A vacuum sublimation purification furnace for purifying high-purity metals

Abstract

The present invention discloses a vacuum sublimation purification furnace for purifying high-purity metals, which includes a heating furnace, a purification device, a purification furnace frame table (11), a vacuum pump (10), and an electrical controller (13). The purification device includes a purification container (6) and a plurality of condensation rings (5) installed inside the purification container (6); one end of the purification container (6) is open, and the open end of the purification container (6) is connected to a vacuum gauge (9) and a vacuum pump (10); the heating furnace includes a heating furnace body (1) and a furnace door (3), the furnace door is installed at one end of the heating furnace body, and the furnace door is close to the purification container; the tabletop of the purification furnace frame table is provided with a furnace body moving guide rail (15), and the heating furnace body is installed on the furnace body moving guide rail; the electrical controller is installed on the side of the purification furnace frame table. The device of the present invention has a simple structure, can improve the vacuum degree inside the device, reduce the probability of vacuum leakage, simplify the operation, and improve the production efficiency.

Description

Technical Field

[0001] The present invention belongs to the technical field of vacuum sublimation purification furnaces, and particularly relates to a vacuum sublimation purification furnace for purifying high-purity metals. Background Art

[0002] Under vacuum heating conditions, a vacuum sublimation purification furnace sublimes substances, and different substances condense in different temperature ranges to separate different substances, thereby achieving the purpose of purification. Currently, the existing device has an integral structure of the furnace body and the purification device. The internal structure of the purification device is complex, and there are two or more places in the whole system that require sealing means, which is prone to vacuum leakage. Some purification devices have a complex internal structure, are difficult to prepare, and are not easy to operate. Summary of the Invention

[0003] Aiming at the problems in the prior art, the present invention provides a vacuum sublimation purification furnace for purifying high-purity metals. By designing a purification device with a single-end opening, the present invention improves the vacuum degree inside the purification device and reduces the probability of vacuum leakage.

[0004] The present invention adopts the following technical solutions:

[0005] A vacuum sublimation purification furnace for purifying high-purity metals, characterized in that the purification furnace includes a heating furnace, a purification device, a purification furnace frame table (11), a vacuum gauge (9), a vacuum pump (10), and an electrical controller (13). The purification device includes a purification container (6) and a plurality of condensation rings (5), and the plurality of condensation rings (5) are all installed inside the purification container (6); one end of the purification container (6) is open, and the open end of the purification container (6) is connected to the vacuum gauge (9) and the vacuum pump (10), and the purification container (6) is installed on the table surface of the purification furnace frame table (11); the heating furnace includes a heating furnace body (1), a thermocouple, and a furnace door (3). The furnace door (3) is installed at one end of the heating furnace body (1), and the furnace door (3) is close to the purification container (6); the thermocouple is installed inside the heating furnace body (1); the table surface of the purification furnace frame table (11) is provided with a furnace body moving guide rail (15), and the heating furnace body (1) is installed on the furnace body moving guide rail (15); the table surface of the purification furnace frame table (11) is provided with a plurality of fans (12), and the plurality of fans (12) are all located directly below the purification container (6); the electrical controller (13) is installed on the side of the purification furnace frame table (11), and the heating element, thermocouple, vacuum pump (10), vacuum gauge (9), and plurality of fans (12) inside the heating furnace body (1) are all connected to the electrical controller (13).

[0006] According to the above-mentioned vacuum sublimation purification furnace for purifying high-purity metals, it is characterized in that a furnace body moving handle (14) is installed on the side of the purification furnace frame table (11), and the furnace body moving handle (14) is connected to the heating furnace body (1).

[0007] According to the above-mentioned vacuum sublimation purification furnace for purifying high-purity metals, it is characterized in that a furnace door opening and closing handle (2) is installed on the heating furnace body (1), and the furnace door opening and closing handle (2) is connected to the furnace door (3).

[0008] According to the above-mentioned vacuum sublimation purification furnace for purifying high-purity metals, it is characterized in that the purification container (6) is installed on the tabletop of the purification furnace frame platform (11) through a support mechanism. The support mechanism includes a first bracket (4) and a second bracket plus a fixing ring (7). One end of the first bracket (4) is connected to the tabletop of the purification furnace frame platform (11), and the other end of the first bracket (4) supports the bottom of the purification container (6); one end of the second bracket plus the fixing ring (7) is connected to the tabletop of the purification furnace frame platform (11), and the other end of the second bracket plus the fixing ring (7) is a fixing ring, and the fixing ring is sleeved on the outer surface of the purification container (6).

[0009] According to the above-mentioned vacuum sublimation purification furnace for purifying high-purity metals, it is characterized in that a plurality of fans (12) are installed inside the purification furnace frame platform (11).

[0010] According to the above-mentioned vacuum sublimation purification furnace for purifying high-purity metals, it is characterized in that a vacuum flange (8) is installed at the open end of the purification container (6), the vacuum flange (8) is connected to a vacuum gauge (9) through a pipeline, and the vacuum gauge (9) is connected to a vacuum pump (10) through a pipeline.

[0011] According to the above-mentioned vacuum sublimation purification furnace for purifying high-purity metals, it is characterized in that a heat insulation layer is installed on the inner wall of the heating furnace body (1); the shape of the heating furnace body (1) is a cylinder or a hollow cuboid.

[0012] According to the above-mentioned vacuum sublimation purification furnace for purifying high-purity metals, it is characterized in that there is a heating furnace tube inside the heating furnace body (1), an electric heating wire is wound around the heating furnace tube, and the temperature inside the heating furnace body (1) is controlled by single-stage heating or multi-stage heating; the temperature inside the heating furnace body (1) is controlled by a single thermocouple or multiple thermocouples.

[0013] According to the above-mentioned vacuum sublimation purification furnace for purifying high-purity metals, it is characterized in that the material of the purification container (6) is glass or quartz.

[0014] According to the above-mentioned vacuum sublimation purification furnace for purifying high-purity metals, it is characterized in that the material of the condensation ring (5) is glass or quartz.

[0015] Advantageous technical effects of the present invention: The present invention adopts a multi-stage temperature control, which can set different furnace temperature distributions according to the needs of the purification material, so as to accurately control the sublimation and condensation of the material. The multi-section condensation ring designed by the present invention can cooperate with the furnace temperature curve to collect different materials at different positions to achieve the effect of precise purification; after adopting the condensation ring, the operation can be simplified and the work efficiency can be improved. The present invention is provided with a furnace body moving guide rail, so that the heating furnace body can move on the furnace body moving guide rail. Therefore, during the whole purification process, the purification container does not need to be moved, avoiding damage to the internal vacuum thereof. The multi-stage temperature control system can set different furnace temperature curves to meet the needs of different material purifications. At the same time, a plurality of condensation rings are placed inside the purification container. After the material to be purified sublimes, substances with different vapor pressures and condensation points condense in different temperature sections and adhere to different condensation rings, facilitating the separation of different substances. The structure of separating the furnace body from the purification device and the device for moving the furnace body designed by the present invention can play two roles: one is that the separation of the furnace body from the purification device can simultaneously raise the temperature of the furnace chamber and evacuate the purification device, which can shorten the working cycle; the other is that the purification device enters the furnace chamber for heating after the vacuum degree reaches the requirement, which can avoid the oxidation phenomenon of the material when heated under low vacuum. Brief Description of the Drawings

[0016] Figure 1 It is a schematic structural diagram of the present invention. Detailed Embodiments

[0017] See Figure 1, a vacuum sublimation purification furnace for purifying high-purity metals according to the present invention, includes a heating furnace, a purification device, a purification furnace frame table 11, a vacuum gauge 9, a vacuum pump 10, and an electrical controller 13. The purification device includes a purification container 6 and a plurality of condensation rings 5. The plurality of condensation rings 5 are all installed inside the purification container 6. The material of the condensation ring 5 is glass or quartz or other materials. The condensation ring 5 is a hollow ring-shaped component with a certain length. The outer diameter of the condensation ring 5 is slightly smaller than the inner diameter of the purification container, and the length of the condensation ring 5 is 100 - 200 mm. One end of the purification container 6 is open, and the open end of the purification container 6 is connected to the vacuum gauge 9 and the vacuum pump 10. The purification container 6 is installed on the tabletop of the purification furnace frame table 11. The purification container 6 is a tubular container with one end closed and the other end open. A vacuum flange 8 is installed at the open end of the purification container 6. The vacuum flange 8 is connected to the vacuum gauge 9 through a pipeline, and the vacuum gauge 9 is connected to the vacuum pump 10 through a pipeline. The heating furnace includes a heating furnace body 1 and a furnace door 3. The heating furnace body 1 includes a heating furnace outer shell, a heating furnace tube, and a heating element. The heating element can be a linear resistance wire, a loop-shaped resistance wire, or other heating materials. The furnace door 3 is installed at one end of the heating furnace body 1, and the furnace door 3 is close to the purification container 6. A thermocouple is installed inside the heating furnace body 1. A furnace body moving guide rail 15 is installed on the tabletop of the purification furnace frame table 11. The heating furnace body 1 is installed on the furnace body moving guide rail 15, and the heating furnace body 1 can move on the furnace body moving guide rail 15 to allow the purification container 6 to enter or exit the furnace cavity. The length of the furnace body moving guide rail 15 is 3400 - 4000 mm, and its cross-section is circular or rectangular or other shapes, and its diameter or side length is 15 - 20 mm. A plurality of fans 12 are installed on the tabletop of the purification furnace frame table 11. The plurality of fans 12 are all located directly below the purification container 6, and the plurality of fans 12 are all installed inside the purification furnace frame table 11. The electrical controller 13 is installed on the side of the purification furnace frame table 11. The heating element, thermocouple, vacuum pump 10, vacuum gauge 9, and plurality of fans 12 inside the heating furnace body 1 are all connected to the electrical controller 13. A furnace body moving handle 14 is installed on the side of the purification furnace frame table 11. The furnace body moving handle 14 is connected to the heating furnace body 1. By rotating the furnace body moving handle 14, the front and back sliding of the heating furnace body 1 is realized. The furnace body moving handle 14 can be in a manual operation mode or an electric operation mode through a motor. After the heating furnace slides towards the purification container, the furnace chamber of the heating furnace body 1 surrounds the purification container 6.

[0018] The furnace body 1 of the heating furnace is equipped with a furnace door opening and closing handle 2, which is connected to the furnace door 3. By controlling the furnace door opening and closing handle 2, the opening and closing of the furnace door 3 can be realized, so as to facilitate the entry and exit of the purification container 6 into or out of the furnace chamber. The purification container 6 is installed on the tabletop of the purification furnace frame platform 11 through a support mechanism. The support mechanism includes a first bracket 4, a second bracket plus a fixing ring 7. One end of the first bracket 4 is connected to the tabletop of the purification furnace frame platform 11, and the other end of the first bracket 4 supports the bottom of the purification container 6; the first bracket 4 is a bracket that reciprocally flips at 90 degrees. The U-shaped top end of the first bracket 4 supports the purification container, and the bottom of the first bracket 4 is fixed on the tabletop of the purification furnace frame platform 11. When the furnace body 1 of the heating furnace moves towards the purification container 6, the first bracket 4 is pressed and falls towards the tabletop of the purification furnace frame platform 11. The purification container 6 is then placed on the furnace tube of the heating furnace 1. When the heating furnace moves in the direction away from the purification container 6, the pressure on the first bracket 4 disappears, and it flips back to the upright state to support the purification container 6. One end of the second bracket plus the fixing ring 7 is connected to the tabletop of the purification furnace frame platform 11, and the other end is a fixing ring that is sleeved on the outer surface of the purification container 6. The material of the purification container 6 is glass or quartz or other materials. Its cross-section is a circle with an inner diameter of 100 - 250 mm, or a square with a side length of 100 - 200 mm, or a rectangle with a side length of 100 - 200 mm. The length of the purification container 6 is 1800 - 2800 mm..

[0019] The inner wall of the furnace body 1 of the heating furnace is installed with a heat insulation layer; the outer shape of the furnace body 1 of the heating furnace is a cuboid box structure or a cylindrical barrel structure. When the outer shape of the furnace body 1 of the heating furnace is a cuboid box structure, the length of the furnace body 1 of the heating furnace is 1500 - 2500 mm, and its cross-section is a square or a rectangle, and the side length of the cross-section is 160 - 360 mm; the cross-section of the internal furnace tube is a circle with a diameter of 110 - 300 mm, or a square with a side length of 110 - 210 mm, or a rectangle with a side length of 110 - 210 mm inside. When the outer shape of the furnace body 1 of the heating furnace is a cylindrical barrel structure, the length of the furnace body 1 of the heating furnace is 1500 - 2500 mm, its cross-section is a circle, the outer diameter of the cross-section is 160 - 360 mm, and the inner diameter of the furnace tube is a circle with a diameter of 110 - 300 mm, or a square with a side length of 110 - 210 mm, or a rectangle with a side length of 110 - 210 mm inside. There is a heating furnace tube inside the furnace body 1 of the heating furnace, and an electric heating wire is wound around the heating furnace tube. The temperature inside the furnace body 1 of the heating furnace is controlled by single-stage heating or multi-stage heating; the temperature inside the furnace body 1 of the heating furnace is controlled by a single thermocouple or multiple thermocouples.

[0020] Working principle: The staff can control the movement of the heating furnace body 1 left and right on the furnace body movement guide rail 15 through the furnace body movement handle 14. When the purification container 6 needs to be heated, move the heating furnace body 1 so that the bottom and part of the area of the purification container 6 enter the furnace chamber inside the heating furnace body 1. When the purification is completed, move the heating furnace body 1 to withdraw the purification container 6 from the heating furnace chamber. After the purification container 6 is cooled to room temperature, take out the condensation ring 5 in the purification container 6, and obtain products with different purities from different condensation rings.

[0021] During operation, load the substance to be purified at the bottom of the purification container 6, place several condensation rings 5 in sequence in the middle of the purification container 6, place the purification container 6 on the bracket as shown in the figure, lock the fixing ring, install the vacuum flange 8, and turn on the vacuum pump 10. At the same time, raise the temperature of the heating furnace chamber. When the inside of the purification container 6 reaches the predetermined vacuum degree and the furnace temperature reaches the predetermined temperature, open the furnace door 3, move the heating furnace body 1, and let part of the area of the purification container 6 near the closed end enter the furnace chamber. After the raw materials at the bottom of the purification container 6 are completely sublimated, move the heating furnace body 1 away, let the purification container 6 completely out of the furnace chamber of the heating furnace body 1, close the furnace door 3, and turn on multiple fans 12 to accelerate the cooling of the purification container 6. After the purification container 6 is cooled to room temperature, turn off the vacuum pump 10 and take out the condensation rings 5 one by one.

Claims

1. A vacuum sublimation purification furnace for purifying high-purity metals, characterized in that, the purification furnace includes a heating furnace, a purification device, a purification furnace frame table (11), a vacuum gauge (9), a vacuum pump (10), and an electrical controller (13). The purification device includes a purification container (6) and a plurality of condensation rings (5), and the plurality of condensation rings (5) are all installed inside the purification container (6); one end of the purification container (6) is open, and the open end of the purification container (6) is connected to the vacuum gauge (9) and the vacuum pump (10), and the purification container (6) is installed on the tabletop of the purification furnace frame table (11); the heating furnace includes a heating furnace body (1), a thermocouple, and a furnace door (3), the furnace door (3) is installed at one end of the heating furnace body (1), and the furnace door (3) is close to the purification container (6); the thermocouple is installed inside the heating furnace body (1); the tabletop of the purification furnace frame table (11) is provided with a furnace body moving guide rail (15), and the heating furnace body (1) is installed on the furnace body moving guide rail (15); the tabletop of the purification furnace frame table (11) is provided with a plurality of fans (12), and the plurality of fans (12) are all located directly below the purification container (6); the electrical controller (13) is installed on the side of the purification furnace frame table (11), and the heating element, thermocouple, vacuum pump (10), vacuum gauge (9), and plurality of fans (12) inside the heating furnace body (1) are all connected to the electrical controller (13); there is a heating furnace tube inside the heating furnace body (1), and an electric heating wire is wound around the heating furnace tube, and the temperature inside the heating furnace body (1) is controlled by single-stage heating or multi-stage heating; the temperature inside the heating furnace body (1) is controlled by a single thermocouple or multiple thermocouples.

2. The vacuum sublimation purification furnace for purifying high-purity metals according to claim 1, characterized in that, a furnace body moving handle (14) is installed on the side of the purification furnace frame table (11), and the furnace body moving handle (14) is connected to the heating furnace body (1).

3. The vacuum sublimation purification furnace for purifying high-purity metals according to claim 1, characterized in that, a furnace door opening and closing handle (2) is installed on the heating furnace body (1), and the furnace door opening and closing handle (2) is connected to the furnace door (3).

4. The vacuum sublimation purification furnace for purifying high-purity metals according to claim 1, characterized in that, the purification container (6) is installed on the tabletop of the purification furnace frame table (11) through a support mechanism, and the support mechanism includes a first support (4) and a second support plus a fixing ring (7). One end of the first support (4) is connected to the tabletop of the purification furnace frame table (11), and the other end of the first support (4) supports the bottom of the purification container (6); one end of the second support plus a fixing ring (7) is connected to the tabletop of the purification furnace frame table (11), and the other end of the second support plus a fixing ring (7) is a fixing ring, and the fixing ring is sleeved on the outer surface of the purification container (6).

5. The vacuum sublimation purification furnace for purifying high-purity metals according to claim 1, characterized in that, the plurality of fans (12) are all installed inside the purification furnace frame table (11).

6. The vacuum sublimation purification furnace for purifying high-purity metal according to claim 1, characterized in that, one end of the opening of the purification container (6) is provided with a vacuum flange (8), the vacuum flange (8) is connected to a vacuum gauge (9) through a pipeline, and the vacuum gauge (9) is connected to a vacuum pump (10) through a pipeline.

7. The vacuum sublimation purification furnace for purifying high-purity metal according to claim 1, characterized in that, the material of the purification container (6) is glass or quartz.

8. The vacuum sublimation purification furnace for purifying high-purity metal according to claim 1, characterized in that, the material of the condensation ring (5) is glass or quartz.

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