling pipe, a first bolt threadedly connected to the first threaded hole is inserted inside the first connecting groove, and a second bolt threadedly connected to the second threaded hole is inserted inside the second connecting groove.

[0011] Preferably, a circular hole is opened at the bottom of the vacuum sublimation furnace body, the nitrogen flushing pipe is fixedly connected to the inner wall of the circular hole, the interior of the nitrogen flushing pipe and the interior of the vacuum sublimation furnace body are mutually connected, the outer wall of the nitrogen flushing pipe is fixedly connected to a vacuum valve, and a quick connector is installed at the bottom of the nitrogen flushing pipe.

[0012] Compared with the prior art, the beneficial effects of the present invention are:

[0013] In contrast, the thermal conductivity of nitrogen is much larger, close to that of air, because the molecules in nitrogen can transfer heat through collision. When the temperature drops below 400℃, inert gas is slowly filled into the interior of the vacuum sublimation furnace body through the nitrogen flushing pipe as a heat transfer medium until the pressure inside the furnace body approaches atmospheric pressure. The inert gas in the furnace body will quickly transfer heat to the furnace body tube wall to achieve the purpose of accelerated cooling. Combined with the circulation of cold water in the first cooling pipe and the second cooling pipe, the cooling speed is very fast, which can have a good cooling effect on the vacuum sublimation furnace body. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 This is a schematic diagram of the external three-dimensional structure of the rapid cooling vacuum sublimation furnace proposed in the present invention;

[0015] Figure 2 This is a schematic diagram of the bottom three-dimensional structure of the rapid cooling vacuum sublimation furnace proposed in the present invention;

[0016] Figure 3 Schematic diagram of the three-dimensional structure of the connection between the first cooling pipe, the second cooling pipe and the connecting plate;

[0017] Figure 4 This is a schematic diagram of the three-dimensional structure of the connection between the second cooling pipe, the water inlet pipe and the water outlet pipe;

[0018] Figure 5 This is a schematic diagram of the three-dimensional connection structure of the first cooling pipe, the second cooling pipe, the connecting plate, the first bolt, and the second bolt.

[0019] In the figure: 1. Vacuum sublimation furnace body; 2. Nitrogen flushing pipe; 3. First cooling pipe; 4. Second cooling pipe; 5. Support plate; 6. Water inlet pipe; 7. Water outlet pipe; 8. Connecting plate; 9. First threaded hole; 10. Second threaded hole; 11. First connecting groove; 12. Second connecting groove; 13. First bolt; 14. Second bolt; 15. Round hole; 16. Vacuum valve; 17. Quick connector. DETAILED DESCRIPTION

[0020] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0021] Reference Figure 1-Figure 5 The rapid cooling vacuum sublimation furnace comprises a vacuum sublimation furnace body 1, a nitrogen flushing pipe 2 for preliminary cooling is provided at the bottom of the vacuum sublimation furnace body 1, and a first cooling pipe 3 and a second cooling pipe 4 for further cooling are provided on the outer wall of the vacuum sublimation furnace body 1.

[0022] It should be noted that the vacuum sublimation furnace body 1 and the quick connector 17 are both existing technologies. The specific model specifications need to be selected and determined based on the actual specifications of the device. The specific selection calculation method adopts the existing technology in this field, so it is not explained. Both can be powered by external equipment and controlled to be turned on and off.

[0023] Furthermore, a support plate 5 for supporting the vacuum sublimation furnace body 1 is symmetrically fixedly connected to the bottom of the vacuum sublimation furnace body 1 .

[0024] It should be noted that the vacuum sublimation furnace body 1 can be supported and fixed by the two support plates 5 .

[0025] Furthermore, the first cooling pipe 3 and the second cooling pipe 4 are both in a snake shape, and the inner walls of the first cooling pipe 3 and the second cooling pipe 4 are in contact with the outer wall of the vacuum sublimation furnace body 1 .

[0026] It should be noted that a cavity for conveying water is provided inside the first cooling pipe 3 and the second cooling pipe 4. By circulating cold water through the first cooling pipe 3 and the second cooling pipe 4, a good cooling effect can be achieved on the vacuum sublimation furnace body 1.

[0027] It should be noted that the first cooling pipe 3 and the second cooling pipe 4 are both made of stainless steel and have good thermal conductivity.

[0028] Furthermore, the bottom of one end of the first cooling pipe 3 and the second cooling pipe 4 are fixedly connected to the water inlet pipe 6, and the bottom of the other end of the first cooling pipe 3 and the second cooling pipe 4 are fixedly connected to the water outlet pipe 7.

[0029] It should be noted that a water tank can be set on one side of the vacuum sublimation furnace body 1, and two water pumps can be set inside the water tank. One end of the two water pumps is provided with a water suction pipe, and the other ends of the two water pumps are connected to the water inlet pipe 6 through two water pipes respectively. A drain pipe is installed at the bottom of the outlet pipe 7, and the drain pipe extends to the inside of the water tank, so that the water pump can suck water in and discharge it into the first cooling pipe 3 and the second cooling pipe 4, and then discharge it from the drain pipe to the inside of the water tank for recycling. When the temperature of the water inside the water tank is no longer low, the water inside the water tank can be discharged and new cold water can be re-injected.

[0030] Furthermore, a U-shaped connecting plate 8 is inserted between the first cooling pipe 3 and the second cooling pipe 4, a first threaded hole 9 is provided on the outer wall of one side of the connecting plate 8, and a second threaded hole 10 is provided on the outer wall of the other side of the connecting plate 8. The first cooling pipe 3 is provided with a plurality of first connecting grooves 11 coaxially arranged with the first threaded hole 9, and the second cooling pipe 4 is provided with a plurality of second connecting grooves 12 coaxially arranged with the second threaded hole 10. A first bolt 13 threadedly connected to the first threaded hole 9 is inserted inside the first connecting groove 11, and a second bolt 14 threadedly connected to the second threaded hole 10 is inserted inside the second connecting groove 12.

[0031] It should be noted that the first bolt 13 is screwed into the first threaded hole 9 and inserted into the inside of the first connecting groove 11, and then the second bolt 14 is screwed into the second threaded hole 10 and inserted into the inside of the second connecting groove 12. In this way, the first cooling pipe 3 and the second cooling pipe 4 can be fixed to the outer wall of the vacuum sublimation furnace body 1 without falling off, and it is also convenient to disassemble the first cooling pipe 3 and the second cooling pipe 4.

[0032] Furthermore, a circular hole 15 is opened at the bottom of the vacuum sublimation furnace body 1, the nitrogen flushing pipe 2 is fixedly connected to the inner wall of the circular hole 15, the interior of the nitrogen flushing pipe 2 and the interior of the vacuum sublimation furnace body 1 are mutually connected, the outer wall of the nitrogen flushing pipe 2 is fixedly connected to a vacuum valve 16, and a quick connector 17 is installed at the bottom of the nitrogen flushing pipe 2.

[0033] It should be noted that the opening and closing of the nitrogen flushing pipe 2 can be controlled by the vacuum valve 16, and the external air intake pipe can be conveniently connected through the quick connector 17.

[0034] It's important to note that nitrogen has a thermal conductivity of approximately 0.0258 W / m·°C. This value, similar to that of air, indicates its excellent thermal conductivity, leading to its frequent use in refrigeration and nitrogen cooling. Its unique physical and chemical properties make nitrogen a useful gas in certain applications, particularly in environments requiring temperature control or oxidation prevention.

[0035] It should be noted that during equipment operation, the reaction materials are in a high vacuum (less than 100kPa). Due to the extremely low molecular collisions under high vacuum, heat transfer is difficult and heat dissipation is slow. The materials can only be cooled by thermal radiation, so the cooling is very slow. In contrast, the thermal conductivity of nitrogen is much larger, close to that of air, because the molecules in nitrogen can transfer heat through collisions. Therefore, when the temperature is below 400 degrees, slowly introducing nitrogen is conducive to rapid cooling, reducing the cooling time from the original 30 hours to 18-20 hours.

[0036] It should be noted that nitrogen cannot be introduced when the temperature is too high. If the temperature is too high, nitrogen will react with the equipment components to generate nitrides, which will affect the service life of the equipment components.

[0037] Working principle of this utility model:

[0038] When the temperature drops below 400°C, inert gas is slowly filled into the interior of the vacuum sublimation furnace body 1 through the nitrogen flushing pipe 2 as a heat transfer medium until the pressure inside the furnace body approaches atmospheric pressure. The inert gas in the furnace body will quickly transfer heat to the furnace body tube wall to achieve the purpose of accelerated cooling. Combined with the circulation of cold water into the first cooling pipe 3 and the second cooling pipe 4, the cooling speed is very fast, which can achieve a good cooling effect on the vacuum sublimation furnace body 1.

[0039] The above are only preferred specific implementation methods of the present invention, but the protection scope of the present invention is not limited to them. Any technician familiar with the technical field can make equivalent replacements or changes based on the technical solution and utility model concept of the present invention within the technical scope disclosed by the present invention, and they should be covered by the protection scope of the present invention.

Claims

1. A vacuum sublimation furnace with rapid cooling, comprising a vacuum sublimation furnace body (1), characterized in that: The bottom of the vacuum sublimation furnace body (1) is provided with a nitrogen flushing pipe (2) for preliminary cooling, and the outer wall of the vacuum sublimation furnace body (1) is provided with a first cooling pipe (3) and a second cooling pipe (4) for further cooling.

2. The rapid cooling vacuum sublimation furnace according to claim 1, characterized in that: A support plate (5) for supporting the vacuum sublimation furnace body (1) is symmetrically fixedly connected to the bottom of the vacuum sublimation furnace body (1).

3. The rapid cooling vacuum sublimation furnace according to claim 1, characterized in that: The first cooling pipe (3) and the second cooling pipe (4) are both in a snake shape, and the inner walls of the first cooling pipe (3) and the second cooling pipe (4) are both in contact with the outer wall of the vacuum sublimation furnace body (1).

4. The rapid cooling vacuum sublimation furnace according to claim 1, characterized in that: The bottoms of one end of each of the first cooling pipe (3) and the second cooling pipe (4) are fixedly connected to a water inlet pipe (6), and the bottoms of the other end of each of the first cooling pipe (3) and the second cooling pipe (4) are fixedly connected to a water outlet pipe (7).

5. The rapid cooling vacuum sublimation furnace according to claim 1, characterized in that: A U-shaped connecting plate (8) is inserted between the first cooling pipe (3) and the second cooling pipe (4), a first threaded hole (9) is provided on one side outer wall of the connecting plate (8), and a second threaded hole (10) is provided on the other side outer wall of the connecting plate (8), a plurality of first connecting grooves (11) coaxially arranged with the first threaded hole (9) are provided on the first cooling pipe (3), a plurality of second connecting grooves (12) coaxially arranged with the second threaded hole (10) are provided on the second cooling pipe (4), a first bolt (13) threadedly connected to the first threaded hole (9) is inserted inside the first connecting groove (11), and a second bolt (14) threadedly connected to the second threaded hole (10) is inserted inside the second connecting groove (12).

6. The rapid cooling vacuum sublimation furnace according to claim 1, characterized in that: A circular hole (15) is provided at the bottom of the vacuum sublimation furnace body (1); the nitrogen flushing pipe (2) is fixedly connected to the inner wall of the circular hole (15); the interior of the nitrogen flushing pipe (2) and the interior of the vacuum sublimation furnace body (1) are interconnected; a vacuum valve (16) is fixedly connected to the outer wall of the nitrogen flushing pipe (2); and a quick connector (17) is installed at the bottom of the nitrogen flushing pipe (2).

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