High-temperature and high-vacuum smelting device for high-purity rhenium and preparation method

Abstract

According to the high-temperature and high-vacuum smelting device for the high-purity metal rhenium and the preparation method, the structure of the high-temperature and high-vacuum smelting device for the high-purity metal rhenium is improved, the vacuum degree in the device is adjusted separately in the purification process of the metal rhenium, and the metal rhenium is heated step by step, so that the temperature and energy consumption required for smelting the metal rhenium are effectively reduced; the process efficiency is greatly improved, and the heating and cooling time is shortened. In addition, by setting the sintering temperature and the vacuum degree, volatilization and oxidation of metal rhenium can be reduced, loss in the purification process is reduced, and the utilization rate of raw materials is increased. And as the process efficiency is improved and the loss is reduced, the production cost is further reduced, so that the economic benefit of the high-temperature and high-vacuum smelting and purifying process for the metal rhenium is improved.

Description

Technical Field

[0001] The present application relates to the technical field of high-purity metal preparation, and in particular to a high-temperature and high-vacuum melting device and a preparation method for high-purity metal rhenium. Background Art

[0002] Rhenium metal has high melting point, high strength, high density, good plasticity and excellent mechanical stability. It has good creep resistance and heat shock resistance under high temperature and rapid cooling and heating conditions. It is widely used in aerospace, petrochemical and electronic industries. With the continuous development of society and the continuous advancement of science and technology, the purity requirements of rhenium metal are getting higher and higher. At present, the largest use of high-purity rhenium metal is mainly used in the manufacture of single-crystal turbine blades of aircraft engines. The low melting and boiling point trace impurities in rhenium metal are easy to form inclusion cores in high-temperature chemical reactions and become fatigue crack sources. When the trace impurity elements are not controlled properly, harmful phases (such as σ and µ phases) will precipitate to damage the strength and toughness of the alloy. Therefore, the requirements for trace impurity elements in rhenium metal are extremely strict.

[0003] The purification of metallic rhenium generally adopts the chemical-physical combined purification process, and chemical impurity removal is carried out through solvent extraction, ion exchange, recrystallization, high temperature and high vacuum melting, electron beam melting, zone melting, etc. Among them, compared with electron beam melting and zone melting technology, high temperature and high vacuum melting has many advantages such as high process yield and good purification effect, which is of great significance to the industrial production of high-purity metallic rhenium.

[0004] However, existing high-temperature and high-vacuum melting and purification usually requires the metal rhenium to be molten, which leads to problems such as slow process efficiency, large losses, and high costs, which is not conducive to improving the economic benefits of the high-temperature and high-vacuum melting and purification process of metal rhenium. Summary of the invention

[0005] In order to solve the above problems, the present invention provides a high-purity metal rhenium high-temperature high-vacuum melting device and a preparation method. By improving the structure of the high-purity metal rhenium high-temperature high-vacuum melting device, the vacuum degree of the device is adjusted step by step during the metal rhenium purification process, and the metal rhenium is heated step by step, thereby effectively reducing the temperature and energy consumption required for molten metal rhenium, greatly improving the process efficiency, and shortening the heating and cooling time. Among them, by setting the sintering temperature and vacuum degree, it is also helpful to reduce the volatilization and oxidation of metal rhenium, reduce the loss in the purification process, and improve the utilization rate of raw materials. Due to the improvement of process efficiency and the reduction of loss, the production cost is further reduced, which is conducive to improving the economic benefits of the high-temperature high-vacuum melting and purification process of metal rhenium.

[0006] In a first aspect, the present invention provides a high-purity metal rhenium high-temperature high-vacuum melting device, the device comprising: A furnace body (1), a heating component (3), a heat-insulating component (4) and a vacuum pump (5); A material rack (11) is provided in the furnace body (1), and the material rack (11) is used to place a crucible containing metal rhenium; The heating component (3) and the heat-insulating component (4) are both located in the furnace body (1), wherein the heating component (3) is sleeved outside the material rack (11), and the heat-insulating component (4) is sleeved outside the heating component (3); The heating component (3) is configured to heat the metal rhenium in the crucible; The vacuum pump (5) comprises a mechanical pump (51) and a molecular pump (52); an interface (115) is provided on one side of the furnace body (1); the mechanical pump (51) is connected to the interface (115), and the molecular pump (52) is connected to an end of the mechanical pump (51) away from the interface (115); The mechanical pump (51) is configured to adjust the vacuum degree inside the furnace body (1) to 10 -1 Pa~10 Pa; the molecular pump (52) is configured to be able to generate a vacuum when the vacuum degree inside the furnace body (1) is 10 -1 When the vacuum degree inside the furnace body (1) is adjusted to 10 -2 Pa~10 -6 Pa; The furnace body (1) is provided with a temperature control structure (2), and the temperature control structure (2) is configured to, when the vacuum degree in the furnace body (1) is 10 -2 Pa~10 -3 Pa, controlling the heating component (3) to heat the metal rhenium to 900°C to 1300°C; and when the vacuum degree in the furnace body (1) is 10 -4 Pa~10 -6 Pa, controlling the heating component (3) to heat the metal rhenium to 1800° C. to 2500° C.; The heat-insulating component (4) is configured to gather and reflect the heat generated by the heating component (3) so as to concentrate the heat on the heating component (3) for heating the metal rhenium.

[0007] Optionally, the distance between the heat preservation component (4) and the heating component (3) is 3 mm to 20 mm; The thermal insulation component (4) comprises a plurality of thermal insulation layers (41); The spacing between adjacent insulation layers is 0-5 mm.

[0008] Optionally, the material of the thermal insulation layer (41) is metal rhenium.

[0009] Optionally, the heating assembly (3) comprises a first heating net (31), a second heating net (32) and a third heating net (33); Wherein, the first heating net (31) is sleeved around the material rack (11); The distance between the side of the first heating net (31) facing the material rack (11) and the material rack (11) is 3 mm to 20 mm; the distance between the side of the first heating net (31) facing away from the material rack (11) and the thermal insulation component (4) is 3 mm to 20 mm; The material rack (11) is provided with a first end (111) and a second end (112) opposite to each other, the second heating net (32) is fixed to the first end (111), and the third heating net (33) is fixed to the second end (112).

[0010] Optionally, the first heating net (31), the second heating net (32) and the third heating net (33) are made of tungsten.

[0011] Optionally, the material rack (11) comprises at least one storage plate (113) and a support rod (114); The placement plate (113) is sleeved on the support rod (114), the placement plate (113) is vertically fixed to the support rod (114), and the placement plate (113) is used to place at least one of the crucibles.

[0012] In a second aspect, the present invention provides a high-purity metal rhenium high-temperature high-vacuum melting preparation method, which is applicable to the high-purity metal rhenium high-temperature high-vacuum melting device described in the first aspect, and the preparation method comprises: S1. Put an appropriate amount of metal rhenium blank into a crucible, and place the crucible containing the blank on a material rack (11); S2, start the mechanical pump (51) and adjust the vacuum degree inside the furnace body (1) to 10 -1 Pa~10 Pa, and then start the molecular pump (52), which adjusts the vacuum degree inside the furnace body (1) to 10 -2 Pa~10 -3 After 0.040 ℃, the temperature control structure (2) controls the heating component (3) to heat the crucible and the blank in the crucible to 900 ℃ to 1300 ℃, and perform a pre-sintering treatment for 1 h to 3 h; S3, after the pre-sintering treatment, the vacuum degree inside the furnace body (1) is adjusted to 10 -4 Pa~10 -6Pa, the temperature control structure (2) controls the heating component (3) to heat the crucible and the blank in the crucible to 1800°C to 2500°C, perform a high-temperature sintering treatment for 1 h to 3 h, and obtain high-purity metallic rhenium after cooling; Wherein, the purity of the high-purity metallic rhenium is greater than 99.99%.

[0013] Optionally, in S2, the temperature control structure (2) controls the heating rate of the heating component (3) to be 8°C / min to 15°C / min.

[0014] Optionally, in S3, the temperature control structure (2) controls the heating rate of the heating component (3) to be 5°C / min to 10°C / min.

[0015] Optionally, in S3, the step of cooling includes: The temperature control structure (2) controls the heating component (3) to cool down at a rate of 10°C / min to 15°C / min until the temperature in the crucible drops to 800°C to 1000°C, and then the temperature control structure (2) and the heating component (3) are closed to allow the crucible and the high-purity metal rhenium in the crucible to naturally cool down to 100°C to 300°C.

[0016] In summary, the present invention includes at least one of the following beneficial technical effects: 1. The present invention provides a high-purity rhenium metal high-temperature and high-vacuum melting device, which mainly includes: a furnace body, a heating component, a heat preservation component and a vacuum pump, wherein the furnace body is also provided with a temperature control structure, and the vacuum pump includes a mechanical pump and a molecular pump; during implementation, the vacuum pump is controlled to accurately adjust the vacuum degree in the furnace body and control the heating temperature of the heating component to achieve efficient purification of the rhenium metal; the setting of the heat preservation component enables the heat generated by the heating component to act more concentratedly on the rhenium metal, reducing the heat loss during the purification process, thereby reducing the overall energy consumption of the device and the loss of rhenium metal; at the same time, when the vacuum pump adjusts the vacuum degree in the furnace body, especially when the vacuum degree in the furnace body reaches 10 -6 When the temperature is 0.0400°C, the high-temperature sintering treatment can further remove the impurities remaining in the metal rhenium to obtain metal rhenium with higher purity; the setting of the vacuum pump can also help reduce the gas residue in the furnace body, further reducing the oxidation and volatilization of the metal rhenium at high temperatures; due to the improvement of the purification efficiency and the reduction of losses in the purification process during the operation of the device, the production cost is reduced, thereby improving the overall economic benefits of the process; 2. The present invention provides a high-temperature and high-vacuum smelting preparation method for high-purity metallic rhenium. Through staged heating treatment (i.e., pre-sintering and high-temperature sintering) and precise control under different vacuum degrees, the purification process of metallic rhenium is made more efficient; wherein, the pre-sintering stage helps to remove some low-boiling impurities and gases in the metallic rhenium, laying a good foundation for the high-temperature sintering stage, thereby improving the overall purification efficiency; and by precisely controlling the heating temperature and vacuum degree in the high-temperature sintering stage, high-boiling impurities in the solid metallic rhenium, such as oxides, carbides, etc., can be effectively removed, thereby obtaining high-purity metallic rhenium with a purity greater than 99.99%, avoiding unnecessary energy consumption and waste, reducing the loss of raw materials, and reducing production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the description of the embodiments of the present application will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0018] Figure 1 The schematic diagram of the structure of the high-purity metal rhenium high-temperature and high-vacuum melting device proposed in the embodiment of the present application is shown; Figure 2 The flowchart of the high-temperature and high-vacuum melting preparation method of high-purity metallic rhenium proposed in the embodiment of the present application is shown.

[0019] Description of reference numerals: 1. Furnace body; 11. Material rack; 111. First end; 112. Second end; 113. Storage plate; 114. Support rod; 115. Interface; 116. Inflating port; 117. Inflating valve; 118. Deflating valve; 119. Water-cooled electrode interface; 2. Temperature control structure; 3. Heating assembly; 31. First heating net; 32. Second heating net; 33. Third heating net; 4. Insulation component; 41. Insulation layer; 5. Vacuum pump; 51. Mechanical pump; 52. Molecular pump. DETAILED DESCRIPTION

[0020] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0021] In the drawings, the size of the constituent elements, the thickness of the layer or the area may be exaggerated for the sake of clarity. Therefore, any implementation of the present disclosure is not necessarily limited to the size shown in the drawings, and the shapes and sizes of the components in the drawings do not reflect the true proportions. In addition, the drawings schematically show ideal examples, and any implementation of the present disclosure is not limited to the shapes or values ​​shown in the drawings.

[0022] In the related technology, metallic rhenium has a high melting point, high strength, high density, good plasticity and excellent mechanical stability. It has good creep resistance and heat shock resistance under high temperature and rapid cooling and heating conditions. It is widely used in aerospace, petrochemical, electronics and other industries.

[0023] The purification of metallic rhenium generally adopts a chemical-physical combined purification process. Chemical impurity removal is purified by means of solvent extraction, ion exchange, recrystallization, etc., and then high-purity rhenium powder is obtained through processes such as roasting and reduction, and then purified by means of high-temperature high-vacuum melting, electron beam melting, and zone melting. Among them, high-purity metallic rhenium of grade 5N (purity greater than 99.99%) or above is obtained by volatilizing the gas and low-melting and boiling point metal impurities in the metallic rhenium under high temperature and high vacuum conditions. Compared with electron beam melting and zone melting technology, high-temperature high-vacuum melting has many advantages such as high process yield and good purification effect, which is of great significance to the development of industrial production of high-purity metallic rhenium.

[0024] The existing high-temperature and high-vacuum melting and purification methods mainly include: melting the billet under vacuum or ammonia atmosphere at a high temperature of 2700 ℃ to 3500 ℃ and high vacuum conditions to remove impurities and obtain molten high-purity metallic rhenium. In this process, a large amount of energy is consumed to heat to reach the melting point of metallic rhenium, resulting in high production costs and high energy consumption. In addition, the process of heating metallic rhenium to a molten state is relatively long, making the purification efficiency low. Continuous high temperature is also likely to cause oxidation and volatilization of some metallic rhenium, resulting in a large loss of raw materials.

[0025] Based on the problems existing in the related art, the present invention proposes an inventive concept: in the process of purifying metallic rhenium, a staged heating strategy is adopted, including two stages of pre-sintering treatment and high-temperature sintering treatment, wherein the pre-sintering stage is carried out at a relatively low temperature and vacuum degree, aiming to preliminarily remove impurities and gases in the metallic rhenium blank, laying a good foundation for the subsequent high-temperature sintering; during the high-temperature sintering treatment, it is further carried out at high temperature and high vacuum degree to further remove impurities such as alkali metals to improve the purity of metallic rhenium. The control of the vacuum degree is also set to be carried out in stages, and combined with the strategy of segmented heating, it is possible to more effectively remove impurities and gases in the metallic rhenium, and obtain high-purity metallic rhenium with at least the same purity as that obtained by existing high-temperature and high-vacuum smelting and purification, but it can effectively reduce energy consumption, and omit the step of heating the metallic rhenium to a molten state, thereby solving many problems caused by the melting treatment of metallic rhenium.

[0026] Based on the above inventive concept, the present invention provides a high-purity metal rhenium high-temperature high-vacuum melting device capable of realizing the above inventive concept, see Figure 1 , the device specifically comprises: Furnace body 1, heating component 3, heat preservation component 4 and vacuum pump 5; A material rack 11 is provided in the furnace body 1, and the material rack 11 is used to place a crucible filled with metal rhenium; The heating component 3 and the heat preservation component 4 are both located in the furnace body 1, wherein the heating component 3 is sleeved outside the material rack 11, and the heat preservation component 4 is sleeved outside the heating component 3; The heating component 3 is configured to heat the metal rhenium in the crucible; The vacuum pump 5 includes a mechanical pump 51 and a molecular pump 52. An interface 115 is provided on one side of the furnace body 1, wherein the mechanical pump 51 is connected to the interface 115, and the molecular pump 52 is connected to an end of the mechanical pump 51 away from the interface 115; The mechanical pump 51 is configured to adjust the vacuum degree inside the furnace body 1 to 10 -1 Pa~10 Pa; the molecular pump 52 is configured to be when the vacuum degree inside the furnace body 1 is 10 -1 When the vacuum degree inside the furnace body 1 is adjusted to 10 -2 Pa~10 -6 Pa; The furnace body 1 is provided with a temperature control structure 2, and the temperature control structure 2 is configured to be -2 Pa~10 -3 Pa, the heating component 3 is controlled to heat the metal rhenium to 900°C-1300°C; and when the vacuum degree in the furnace body 1 is 10 -4Pa~10 -6 Pa, controlling the heating component 3 to heat the metal rhenium to 1800°C-2500°C; The heat preservation component 4 is configured to gather and reflect the heat generated by the heating component 3 to concentrate on the heating component 3 for heating the metal rhenium.

[0027] It should be noted that the furnace body 1 refers to a container for accommodating the heating component 3, the heat-insulating component 4 and the crucible, and has the characteristics of high temperature resistance and corrosion resistance; The material rack 11 in the furnace body 1 is located at the center of the furnace body 1, and the crucible can be placed on the material rack 11 from bottom to top; The cross-sectional shape of the furnace body 1 can be circular, square, diamond, elliptical, etc.; The material of the furnace body 1 can be a high temperature resistant and strong metal such as stainless steel; The material rack 11 has the advantages of stable physical and chemical properties, high temperature resistance, and not easy to volatilize at high temperatures; The metallic rhenium contained in the crucible is in solid form; The heating component 3 refers to a device that provides heat, which may be a heating element such as a resistance wire, an electric heating tube, a tungsten mesh, etc. The shape of the heating component 3 may be cylindrical, conical, columnar, etc.; The heating component 3 is configured to heat the metal rhenium in the crucible, which means that the heating component 3 releases heat in the furnace body 1, and the heat flows in the furnace body 1 and reaches the material rack 11, and the crucible and the metal rhenium in the crucible absorb heat and heat up. Even if the heat absorption efficiency of the metal rhenium and the crucible is different, the metal rhenium is placed in the crucible, so there is a heat transfer process between the metal rhenium and the crucible, so that the temperature of the metal rhenium and the crucible is consistent; The heating component 3 is sleeved outside the material rack 11, as shown in FIG. Figure 1 When the furnace body 1 is placed as shown, the heating component 3 surrounds the material rack 11; the heat preservation component 4 is sleeved outside the heating component 3, which means that the heat preservation component 4 surrounds the heating component 3 and the bottom of the heating component 3 to reduce heat loss and improve heating efficiency; The heat preservation component 4 can be made of a material that is resistant to high temperatures and has good thermal conductivity, such as ceramic fiber, and its shape can be set to be cylindrical or conical to fit closely with the inner wall of the furnace body 1 to maximize the collection and reflection of heat; The heat preservation component 4 is used to gather and reflect the heat generated by the heating component 3, which means that the heat released by the heating component 3 during heating flows in the furnace body 1, mainly in the space surrounded by the heat preservation component 4, and the heat is preserved in the space by the heat preservation component 4. When the heat is dispersed to the heat preservation component 4, the heat preservation component 4 can reflect the heat to the heating component 3; Reflected heat means that when heat radiation (i.e., heat released by the heating component 3) flows from the heating component 3 to the heat-insulating component 4, the heat-insulating component 4 will reflect most of it, causing the heat radiation to flow back to the heating component 3; The vacuum pump 5 is a device for extracting gas from the furnace body 1. The vacuum pump 5 can be controlled by a program control method. By comparing a preset vacuum degree curve with a current vacuum degree signal, the working state of the mechanical pump 51 and the molecular pump 52 is automatically adjusted to maintain the vacuum degree in the furnace body 1. The mechanical pump 51 is a preliminary exhaust device that compresses and exhausts gas by mechanical movement (such as a piston, a vane or a screw, etc.), thereby reducing the pressure in the furnace body 1. In the present invention, the mechanical pump 51 is within a relatively low vacuum range (such as 10 -1 Pa~10 Pa) has a good exhaust effect, and can quickly exhaust the gas in the furnace body 1, laying the foundation for the subsequent high vacuum exhaust process (exhaustion by molecular pump 52); The molecular pump 52 is a high vacuum pump 5 that can further reduce the vacuum degree to a higher vacuum level (10 -2 Pa~10 -6 Pa), which collides and extracts gas molecules through a high-speed rotating rotor (usually with blades or grooves of special shapes), thereby achieving the effect of improving the vacuum degree. In the high-temperature and high-vacuum melting process of metal rhenium, the molecular pump 52 is used to further adjust the vacuum degree inside the furnace body 1 to 10 after the mechanical pump 51 initially evacuates the gas. -2 Pa~10 -3 Pa was pre-sintered and adjusted to 10 -4 Pa~10 -6 Pa conducts high-temperature sintering treatment, coupling a high vacuum environment with a high-temperature environment, which can more effectively remove impurities and gases in the metal rhenium blank, improve the purity of the metal rhenium, and also reduce the oxidation and volatilization of the metal rhenium during the smelting process, reduce losses, and ensure the smelting effect and product quality; The molecular pump 52 is used to replace the traditional diffusion pump, which can shorten the exhaust time in the furnace body 1 and obtain a clean vacuum environment without oil pollution. The temperature control structure 2 refers to a device for controlling the heat release of the heating component 3, which may include a temperature sensor and a controller, etc.; The temperature control structure 2 can adopt a closed-loop control method, monitor the temperature in the furnace body 1 in real time through the temperature sensor, and feed back the temperature signal to the controller; the controller adjusts the heating power of the heating component 3 according to the comparison result between the set temperature curve and the current temperature signal to maintain the constant temperature in the furnace body 1, and achieve a temperature control accuracy of ±1 ℃~±3 ℃; The temperature control structure 2 may also include a temperature controller, a high-temperature thermocouple, a voltage regulator, and the like; wherein the temperature controller may be connected to the heating component 3 to control the heating rate and heating time of the heating component 3; the high-temperature thermocouple may be located near the material rack 11 to detect the temperature of the crucible on the material rack 11 and the metal rhenium in the crucible, and transmit a temperature signal to the temperature controller, the temperature controller is configured to control the heating component 3 in response to the temperature signal, and an infrared thermometer may be used to replace the high-temperature thermocouple during implementation; the voltage regulator is connected to the heating component 3 to accurately adjust the power supply voltage or current of the heating component 3, thereby achieving accurate control of the heating power; in the present invention, the temperature controller may also ensure that the heating component 3 operates at an appropriate power at different stages by adjusting the voltage regulator to avoid overheating or underheating; In one case, when the temperature control structure 2 includes a high-temperature thermocouple or an infrared thermometer, a temperature measurement interface 115 can be opened on the furnace body 1 near the material rack 11 to facilitate accurate temperature measurement.

[0028] In the specific implementation, put the metal rhenium into the crucible, and then place the crucible on the material rack 11. If multiple crucibles are provided, the multiple crucibles need to be placed at intervals; start the mechanical pump 51, and adjust the vacuum degree in the furnace body 1 to 10 -1 Then start the molecular pump 52 to adjust the vacuum degree in the furnace body 1 to 10 -2 Pa~10 -3 Pa, at this time, the temperature control system starts the heating component 3, and the heating component 3 releases heat to heat the crucible and the metal rhenium in the crucible to 900 ℃ ~ 1300 ℃. After the metal rhenium is initially purified at this temperature, the molecular pump 52 is used to adjust the vacuum degree in the furnace body 1 to 10 -4 Pa~10 -6 Pa, the temperature control structure 2 then controls the heating component 3 to heat the crucible and the metal rhenium in the crucible to 1800 ℃ ~ 2500 ℃, so that the metal rhenium is further purified to obtain high-purity metal rhenium. During the purification process, the heat released by the heating component 3 is gathered at the heating component 3 by the insulation component 4, so that the heat is used to heat the crucible and the metal rhenium in the crucible as much as possible. The small amount of heat that contacts the insulation component 4 is reflected by the insulation component 4 to the heating component 3, thereby minimizing heat loss.

[0029] The present invention provides a temperature control structure 2 to accurately control the heating temperature of the heating component 3 to ensure that the metal rhenium is stably purified at different temperatures. The mechanical pump 51 is then used to initially evacuate the interior of the furnace body 1 to quickly reduce the initial atmospheric pressure in the furnace to 10 -1Pa~10 Pa, effectively removing most of the air and water vapor in the furnace, and using gentle heating at low vacuum to avoid the risk of oxidation caused by excessive temperature. Molecular pump 52 further increases the vacuum degree in the furnace to 10 Pa based on the initial vacuum pumping by mechanical pump 51. -2 Pa~10 -6 Pa high vacuum state. As the vacuum degree increases, the heating temperature is gradually increased to ensure that the metal rhenium can remain stable at high temperatures and avoid oxidation and contamination. The high vacuum environment combined with high-temperature refining promotes the decomposition of intermetallic compounds and the removal of impurities, thereby improving the purity of metal rhenium. This is of great significance for the preparation of high-quality, high-performance metal rhenium materials.

[0030] The setting of the heat preservation component 4 enables the heat generated by the heating component 3 to act more concentratedly on the metal rhenium, thereby reducing heat loss, reducing energy consumption during the operation of the device and the loss of metal rhenium. When the purification efficiency of the device is improved and the loss is reduced, the corresponding production cost is also greatly reduced, thereby improving the economic benefits of the process. It should also be noted that through the precise control of the temperature control structure 2 and the vacuum pump 5, the automation of the metal rhenium purification process is achieved, reducing manual intervention.

[0031] In some embodiments, Figure 1 When the furnace body 1 is placed as shown, the upper end of the furnace body 1 can be set as an opening, and a furnace cover is set on the side of the furnace body 1 where the opening is set, and the bottom wall of the furnace cover is in contact with the upper end surface of the furnace body 1; The upper end of the material rack 11 is fixedly connected to the inner wall of the furnace cover on the side facing the furnace body 1 , and the diameter of the opening is set to be larger than the size of the material rack 11 .

[0032] In specific implementation, the furnace cover is moved upward, and the furnace cover drives the material rack 11 to move upward. At this time, the bottom wall of the furnace cover is separated from the upper end surface of the furnace body 1, and the material rack 11 is separated from the furnace body 1 upward along the opening. Then, the crucible containing metal rhenium can be placed on the material rack 11, and then the furnace cover is moved downward, so that the material rack 11 with the crucible placed can enter the furnace body 1 downward along the opening. This makes it easy to place the crucible outside the furnace body 1, avoiding the limitation of the space inside the furnace body 1.

[0033] In some embodiments, see Figure 1 ,like Figure 1 When the furnace body 1 shown is placed, a ball screw lifting device can be provided on the furnace cover; The ball screw lifting device may include a screw, a nut and a ball, the ball is arranged in the nut, the nut is connected to the furnace cover, and the screw is arranged parallel to the material rack 11, that is, the moving direction of the material rack 11 is parallel to the length direction of the screw.

[0034] During specific implementation, the rotation of the lead screw drives the ball to roll in the nut, so that the nut moves upward or downward along the length direction of the lead screw, the nut drives the furnace cover to move, and the furnace cover drives the material rack 11 to move, thereby realizing automatic lifting of the material rack 11, simplifying the operation difficulty and improving production efficiency.

[0035] In some embodiments, a pneumatic baffle valve may be further provided on the connecting pipeline between the interface 115 and the mechanical pump 51 .

[0036] It should be noted that the pneumatic flapper valve refers to a valve that controls the opening and closing of the flapper through a pneumatic actuator, thereby achieving control of the fluid flow in the pipeline.

[0037] The pneumatic baffle valve of the present invention can be freely opened and closed in the pipeline, thereby accurately controlling the gas flow in the furnace body 1.

[0038] In some embodiments, the mechanical pump 51 and the interface 115 may be connected by a vacuum bellows, and the mechanical pump 51 and the molecular pump 52 may be connected by a vacuum bellows.

[0039] It should be noted that the vacuum bellows refers to an axisymmetric tube shell with a corrugated busbar and a certain degree of curvature, also known as a flexible tube or a flexible tube. Its corrugated shape allows the bellows to change in axial length when subjected to force.

[0040] The vacuum bellows provided in the present invention is used as a connecting pipe fitting to connect the mechanical pump 51 and the interface 115, as well as the mechanical pump 51 and the molecular pump 52, to build a complete vacuum system. Its excellent connectivity enables the entire vacuum system to be well sealed, ensuring that the gas inside the furnace body 1 can be effectively extracted to achieve the required low-pressure state. When the vacuum pump 5 is working, due to factors such as equipment vibration and temperature changes, the pipes in the device will undergo slight displacements and deformations. The vacuum bellows can flexibly absorb these displacements, avoid excessive force on the connection, and protect the stability of the device. The vacuum bellows can also absorb and mitigate the vibration and impact force generated when the vacuum pump 5 is in operation, reduce the impact on other parts of the device, extend the life of the equipment, and ensure long-term stable operation of the device.

[0041] In some embodiments, see Figure 1 , the distance between the insulation component 4 and the heating component 3 is 3 mm to 20 mm; The thermal insulation component 4 includes a plurality of thermal insulation layers 41; The spacing between adjacent thermal insulation layers 41 is 0-5 mm.

[0042] It should be noted that if Figure 1When the furnace body 1 is placed as shown, the distance between the heat preservation component 4 and the heating component 3 is: the vertical distance between the heat preservation component 4 and the heating component 3 along the width direction of the furnace body 1; The distance between the heat preservation component 4 and the heating component 3 can be 3 mm, 6 mm, 9 mm, 10 mm, 12 mm, 14 mm, 16 mm, 18 mm, 20 mm; The plurality of insulation layers 41 may be 2 layers, 6 layers, 8 layers, 10 layers, 15 layers, etc.; like Figure 1 When the furnace body 1 is placed as shown, the spacing between adjacent insulation layers 41 is the vertical distance between the outer wall of one insulation layer 41 and the inner wall of another insulation layer 41 along the width direction of the furnace body 1; The spacing between adjacent insulation layers 41 may be 0 mm, 1 mm, 2 mm, 3 mm, 4 mm, or 5 mm.

[0043] In specific implementation, by setting the distance between the heat preservation component 4 and the heating component 3, excessive heat concentration and loss caused by too close distance can be avoided. By setting the heat preservation component 4 to include multiple heat preservation layers 41, heat loss can be more effectively blocked. The multiple heat preservation layers 41 can form a "barrier" for heat transfer, so that more heat is retained around the heating component 3, which helps to improve the stability and efficiency of the purification process. Especially in a high vacuum environment, the heat preservation effect is more significant.

[0044] By setting the spacing between adjacent insulation layers 41, the heat conduction between adjacent insulation layers 41 can be reduced, so that more heat is retained around the heating component 3. At the same time, a certain expansion space can be provided for the insulation layer 41 to avoid damage or deformation of the insulation layer 41 due to thermal expansion at high temperature.

[0045] In some embodiments, see Figure 1 When more than two insulation layers 41 are provided, in one case, the diameters of the plurality of insulation layers 41 are different, wherein the insulation layer 41 with a larger diameter is sleeved on the insulation layer 41 with a smaller diameter, and adjacent insulation layers 41 are closely fitted; In another case, an isolation ring can be set between adjacent insulation layers 41, and the two ends of the isolation ring are respectively connected to the two insulation layers 41, which on the one hand plays a supporting and fixing role; on the other hand, it separates the adjacent insulation layers 41, so that the heat can be more evenly and effectively applied and reflected on the central material rack 11, thereby maintaining the uniformity of the temperature in the furnace and reducing heat loss.

[0046] In some embodiments, when multiple thermal insulation layers 41 are provided, support rods 114 may also be provided, and the support rods 114 are connected to the multiple thermal insulation layers 41 to play a supporting and fixing role.

[0047] In some embodiments, see Figure 1 , the material of the thermal insulation layer 41 is metal rhenium.

[0048] Metal rhenium has the characteristics of high melting point, heat resistance, high temperature resistance and corrosion resistance. It has good heat protection effect, strong heat resistance, long service life, and is not easy to deform. At the same time, it can also avoid impurity contamination caused by high-purity metal rhenium during the preparation process.

[0049] In some embodiments, see Figure 1 , the heating assembly 3 includes a first heating net 31, a second heating net 32 ​​and a third heating net 33; Wherein, the first heating net 31 is set around the material rack 11; The distance between the side of the first heating net 31 facing the material rack 11 and the material rack 11 is 3 mm to 20 mm; the distance between the side of the first heating net 31 facing away from the material rack 11 and the heat preservation component 4 is 3 mm to 20 mm; The material rack 11 is provided with a first end 111 and a second end 112 opposite to each other. The second heating net 32 ​​is fixed to the first end 111 , and the third heating net 33 is fixed to the second end 112 .

[0050] It should be noted that the cross-sectional shape of the first heating net 31 can be circular, square, diamond, etc.; The shapes of the second heating net 32 ​​and the third heating net 33 can be the same as the shape of the first heating net 31, or different from the shape of the first heating net 31, or the shape of one of the heating nets can be the same as the shape of the first heating net 31, and the shape of the other heating net can be different from the shape of the first heating net 31; The materials of the first heating net 31, the second heating net 32 ​​and the third heating net 33 can be selected from metal materials with high temperature resistance, good electrical conductivity, and good corrosion resistance and mechanical strength; such as nickel-chromium alloy, stainless steel, etc.; The first heating net 31, the second heating net 32 ​​and the third heating net 33 may be a mesh structure woven from fine metal wires to ensure that the heat can be evenly distributed; like Figure 1 When the furnace body 1 is placed as shown, the first heating net 31 faces the side of the material rack 11, that is, the inner wall of the first heating net 31, and the side of the first heating net 31 facing away from the material rack 11, that is, the outer wall of the first heating net 31; The size of the second heating net 32 ​​and the third heating net 33 along the width direction of the furnace body 1 is at least the same as the size of the material rack 11 along the width of the furnace body 1, or is larger than the size of the material rack 11 along the width of the furnace body 1; like Figure 1When the furnace body 1 is placed as shown, the first end 111 and the second end 112 arranged opposite to each other on the material rack 11 correspond to the upper end and the lower end of the material rack 11 respectively; wherein the bottom wall of the second heating net 32 ​​is fixed to the first end 111, and the top wall of the third heating net 33 is fixed to the second end 112; In specific implementation, during the purification process, the temperature control structure 2 controls the first heating network 31, the second heating network 32 and the third heating network 33 to start simultaneously, and the heating rate, time, etc. of each heating network are kept synchronized.

[0051] The present invention sets the first heating net 31 to be sleeved around the material rack 11 to ensure that the metal rhenium on the material rack 11 can be heated evenly. At the same time, the distance between the first heating net 31 and the material rack 11 and the distance between the first heating net 31 and the insulation component 4 are controlled within the range of 3 mm to 20 mm to reduce the loss of heat during the transfer process and further improve the uniformity of heating.

[0052] The second heating net 32 ​​and the third heating net 33 are respectively fixed to the first end 111 and the second end 112 of the material rack 11, so that the heating component 3 can provide the same heating intensity as the first heating net 31 in different areas, thereby achieving precise heating of metal rhenium at different positions on the material rack 11 and meeting the specific requirements for temperature distribution during the purification process.

[0053] In some embodiments, see Figure 1 The first heating net 31, the second heating net 32 ​​and the third heating net 33 are made of tungsten.

[0054] In specific implementation, tungsten is a metal with a high melting point (about 3410 ° C) that can maintain stable physical and chemical properties at extremely high temperatures. In the process of purifying metal rhenium in the present invention, a higher temperature needs to be reached to remove impurities, and the heating net made of tungsten can more easily cope with such a high temperature environment to ensure the smooth progress of the purification process. Tungsten is not only resistant to high temperatures, but also has good thermal conductivity. It can quickly convert electrical energy into thermal energy and evenly transfer heat to the metal rhenium on the material rack 11, thereby shortening the purification cycle and improving production efficiency. Tungsten also has good corrosion resistance and can maintain stable performance in the purification environment.

[0055] In some embodiments, see Figure 1 The first heating net 31, the second heating net 32 ​​and the third heating net 33 can all be made of tungsten wire twisted tungsten nets, wherein the main mesh belts can be 4-8. The tungsten net is heated by a three-phase power supply. After power is turned on and heated, the electrical energy is quickly converted into thermal energy, achieving efficient heating and providing a uniform and stable temperature field to meet the requirements of heating power.

[0056] It should be noted that three-phase power supply refers to a system that provides three alternating currents with a phase difference of 120 degrees. Compared with single-phase power supply, three-phase power supply can reduce line losses and improve energy utilization efficiency when transmitting the same power, and has higher stability and reliability.

[0057] In some embodiments, see Figure 1 , the material rack 11 includes at least one storage plate 113 and a support rod 114; The placing plate 113 is sleeved on the supporting rod 114 . The placing plate 113 is vertically fixed to the supporting rod 114 . The placing plate 113 is used to place at least one crucible.

[0058] It should be noted that the cross-sectional shape of the storage plate 113 may be circular, rectangular, oval, etc.; The cross-sectional shape of the support rod 114 can be circular, square, etc.; like Figure 1 When the furnace body 1 is placed as shown, the dimension of the support rod 114 along the length direction of the furnace body 1 is greater than the total dimension of the plurality of placement plates 113 along the length of the furnace body 1; The size of each placement plate 113 along the length direction of the furnace body 1 may be 3 mm to 5 mm; for example, the size of each placement plate 113 along the length direction of the furnace body 1 may be 3 mm, 3.5 mm, 4 mm, 4.5 mm, or 5 mm; like Figure 1 When the furnace body 1 is placed as shown, when the material rack 11 includes more than two placement plates 113, the more than two placement plates 113 are arranged on the support rod 114 at intervals along the length direction of the support rod 114, forming a layered structure from top to bottom on the support rod 114, so that a crucible containing metal rhenium can be placed on each layer of the placement plates 113; The material rack 11 may include one storage plate 113, or may include 2, 4, 8, 10, 15, etc. The number of storage plates 113 included in the material rack 11 may be reasonably set according to the size of the furnace body 1; One crucible, five crucibles, etc. can be placed on one placement plate 113; The fixing method of the storage plate 113 and the support rod 114 can be welding, bolt connection, snap connection, etc.; The material of the storage plate 113 needs to be able to withstand high temperatures and the weight of the materials, and also needs to have good thermal conductivity; for example, stainless steel, aluminum, copper alloy, high temperature resistant ceramics, etc.

[0059] The present invention can adapt to crucibles of different sizes and different material amounts when the device is used by setting the number and position of the placement plates 113 on the material rack 11, thereby improving the versatility and utilization rate of the device. The placement plates 113 are vertically fixed to the support rods 114 to ensure stable support of the crucible during the purification process, and prevent the crucible from tilting or collapsing due to temperature changes or material reactions during the heating process, thereby ensuring the safety and reliability of the purification process.

[0060] In some embodiments, see Figure 1 The storage plate 113 can be made of metal rhenium material to avoid impurity contamination during the high-purity metal rhenium high-temperature and high-vacuum preparation process; Among them, the storage plate 113 can be set to 5-10 layers to increase the processing volume of each furnace and improve production efficiency.

[0061] In some embodiments, the crucible can be made of metal rhenium by welding and has a rectangular or square shape. The bottom of the crucible can be covered with zirconium oxide or aluminum oxide pads to prevent high-purity metal rhenium from sticking to or dissolving the crucible under high temperature conditions.

[0062] In some embodiments, the apparatus may further include a water cooling assembly; In one case, the water cooling assembly may be composed of an all-stainless steel manifold, a water pressure sensor, a main branch stop valve, a water flow monitor, etc.; A water-cooled electrode interface 119 can be provided on the furnace body 1. The furnace body 1 can adopt a double-layer jacket water-cooled structure with a polished surface. The furnace body 1 can be cooled by a water cooling system to keep the surface temperature of the furnace body 1 below 30°C to 50°C.

[0063] It should be noted that the water cooling component refers to a component used to reduce the temperature of the furnace body 1 by circulating water; The all-stainless steel water distribution main pipe refers to a water distribution device made of stainless steel, which is used to evenly distribute cooling water to each water-cooling branch pipe; the water pressure sensor refers to a sensor used to monitor the water pressure in the water-cooling component in real time to ensure that the water-cooling component operates within the normal water pressure range; the main branch pipe stop valve refers to a switch used to control the main inlet and outlet water pipes of the water-cooling component, so as to shut down the water-cooling component or perform maintenance when necessary; the water flow monitor refers to a device used to monitor the water flow state in the water-cooling component, which can be used to detect parameters such as water flow velocity and flow rate to ensure the normal operation of the water-cooling component; The double-layer jacket water-cooling structure refers to a structure in which a water-cooling pipe is embedded in the double-layer jacket of the furnace body 1, and the heat generated on the surface of the furnace body 1 is taken away by water circulation to achieve a cooling effect; the surface polishing treatment refers to a process for smoothing the surface of the furnace body 1, which can improve the aesthetics and corrosion resistance of the surface of the furnace body 1.

[0064] The present invention introduces a water cooling component and adopts a water cooling system composed of a full stainless steel water manifold, a water pressure sensor, a main branch stop valve, a water flow monitor, etc., which can efficiently take away the heat generated on the surface of the furnace body 1 and ensure that the surface temperature of the furnace body 1 is maintained below 30°C~50°C, thereby improving the stability and safety of the system.

[0065] In some embodiments, see Figure 1 A charging port 116 is provided on one side of the furnace body 1, and a charging valve 117 is connected to the charging port 116, and the charging valve 117 is in a normally closed state.

[0066] It should be noted that the inflation valve 117 refers to a key component used to control and adjust the gas filling into the vacuum state of the space, and can be opened or closed as needed to allow or prevent the flow of gas.

[0067] In some embodiments, see Figure 1 In one case, when the charging valve 117 is provided on the furnace body 1 , the exhaust valve 118 is also required to be provided on the furnace body 1 to discharge the inert gas filled into the furnace body 1 .

[0068] When the device provided by the present invention is implemented, the furnace body 1 is in a high vacuum state. In order to smoothly take out the purified high-purity metallic rhenium, after cooling, the charging valve 117 is opened to charge the furnace body 1 with inert gas, and then closed after it is full, so as to balance the atmospheric pressure in the furnace body 1, so that the furnace cover and other devices arranged on the furnace body 1 can be opened smoothly. The inert gas can be argon or nitrogen. After the high-purity metallic rhenium in the furnace body 1 is taken out, the inert gas in the furnace body 1 can be discharged through the venting gate 118.

[0069] The present invention also provides a high-purity metal rhenium high-temperature high-vacuum melting preparation method suitable for the above-mentioned high-purity metal rhenium high-temperature high-vacuum melting device, see Figure 2 , the preparation method comprises: Step S1, putting an appropriate amount of metal rhenium blank into a crucible, and placing the crucible containing the blank on a material rack 11; Step S2: Turn on the mechanical pump 51 to adjust the vacuum degree inside the furnace body 1 to 10 -1 Pa~10 Pa, and then the molecular pump 52 is turned on, and the molecular pump 52 adjusts the vacuum degree inside the furnace body 1 to 10 -2 Pa~10 -3 After Pa, the temperature control structure 2 controls the heating assembly 3 to heat the crucible and the blank in the crucible to 900°C~1300°C, and perform a pre-sintering treatment for 1 h~3 h; Step S3: After the pre-sintering process, the vacuum degree inside the furnace body 1 is adjusted to 10 -4 Pa~10-6 Pa, the temperature control structure 2 controls the heating assembly 3 to heat the crucible and the blank in the crucible to 1800°C~2500°C, perform a high-temperature sintering treatment for 1 h~3 h, and obtain high-purity metallic rhenium after cooling; Wherein, the purity of the high-purity metallic rhenium is greater than 99.99%.

[0070] It should be noted that the metal rhenium used for purification in the present invention is in a solid state. During the pre-sintering treatment and the high-temperature sintering treatment, the metal rhenium remains in a solid state, and the high-purity metal rhenium finally purified is also in a solid state.

[0071] In specific implementation, the mechanical pump 51 and the molecular pump 52 are used in combination to achieve precise control of the vacuum degree in the furnace body 1, provide a good environment for subsequent sintering, and avoid purity reduction caused by factors such as oxidation and pollution. During purification, a pre-sintering treatment is first performed to make the metal rhenium blank initially densified, and then high-temperature sintering is performed under high vacuum to further remove impurities in the blank and improve the quality of the product. The present invention effectively removes impurities in the metal rhenium by coupling the vacuum treatment and high-temperature sintering steps, so that the purity of the final product reaches more than 99.99%, meeting the preparation requirements of high-purity metal rhenium.

[0072] In specific implementation, the pre-sintering treatment can preliminarily remove pores and impurities in the blank, making the blank denser. At the same time, pre-sintering can also reduce thermal stress during high-temperature sintering and prevent the product from cracking due to excessive thermal stress. Sintering at different vacuum levels is to better control oxidation and pollution during the sintering process. At a lower vacuum level, the air and most impurities in the furnace body 1 can be preliminarily removed; at a higher vacuum level, the influence of oxygen and other impurities on the sintering process can be further reduced, which can ensure the purity of the product and avoid the step of melting metal rhenium. Compared with the prior art, the purification temperature is greatly reduced, which effectively reduces unnecessary energy consumption and improves the economic benefits of the high-temperature and high-vacuum smelting and purification process of metal rhenium.

[0073] In the specific implementation, in step S2, the mechanical pump 51 is turned on to adjust the vacuum degree inside the furnace body 1 to 10 - 1 Pa, 1 Pa, 2 Pa, 3 Pa, 4 Pa, 5 Pa, 6 Pa, 7 Pa, 8 Pa, 9 Pa, 10 Pa; In step S2, the temperature control structure 2 controls the heating component 3 to heat the crucible and the blank in the crucible to 900°C, 950°C, 1000°C, 1100°C, 1200°C, and 1300°C, and a pre-sintering treatment can be performed for 1 h, 1.5 h, 2 h, 2.5 h, and 3 h; In step S3, the molecular pump 52 can adjust the vacuum degree inside the furnace body 1 to 10 -4 Pa, 10 -5 Pa, 10 -6 Pa; In step S3, the temperature control structure 2 controls the heating component 3 to heat the crucible and the blank in the crucible to 1800°C, 1900°C, 2000°C, 2100°C, 2200°C, 2300°C, 2400°C, and 2500°C, and a high temperature sintering treatment can be performed for 1 h, 1.5 h, 2 h, 2.5 h, and 3 h; In some embodiments, in S2, the temperature control structure 2 controls the heating rate of the heating component 3 to be 8°C / min-15°C / min.

[0074] In specific implementation, during the pre-sintering stage, controlling the heating rate helps to ensure that the blank is evenly heated during the pre-sintering stage, so that the blank quickly reaches the ideal temperature and insulation time during the pre-sintering stage, thereby effectively removing most of the pores and impurities, reducing the duration of subsequent high-temperature sintering treatment, and thus reducing energy consumption.

[0075] In specific implementation, in S2, the temperature control structure 2 may control the heating component 3 to have a heating rate of 8°C / min, 9°C / min, 10°C / min, 11°C / min, 12°C / min, 13°C / min, 14°C / min, or 15°C / min.

[0076] In some embodiments, in S3, the temperature control structure 2 controls the heating rate of the heating component 3 to be 5°C / min-10°C / min.

[0077] In specific implementation, during the high-temperature sintering stage, a slower heating rate helps ensure that the blank is heated evenly and stably throughout the heating process, avoiding local overheating caused by too fast a heating rate, and reducing the risk of thermal stress concentration and blank cracking. A slower heating rate also helps to promote the gradual closure of pores inside the blank and the uniform growth of grains, and helps to form a dense sintered body to improve the mechanical properties and purity of the final product. Slow heating also helps to reduce the volatilization and redeposition of impurities caused by rapid heating during high-temperature sintering, especially in a high vacuum environment, where slow heating can more effectively remove residual gases and volatile impurities in the blank.

[0078] In specific implementation, in S3, the temperature control structure 2 may control the heating component 3 to have a heating rate of 5°C / min, 6°C / min, 7°C / min, 8°C / min, 9°C / min, or 10°C / min.

[0079] In some embodiments, in S3, the step of cooling includes: The temperature control structure 2 controls the heating component 3 to cool down at a rate of 10°C / min~15°C / min until the temperature in the crucible drops to 800°C~1000°C, and then the temperature control structure 2 and the heating component 3 are closed to allow the crucible and the high-purity metal rhenium in the crucible to naturally cool down to 100°C~300°C.

[0080] In specific implementation, by adjusting the cooling rate, preliminary cooling is first performed to effectively reduce the thermal stress caused by rapid cooling. Thermal stress is one of the main causes of material cracking and performance degradation, especially in metal rhenium after high-temperature sintering. Therefore, this step helps to protect the integrity of the product and avoid cracks or deformation during the cooling process. Rapid cooling may also cause redistribution of impurities inside the metal rhenium. By controlling the cooling rate, this situation can be avoided and the high purity of the final product can be ensured. Then the temperature is naturally cooled without additional energy input and manual operation, which is more conducive to energy conservation and emission reduction. After naturally cooling to a lower temperature (100 ℃~300 ℃), the residual heat and potential danger of the metal rhenium are greatly reduced, reducing the risk of equipment damage caused by high temperature.

[0081] In specific implementation, the temperature control structure 2 can control the heating component 3 to cool down at a rate of 10°C / min, 11°C / min, 12°C / min, 13°C / min, 14°C / min, 15°C / min until the temperature in the crucible drops to 800°C, 850°C, 900°C, 950°C or 1000°C; the crucible and the high-purity metal rhenium in the crucible can be naturally cooled to 100°C, 150°C, 200°C, 250°C, 300°C.

[0082] In order to enable those skilled in the art to more clearly understand the present invention, a high-purity metallic rhenium high-temperature and high-vacuum melting device and a preparation method thereof described in the present invention are now described in detail through the following examples.

[0083] Example 1 See Figure 1 The high-purity metal rhenium high-temperature and high-vacuum melting device shown.

[0084] (1) Cover the bottom of the crucible with zirconium oxide padding and place the metal rhenium blank in the crucible; (2) placing the crucibles containing the metal rhenium blanks on the material rack 11 in order from bottom to top; (3) Start the mechanical pump 51 to perform vacuum treatment on the furnace body 1. When the vacuum degree in the furnace body 1 reaches 10 -1 After Pa, turn on the molecular pump 52 to draw a high vacuum; (4) Set the temperature control curve in the temperature control structure 2. When the vacuum degree reaches 10 -3 After Pa, the three-phase power supply connected to the tungsten mesh is turned on. The tungsten mesh converts electrical energy into thermal energy and releases it into the furnace body 1. The heating rate is set to 15 °C / min, the sintering temperature is set to 1300 °C, and the pre-sintering treatment is carried out. The sintering time is set to 1 h. (5) After the pre-sintering treatment is completed, when the vacuum degree reaches 10 -4 Pa, the temperature starts to rise, the temperature control structure 2 controls the heating rate on the tungsten mesh to be 10 ℃ / min, the sintering temperature is 1800 ℃, and the high-temperature sintering treatment is performed, and the sintering time is set to 3 h; (6) After the vacuum high-temperature sintering treatment is completed, the temperature is lowered. The temperature control structure 2 controls the cooling rate on the tungsten mesh to be 10°C / min. When the temperature of the crucible and the material in the crucible drops to 1000°C, the temperature control structure 2 and the tungsten mesh are closed to allow the crucible and the material in the crucible to cool naturally. When the temperature drops below 300°C, the mechanical pump 51 and the molecular pump 52 are closed to stop vacuuming, and high-purity metallic rhenium with a purity greater than 99.99% is obtained in the crucible.

[0085] Example 2 See Figure 1 The high-purity metal rhenium high-temperature and high-vacuum melting device shown.

[0086] (1) Spread alumina padding on the bottom of the crucible and place the metal rhenium blank in the crucible; (2) placing the crucibles containing the metal rhenium blanks on the material rack 11 in order from bottom to top; (3) Start the mechanical pump 51 to perform vacuum treatment on the furnace body 1. When the vacuum degree in the furnace body 1 reaches 10 Pa, turn on the molecular pump 52 to draw a high vacuum; (4) Set the temperature control curve in the temperature control structure 2. When the vacuum degree reaches 10 -2 After Pa, the three-phase power supply connected to the tungsten mesh is turned on. The tungsten mesh converts electrical energy into thermal energy and releases it into the furnace body 1. The heating rate is set to 8 °C / min, the sintering temperature is set to 900 °C, and the pre-sintering treatment is performed. The sintering time is set to 3 h. (5) After the pre-sintering treatment is completed, when the vacuum degree reaches 10 -6 Pa, the temperature starts to rise, the temperature control structure 2 controls the heating rate on the tungsten mesh to be 10 ℃ / min, the sintering temperature is 2500 ℃, and high-temperature sintering treatment is performed, and the sintering time is set to 1 h; (6) After the vacuum high-temperature sintering treatment is completed, the temperature is lowered. The temperature control structure 2 controls the cooling rate on the tungsten mesh to be 15°C / min. When the temperature of the crucible and the material in the crucible drops to 800°C, the temperature control structure 2 and the tungsten mesh are closed to allow the crucible and the material in the crucible to cool naturally. When the temperature drops below 100°C, the mechanical pump 51 and the molecular pump 52 are closed to stop vacuuming, and high-purity metallic rhenium with a purity greater than 99.99% is obtained in the crucible.

[0087] Example 3 See Figure 1 The high-purity metal rhenium high-temperature and high-vacuum melting device shown.

[0088] (1) Cover the bottom of the crucible with zirconium oxide padding and place the metal rhenium blank in the crucible; (2) placing the crucibles containing the metal rhenium blanks on the material rack 11 in order from bottom to top; (3) Start the mechanical pump 51 to perform vacuum treatment on the furnace body 1. When the vacuum degree in the furnace body 1 reaches 1 Pa, turn on the molecular pump 52 to draw a high vacuum; (4) Set the temperature control curve in the temperature control structure 2. When the vacuum degree reaches 10 -3 After Pa, the three-phase power supply connected to the tungsten mesh is turned on. The tungsten mesh converts electrical energy into thermal energy and releases it into the furnace body 1. The heating rate is set to 10 °C / min, the sintering temperature is set to 1200 °C, and the pre-sintering treatment is performed. The sintering time is set to 2 h. (5) After the pre-sintering treatment is completed, when the vacuum degree reaches 10 -5 Pa, the temperature starts to rise, the temperature control structure 2 controls the heating rate on the tungsten mesh to 8 °C / min, the sintering temperature is 2200 °C, and the high-temperature sintering treatment is performed, and the sintering time is set to 2 h; (6) After the vacuum high-temperature sintering treatment is completed, the temperature is lowered. The temperature control structure 2 controls the cooling rate on the tungsten mesh to be 12 °C / min. When the temperature of the crucible and the material in the crucible drops to 900 °C, the temperature control structure 2 and the tungsten mesh are closed to allow the crucible and the material in the crucible to cool naturally. When the temperature drops below 200 °C, the mechanical pump 51 and the molecular pump 52 are closed to stop vacuuming, and high-purity metallic rhenium with a purity greater than 99.99% is obtained in the crucible.

[0089] In summary, the high-purity metal rhenium high-temperature and high-vacuum melting device and preparation method provided by the present invention, compared with traditional vacuum induction melting equipment, realizes precise control of the melting temperature under ultra-high vacuum conditions, and is simple to operate, and can effectively reduce material loss, reduce production energy consumption, and shorten the process flow.

[0090] The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the various embodiments can be referenced to each other.

[0091] Although the preferred embodiments of the present application have been described, those skilled in the art may make additional changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the embodiments of the present application.

[0092] Finally, it should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or terminal device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or terminal device. In the absence of further restrictions, the elements defined by the sentence "including one..." do not exclude the existence of other identical elements in the process, method, article or terminal device including the elements.

[0093] The above is a detailed introduction to a high-purity metal rhenium high-temperature and high-vacuum melting device and preparation method provided by the present application. Specific examples are used in this article to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the method of the present application and its core idea; at the same time, for general technicians in this field, according to the ideas of the present application, there will be changes in the specific implementation methods and application scopes. In summary, the content of this specification should not be understood as a limitation on the present application.

Claims

1. A high-purity metal rhenium high-temperature high-vacuum melting device, characterized in that: The device comprises: A furnace body (1), a heating component (3), a heat-insulating component (4) and a vacuum pump (5); A material rack (11) is provided in the furnace body (1), and the material rack (11) is used to place a crucible containing metal rhenium; The heating component (3) and the heat-insulating component (4) are both located in the furnace body (1), wherein the heating component (3) is sleeved outside the material rack (11), and the heat-insulating component (4) is sleeved outside the heating component (3); The heating component (3) is configured to heat the metal rhenium in the crucible; The vacuum pump (5) comprises a mechanical pump (51) and a molecular pump (52); an interface (115) is provided on one side of the furnace body (1); the mechanical pump (51) is connected to the interface (115), and the molecular pump (52) is connected to an end of the mechanical pump (51) away from the interface (115); The mechanical pump (51) is configured to adjust the vacuum degree inside the furnace body (1) to 10 -1 Pa~10 Pa; the molecular pump (52) is configured to be able to generate a vacuum when the vacuum degree inside the furnace body (1) is 10 -1 When the vacuum degree inside the furnace body (1) is adjusted to 10 -2 Pa~10 -6 Pa; The furnace body (1) is provided with a temperature control structure (2), and the temperature control structure (2) is configured to, when the vacuum degree in the furnace body (1) is 10 -2 Pa~10 -3 Pa, controlling the heating component (3) to heat the metal rhenium to 900°C to 1300°C; and when the vacuum degree in the furnace body (1) is 10 -4 Pa~10 -6 Pa, controlling the heating component (3) to heat the metal rhenium to 1800° C. to 2500° C.; The heat-insulating component (4) is configured to gather and reflect the heat generated by the heating component (3) so as to concentrate the heat on the heating component (3) for heating the metal rhenium.

2. The high-purity metal rhenium high-temperature and high-vacuum melting device according to claim 1, characterized in that: The distance between the heat preservation component (4) and the heating component (3) is 3 mm to 20 mm; The thermal insulation component (4) comprises a plurality of thermal insulation layers (41); The spacing between adjacent insulation layers is 0-5 mm.

3. The high-purity metal rhenium high-temperature and high-vacuum melting device according to claim 2, characterized in that: The material of the thermal insulation layer (41) is metal rhenium.

4. The high-purity metal rhenium high-temperature and high-vacuum melting device according to claim 1, characterized in that: The heating assembly (3) comprises a first heating net (31), a second heating net (32) and a third heating net (33); Wherein, the first heating net (31) is sleeved around the material rack (11); The distance between the side of the first heating net (31) facing the material rack (11) and the material rack (11) is 3 mm to 20 mm; the distance between the side of the first heating net (31) facing away from the material rack (11) and the thermal insulation component (4) is 3 mm to 20 mm; The material rack (11) is provided with a first end (111) and a second end (112) opposite to each other, the second heating net (32) is fixed to the first end (111), and the third heating net (33) is fixed to the second end (112).

5. The high-purity metal rhenium high-temperature and high-vacuum melting device according to claim 4, characterized in that: The material of the first heating net (31), the second heating net (32) and the third heating net (33) is tungsten.

6. The high-purity metal rhenium high-temperature and high-vacuum melting device according to claim 1, characterized in that: The material rack (11) comprises at least one storage plate (113) and a support rod (114); The placement plate (113) is sleeved on the support rod (114), the placement plate (113) is vertically fixed to the support rod (114), and the placement plate (113) is used to place at least one of the crucibles.

7. A method for preparing high-purity metallic rhenium by high-temperature and high-vacuum smelting, characterized in that: Applicable to the high-purity metal rhenium high-temperature and high-vacuum melting device according to any one of claims 1 to 6, the preparation method comprising: S1. Put an appropriate amount of metal rhenium blank into a crucible, and place the crucible containing the blank on a material rack (11); S2, start the mechanical pump (51) and adjust the vacuum degree inside the furnace body (1) to 10 -1 Pa~10 Pa, and then start the molecular pump (52), which adjusts the vacuum degree inside the furnace body (1) to 10 -2 Pa~10 -3 After Pa, the temperature control structure (2) controls the heating component (3) to heat the crucible and the blank in the crucible to 900°C to 1300°C, and perform a pre-sintering treatment for 1h to 3h; S3, after the pre-sintering treatment, the vacuum degree inside the furnace body (1) is adjusted to 10 -4 Pa~10 -6 Pa, the temperature control structure (2) controls the heating component (3) to heat the crucible and the blank in the crucible to 1800°C to 2500°C, perform a high-temperature sintering treatment for 1 h to 3 h, and obtain high-purity metallic rhenium after cooling; Wherein, the purity of the high-purity metallic rhenium is greater than 99.99%.

8. The high-temperature and high-vacuum smelting method for preparing high-purity metallic rhenium according to claim 7, characterized in that: In S2, the temperature control structure (2) controls the heating rate of the heating component (3) to be 8°C / min to 15°C / min.

9. The high-temperature and high-vacuum smelting method for preparing high-purity metallic rhenium according to claim 7, characterized in that: In S3, the temperature control structure (2) controls the heating rate of the heating component (3) to be 5°C / min to 10°C / min.

10. The high-temperature and high-vacuum melting method for preparing high-purity metallic rhenium according to claim 7, characterized in that: In S3, the step of cooling includes: The temperature control structure (2) controls the heating component (3) to cool down at a rate of 10°C / min to 15°C / min until the temperature in the crucible drops to 800°C to 1000°C, and then the temperature control structure (2) and the heating component (3) are closed to allow the crucible and the high-purity metal rhenium in the crucible to naturally cool down to 100°C to 300°C.

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