A high-purity rhenium high-temperature and high-vacuum melting device and preparation method

Abstract

The present application provides a high-purity rhenium high-temperature and high-vacuum melting device and a preparation method. By improving the structure of the high-purity rhenium high-temperature and high-vacuum melting device, the vacuum degree inside the device can be adjusted separately during the purification process of rhenium metal, and rhenium metal can be heated step by step, thereby effectively reducing the temperature and energy consumption required for melting rhenium metal, greatly improving the process efficiency, and shortening the heating and cooling time. Among them, by setting the sintering temperature and vacuum degree, it also helps to reduce the volatilization and oxidation of rhenium metal, reduce the loss during the purification process, and improve the utilization rate of raw materials. Due to the improvement of process efficiency and the reduction of losses, the production cost is further reduced, thereby improving the economic benefits of the high-temperature and high-vacuum melting and purification process of rhenium metal.

Description

Technical Field

[0001] The present application relates to the technical field of high-purity metal preparation. Specifically, it relates to a high-temperature and high-vacuum melting device for high-purity rhenium metal and a preparation method thereof. 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 thermal shock resistance under high temperature and rapid heating and cooling conditions, and is widely used in industries such as aerospace, petrochemical and electronics. With the continuous development of society and the continuous progress of technology, the purity requirements for rhenium metal are getting higher and higher. Currently, the largest use of high-purity rhenium metal is mainly for the manufacture of single-crystal turbine blades of aeroengines. Trace impurities with low melting and boiling points in rhenium metal are prone to form inclusion cores in high-temperature chemical reactions and become fatigue crack sources. When the control of trace impurity elements is unqualified, harmful phases (such as σ and µ phases) will precipitate, damaging the strength and toughness of the alloy. Therefore, the requirements for trace impurity elements in rhenium metal are extremely strict.

[0003] The purification of rhenium metal generally adopts a combined chemical-physical purification process. Chemical impurity removal is carried out by means such as solvent extraction, ion exchange, recrystallization, high-temperature and high-vacuum melting, electron beam melting, and zone melting. Among them, compared with electron beam melting and zone melting technologies, high-temperature and high-vacuum melting has various advantages such as high process yield and good purification effect, which is of great significance for the industrial production of high-purity rhenium metal.

[0004] However, the existing high-temperature and high-vacuum melting purification usually requires making rhenium metal into a molten state, resulting in problems such as slow process efficiency, large loss, and high cost, which is not conducive to improving the economic benefits of the high-temperature and high-vacuum melting purification process of rhenium metal. Summary of the Invention

[0005] To solve the above problems, the present invention provides a high-temperature and high-vacuum melting device for high-purity rhenium metal and a preparation method thereof. By improving the structure of the high-temperature and high-vacuum melting device for high-purity rhenium metal, the vacuum degree of the device is adjusted step by step during the purification process of rhenium metal, and rhenium metal is heated step by step, thereby effectively reducing the temperature and energy consumption required for melting rhenium metal, greatly improving the process efficiency, and shortening the heating and cooling time. Among them, by setting the sintering temperature and vacuum degree, it also helps to reduce the volatilization and oxidation of rhenium metal, reduce the loss during 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 and high-vacuum melting purification process of rhenium metal.

[0006] In the first aspect, the present invention provides a high-temperature and high-vacuum melting device for high-purity rhenium metal, and the device includes:

[0007] A furnace body (1), a heating component (3), a heat preservation component (4), and a vacuum pump (5);

[0008] A material rack (11) is arranged inside the furnace body (1), and the material rack (11) is used for placing a crucible containing rhenium metal;

[0009] Both the heating component (3) and the heat preservation component (4) are located inside the furnace body (1). Among them, the heating component (3) is sleeved outside the material rack (11), and the heat preservation component (4) is sleeved outside the heating component (3);

[0010] The heating component (3) is configured to heat the rhenium metal in the crucible;

[0011] The vacuum pump (5) includes a mechanical pump (51) and a molecular pump (52). An interface (115) is opened on one side of the furnace body (1). Among them, the mechanical pump (51) is connected to the interface (115), and the molecular pump (52) is connected to one end of the mechanical pump (51) away from the interface (115);

[0012] The mechanical pump (51) is configured to adjust the vacuum degree inside the furnace body (1) to be 10 -1 Pa to 10 Pa; the molecular pump (52) is configured to adjust the vacuum degree inside the furnace body (1) to be 10 -1 Pa to 10 Pa when the vacuum degree inside the furnace body (1) is 10 -2 Pa to 10 -6 Pa;

[0013] A temperature control structure (2) is arranged on the furnace body (1). The temperature control structure (2) is configured to control the heating component (3) to heat the rhenium metal to 900 °C to 1300 °C when the vacuum degree inside the furnace body (1) is 10 -2 Pa to 10 -3 Pa; and when the vacuum degree inside the furnace body (1) is 10 -4 Pa to 10 -6 Pa, control the heating component (3) to heat the rhenium metal to 1800 °C to 2500 °C;

[0014] The heat preservation component (4) is configured to gather and reflect the heat generated by the heating component (3) and concentrate it on the heating component (3) for heating the rhenium metal.

[0015] Optionally, the distance between the heat preservation component (4) and the heating component (3) is 3 mm to 20 mm;

[0016] The thermal insulation assembly (4) includes a plurality of thermal insulation layers (41);

[0017] The distance between adjacent thermal insulation layers is 0 - 5 mm.

[0018] Optionally, the material of the thermal insulation layer (41) is rhenium metal.

[0019] Optionally, the heating assembly (3) includes a first heating mesh (31), a second heating mesh (32), and a third heating mesh (33);

[0020] Among them, the first heating mesh (31) is sleeved around the material rack (11);

[0021] The distance between the side of the first heating mesh (31) facing the material rack (11) and the material rack (11) is 3 mm - 20 mm; the distance between the side of the first heating mesh (31) facing away from the material rack (11) and the thermal insulation assembly (4) is 3 mm - 20 mm;

[0022] The material rack (11) is provided with a first end (111) and a second end (112) oppositely arranged. The second heating mesh (32) is fixed to the first end (111), and the third heating mesh (33) is fixed to the second end (112).

[0023] Optionally, the materials of the first heating mesh (31), the second heating mesh (32), and the third heating mesh (33) are tungsten.

[0024] Optionally, the material rack (11) includes at least one placement plate (113) and a support rod (114);

[0025] The placement plate (113) is sleeved on the support rod (114), the placement plate (113) is perpendicularly fixed to the support rod (114), and the placement plate (113) is used to place at least one of the crucibles.

[0026] In a second aspect, the present invention provides a method for preparing high-purity rhenium metal by high-temperature and high-vacuum melting, which is applicable to the high-purity rhenium metal high-temperature and high-vacuum melting device described in the first aspect above. The preparation method includes:

[0027] S1. Put an appropriate amount of rhenium metal blank into the crucible, and place the crucible containing the blank on the material rack (11);

[0028] S2. Turn on the mechanical pump (51), adjust the vacuum degree inside the furnace body (1) to 10 -1 Pa - 10 Pa, and then turn on the molecular pump (52). The molecular pump (52) adjusts the vacuum degree inside the furnace body (1) to 10 -2Pa to 10 -3 After reaching 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 for 1 h to 3 h of pre-sintering treatment;

[0029] S3. After the pre-sintering treatment, use the molecular pump (52) to adjust the vacuum degree inside the furnace body (1) to 10 -4 Pa to 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 for 1 h to 3 h of high-temperature sintering treatment, and high-purity rhenium metal is obtained after cooling;

[0030] Among them, the purity of the high-purity rhenium metal is greater than 99.99%.

[0031] Optionally, in S2, the temperature control structure (2) controls the heating component (3) to increase the temperature at a rate of 8 °C / min to 15 °C / min.

[0032] Optionally, in S3, the temperature control structure (2) controls the heating component (3) to increase the temperature at a rate of 5 °C / min to 10 °C / min.

[0033] Optionally, in S3, the step of cooling includes:

[0034] The temperature control structure (2) controls the heating component (3) to cool 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 turned off, so that the crucible and the high-purity rhenium metal in the crucible are naturally cooled to 100 °C to 300 °C.

[0035] In summary, the present invention includes at least one of the following beneficial technical effects:

[0036] 1. The present invention provides a high-temperature and high-vacuum melting device for high-purity rhenium metal, which mainly includes: a furnace body, a heating component, a heat preservation component and a vacuum pump. Among them, a temperature control structure is also provided on the furnace body, and the vacuum pump includes a mechanical pump and a molecular pump; during implementation, by controlling the vacuum degree inside the furnace body by the vacuum pump and the heating temperature of the heating component, efficient purification of rhenium metal is achieved. 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 loss of heat 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 inside the furnace body, especially when the vacuum degree inside the furnace body reaches 10 -6At Pa, high-temperature sintering treatment can further remove the residual impurities in rhenium metal to obtain rhenium metal with higher purity; the setting of the vacuum pump also helps to reduce the gas residue in the furnace body, further reducing the oxidation and volatilization of rhenium metal 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 benefit of the process;

[0037] 2. The present invention provides a method for preparing high-purity rhenium metal by high-temperature and high-vacuum melting. Through staged heating treatment (i.e., pre-sintering and high-temperature sintering), and precise control under different vacuum degrees, the purification process of rhenium metal is made more efficient; among them, the pre-sintering stage helps to remove some low-boiling impurities and gases in rhenium metal, 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-sintering stage, high-boiling impurities such as oxides and carbides in solid rhenium metal can be effectively removed, so as to obtain high-purity rhenium metal with a purity greater than 99.99%, avoiding unnecessary energy consumption and waste, reducing the loss of raw materials, and lowering the production cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] 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 in the following description are only some embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0039] Figure 1 Shows a schematic structural diagram of a high-temperature and high-vacuum melting device for high-purity rhenium metal proposed by an embodiment of the present application;

[0040] Figure 2 Shows a flow chart of a method for preparing high-purity rhenium metal by high-temperature and high-vacuum melting proposed by an embodiment of the present application.

[0041] Description of the reference numerals in the drawings:

[0042] 1. Furnace body; 11. Material rack; 111. First end; 112. Second end; 113. Placing plate; 114. Support rod; 115. Interface; 116. Inflation port; 117. Inflation valve; 118. Deflation valve; 119. Water-cooled electrode interface;

[0043] 2. Temperature control structure;

[0044] 3. Heating component; 31. First heating mesh; 32. Second heating mesh; 33. Third heating mesh;

[0045] 4. Heat preservation component; 41. Heat preservation layer;

[0046] 5. Vacuum pump; 51. Mechanical pump; 52. Molecular pump. Detailed implementation manners

[0047] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are some, but not all, of the embodiments of the present application. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in the present application without creative efforts shall fall within the protection scope of the present application.

[0048] In the drawings, sometimes for clarity, the sizes of the constituent elements, the thicknesses of the layers, or the areas may be exaggerated. Therefore, any implementation manner of the present disclosure is not necessarily limited to the dimensions 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 manner of the present disclosure is not limited to the shapes or values shown in the drawings.

[0049] In the related art, rhenium metal has a high melting point, high strength, high density, good plasticity and excellent mechanical stability, and has good creep resistance and heat shock resistance under high temperature and rapid heating and cooling conditions, and is widely used in industries such as aerospace, petrochemical and electronics industries.

[0050] The purification of rhenium metal generally adopts a combined chemical-physical purification process. Chemical impurity removal is carried out by means such as solvent extraction, ion exchange, recrystallization, etc., and then high-purity rhenium powder is obtained through processes such as roasting and reduction, and is purified by means such as high-temperature high-vacuum melting, electron beam melting, and zone melting. Among them, through high-temperature and high-vacuum conditions, gases and low-melting-point metal impurities in rhenium metal are volatilized to obtain high-purity rhenium metal above 5N grade (purity greater than 99.99%). Compared with electron beam melting and zone melting technologies, high-temperature high-vacuum melting has many advantages such as high process yield and good purification effect, and is of great significance for the development of industrial production of high-purity rhenium metal.

[0051] The existing high-temperature high-vacuum melting purification means mainly include: the blank bar is melted under vacuum or ammonia atmosphere at a high temperature of 2700 °C to 3500 °C and high-vacuum conditions to remove impurities and obtain molten high-purity rhenium metal. In this process, a large amount of energy is required to heat to reach the melting point of rhenium metal, resulting in high production costs and large energy consumption. In addition, the process of heating rhenium metal to the molten state is relatively long, resulting in low purification efficiency. The continuous high temperature is also likely to cause partial oxidation and volatilization of rhenium metal, resulting in large losses of raw materials.

[0052] Based on the problems existing in the related art, the present invention proposes an inventive concept: in the process of purifying rhenium metal, a staged heating strategy is adopted, including two stages of pre-sintering treatment and high-temperature sintering treatment. Among them, the pre-sintering stage is carried out at a relatively low temperature and vacuum degree, aiming to initially remove impurities and gases in the rhenium metal blank and lay a good foundation for subsequent high-temperature sintering; during the high-temperature sintering treatment, it is carried out at a high temperature and high vacuum degree to further remove impurities such as alkali metals to improve the purity of rhenium metal. The control of the vacuum degree is also set to be carried out in stages. Combining with the staged heating strategy, it can more effectively remove impurities and gases in rhenium metal and obtain high-purity rhenium metal with at least the same purity as that obtained by existing high-temperature and high-vacuum melting and purification, but can effectively reduce energy consumption and omit the step of heating rhenium metal to the molten state, thus solving many problems generated by the melting treatment of rhenium metal.

[0053] Based on the above inventive concept, the present invention provides a high-temperature and high-vacuum melting device for high-purity rhenium metal that can realize the above inventive concept. See Figure 1 , and the device specifically includes:

[0054] A furnace body 1, a heating component 3, a heat preservation component 4, and a vacuum pump 5;

[0055] A material rack 11 is arranged in the furnace body 1, and the material rack 11 is used for placing a crucible containing rhenium metal;

[0056] Both the heating component 3 and the heat preservation component 4 are located in the furnace body 1. Among them, the heating component 3 is sleeved outside the material rack 11, and the heat preservation component 4 is sleeved outside the heating component 3;

[0057] The heating component 3 is configured to heat the rhenium metal in the crucible;

[0058] The vacuum pump 5 includes a mechanical pump 51 and a molecular pump 52. An interface 115 is opened on one side of the furnace body 1. Among them, the mechanical pump 51 is connected to the interface 115, and the molecular pump 52 is connected to one end of the mechanical pump 51 away from the interface 115;

[0059] 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 adjust the vacuum degree inside the furnace body 1 to 10 -1 Pa~10 Pa when the vacuum degree inside the furnace body 1 is 10 -2 Pa~10 -6 Pa;

[0060] A temperature control structure 2 is arranged on the furnace body 1, and the temperature control structure 2 is configured to when the vacuum degree inside the furnace body 1 is 10-2 Pa to 10 -3 Pa, control the heating component 3 to heat the rhenium metal to 900 °C to 1300 °C; and, when the vacuum degree in the furnace body 1 is 10 -4 Pa to 10 -6 Pa, control the heating component 3 to heat the rhenium metal to 1800 °C to 2500 °C;

[0061] The heat preservation component 4 is configured to concentrate and reflect the heat generated by the heating component 3 and act on the heating component 3 to heat the rhenium metal.

[0062] It should be noted that the furnace body 1 refers to a container for accommodating the heating component 3, the heat preservation component 4 and the crucible, and has the characteristics of high temperature resistance and corrosion resistance;

[0063] The material rack 11 in the furnace body 1 is located at the central position in the furnace body 1, and the crucible can be placed on the material rack 11 from bottom to top;

[0064] The cross-sectional shape of the furnace body 1 can be circular, square, rhombic, elliptical, etc.;

[0065] The material of the furnace body 1 can be metals with high temperature resistance and high strength such as stainless steel;

[0066] The material rack 11 has specific characteristics of stable physical and chemical properties, high temperature resistance, and the advantage of not being easily volatilized at high temperatures;

[0067] The rhenium metal contained in the crucible is in a solid state;

[0068] The heating component 3 refers to a device that provides heat, and can be a heating element such as a resistance wire, an electric heating tube, a tungsten mesh, etc.; the shape of the heating component 3 can be cylindrical, conical, columnar, etc.;

[0069] The heating component 3 is configured to heat the rhenium metal 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 then reaches the material rack 11. Both the crucible and the rhenium metal in the crucible absorb heat and increase in temperature. Even though the heat absorption efficiency of the rhenium metal and the crucible is different, since the rhenium metal is placed in the crucible, there is also a heat transfer process between the rhenium metal and the crucible, so that the temperatures of the rhenium metal and the crucible are kept the same;

[0070] The heating component 3 is sleeved outside the material rack 11, which means that when the furnace body 1 is placed as shown in Figure 1 the heating component 3 surrounds the material rack 11 on all sides; 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 on all sides and at the bottom of the heating component 3 to reduce heat dissipation and improve heating efficiency;

[0071] The heat insulation component 4 can be made of materials with high temperature resistance and good thermal conductivity, such as ceramic fiber, and its shape can be set as a cylindrical or conical shape that closely fits the inner wall of the furnace body 1 to maximize the aggregation and reflection of heat;

[0072] The heat insulation component 4 is used to aggregate 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 insulation component 4. Relying on the heat insulation component 4, the heat is stored in this space. When the heat spreads to the heat insulation component 4, the heat insulation component 4 can reflect the heat back to the heating component 3;

[0073] Reflecting heat means that when the thermal radiation (i.e., the heat released by the heating component 3) flows from the heating component 3 to the heat insulation component 4, the heat insulation component 4 will reflect most of it, causing the thermal radiation to flow back to the heating component 3;

[0074] The vacuum pump 5 is a device used to pump out the gas in the furnace body 1; the control of the vacuum pump 5 can adopt a program control method. By comparing the preset vacuum degree curve with the current vacuum degree signal, the working states of the mechanical pump 51 and the molecular pump 52 are automatically adjusted to maintain the vacuum degree in the furnace body 1;

[0075] Among them, the mechanical pump 51 is a preliminary gas pumping device that compresses and discharges gas through mechanical movement (such as pistons, vanes, or screws) to reduce the pressure in the furnace body 1; in the present invention, the mechanical pump 51 has a good gas pumping effect in the range of relatively low vacuum degrees (such as 10 -1 Pa~10 Pa), and can quickly pump out the gas in the furnace body 1, laying a foundation for the subsequent high-vacuum gas pumping process (molecular pump 52 gas pumping);

[0076] The molecular pump 52 is a high-vacuum pump 5 that can further reduce the vacuum degree to reach a higher vacuum level (10 -2 Pa~10 -6 Pa). It collides with and pumps out gas molecules through a high-speed rotating rotor (usually with special-shaped blades or channels) to achieve the effect of increasing the vacuum degree. In the present invention, during the high-temperature and high-vacuum melting process of rhenium metal, after the mechanical pump 51 preliminarily pumps out the gas, the molecular pump 52 is used to further adjust the vacuum degree inside the furnace body 1 to 10 -2 Pa~10 -3 Pa for pre-sintering treatment, and adjusted to 10 -4 Pa~10 -6 Pa for high-temperature sintering treatment. Coupling the high-vacuum environment with the high-temperature environment can more effectively remove impurities and gas in the rhenium metal blank, improve the purity of rhenium metal, reduce oxidation and volatilization of rhenium metal during the melting process, reduce losses, and ensure the melting effect and product quality;

[0077] The use of a molecular pump 52 to replace the traditional diffusion pump can shorten the evacuation time in the furnace body 1 and obtain a clean vacuum environment without oil pollution;

[0078] The temperature control structure 2 refers to a device for controlling the heat released by the heating component 3, which may include a temperature sensor, a controller, and so on;

[0079] The temperature control structure 2 can adopt a closed-loop control method, in which the temperature in the furnace body 1 is monitored in real time through a temperature sensor, and the temperature signal is fed back 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 a constant temperature in the furnace body 1 and achieve a temperature control accuracy of ±1 °C to ±3 °C;

[0080] The temperature control structure 2 may further include a temperature controller, a high-temperature thermocouple, a voltage regulator, and so on; among them, the temperature controller can be connected to the heating component 3 to control the heating rate, heating time, etc. of the heating component 3; the high-temperature thermocouple can be located near the material rack 11 to detect the temperature of the crucible on the material rack 11 and the rhenium metal in the crucible and transmit the temperature signal to the temperature controller, and the temperature controller is configured to control the heating component 3 in response to the temperature signal. In practice, an infrared thermometer can also be used to replace the high-temperature thermocouple; the voltage regulator is connected to the heating component 3 to accurately adjust the supply voltage or current of the heating component 3, thereby achieving precise control of the heating power; in the present invention, the temperature controller can also ensure that the heating component 3 operates at an appropriate power in different stages by adjusting the voltage regulator, avoiding overheating or insufficiency;

[0081] 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.

[0082] In specific implementation, put rhenium metal into the crucible, and then place the crucible on the material rack 11. If multiple crucibles are set, the multiple crucibles need to be placed at intervals; start the mechanical pump 51 to adjust the vacuum degree in the furnace body 1 to 10 -1 Pa to 10 Pa; then start the molecular pump 52 to adjust the vacuum degree in the furnace body 1 to 10 -2 Pa to 10 -3 Pa. At this time, the temperature control system controls the start of the heating component 3, and the heating component 3 releases heat to heat the crucible and the rhenium metal in the crucible to 900 °C to 1300 °C. After the rhenium metal is preliminarily purified at this temperature, then use the molecular pump 52 to adjust the vacuum degree in the furnace body 1 to 10 -4 Pa to 10 -6Pa, 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.

[0083] 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 -1 Pa~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.

[0084] 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.

[0085] 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;

[0086] 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 .

[0087] 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.

[0088] 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;

[0089] 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.

[0090] 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.

[0091] In some embodiments, a pneumatic baffle valve may be further provided on the connecting pipeline between the interface 115 and the mechanical pump 51 .

[0092] 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.

[0093] 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.

[0094] 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.

[0095] 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.

[0096] The vacuum bellows provided in the present invention are used as connecting pipe fittings to connect the mechanical pump 51 with the interface 115 and the mechanical pump 51 with the molecular pump 52, thus constructing 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 evacuated to achieve the required low-pressure state. When the vacuum pump 5 is operating, due to factors such as equipment vibration and temperature change, the pipes in the device will undergo minor displacements and deformations. The vacuum bellows can flexibly absorb these displacements, avoid excessive stress at the connection points, protect the stability of the device, absorb and mitigate the vibrations and impact forces generated during the operation of the vacuum pump 5, reduce the impact on other components of the device, extend the service life of the equipment, and ensure the long-term stable operation of the device.

[0097] In some embodiments, referring to Figure 1 , the distance between the heat insulation component 4 and the heating component 3 is 3 mm to 20 mm;

[0098] The heat insulation component 4 includes a plurality of heat insulation layers 41;

[0099] The distance between adjacent heat insulation layers 41 is 0 - 5 mm.

[0100] It should be noted that when the furnace body 1 is placed as shown in Figure 1 , the distance between the heat insulation component 4 and the heating component 3 is: the vertical distance between the heat insulation component 4 and the heating component 3 in the width direction of the furnace body 1;

[0101] The distance between the heat insulation 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;

[0102] The plurality of heat insulation layers 41 can be 2 layers, 6 layers, 8 layers, 10 layers, 15 layers, etc.;

[0103] As Figure 1 shown when the furnace body 1 is placed, the distance between adjacent heat insulation layers 41 is the vertical distance between the outer wall of one heat insulation layer 41 and the inner wall of another heat insulation layer 41 in the width direction of the furnace body 1;

[0104] The distance between adjacent heat insulation layers 41 can be 0 mm, 1 mm, 2 mm, 3 mm, 4 mm, 5 mm.

[0105] In specific implementation, by setting the distance between the heat preservation component 4 and the heating component 3, the excessive concentration and loss of heat caused by too close a distance can be avoided. By setting the heat preservation component 4 to include multiple heat preservation layers 41, the heat dissipation can be blocked more effectively. 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.

[0106] And by setting the distance between adjacent heat preservation layers 41, the heat conduction between adjacent heat preservation 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 heat preservation layer 41 to avoid damage or deformation of the heat preservation layer 41 caused by thermal expansion at high temperatures.

[0107] In some embodiments, referring to Figure 1 , when two or more heat preservation layers 41 are set, in one case, the diameters of the multiple heat preservation layers 41 are different. Among them, the heat preservation layer 41 with a larger diameter is sleeved on the heat preservation layer 41 with a smaller diameter, and the adjacent heat preservation layers 41 are closely attached to each other;

[0108] In another case, a separation ring can be set between adjacent heat preservation layers 41. The two ends of the separation ring are respectively connected to the two heat preservation layers 41. On the one hand, it plays a role of support and fixation; on the other hand, it separates the adjacent heat preservation layers 41, so that the heat can act and be reflected more evenly and effectively on the central material rack 11, maintaining the uniform consistency of the temperature in the furnace and reducing heat loss.

[0109] In some embodiments, when multiple heat preservation layers 41 are set, a support rod 114 can also be set. The support rod 114 is connected to the multiple heat preservation layers 41 to play a role of support and fixation.

[0110] In some embodiments, referring to Figure 1 , the material of the heat preservation layer 41 is rhenium metal.

[0111] Rhenium metal has characteristics such as high melting point, heat resistance, high temperature resistance and corrosion resistance. It has good heat prevention effect, strong heat resistance, long service life, and is not easy to deform. At the same time, it can also avoid impurity pollution brought by high-purity rhenium metal during the preparation process.

[0112] In some embodiments, referring to Figure 1 , the heating component 3 includes a first heating mesh 31, a second heating mesh 32 and a third heating mesh 33;

[0113] Among them, the first heating mesh 31 is sleeved around the material rack 11;

[0114] The distance between one side of the first heating grid 31 facing the material rack 11 and the material rack 11 is 3 mm to 20 mm; the distance between the other side of the first heating grid 31 facing away from the material rack 11 and the heat preservation component 4 is 3 mm to 20 mm;

[0115] On the material rack 11, a first end 111 and a second end 112 are oppositely arranged, the second heating grid 32 is fixed to the first end 111, and the third heating grid 33 is fixed to the second end 112.

[0116] It should be noted that the cross-sectional shape of the first heating grid 31 can be circular, square, diamond, etc.

[0117] The shapes of the second heating grid 32 and the third heating grid 33 can be the same as that of the first heating grid 31, can also be different from that of the first heating grid 31, or one of the heating grids can have the same shape as the first heating grid 31 and the other can have a different shape from the first heating grid 31;

[0118] The materials of the first heating grid 31, the second heating grid 32 and the third heating grid 33 can be selected from metal materials with high temperature resistance, good electrical conductivity, and also require good corrosion resistance and mechanical strength; such as nickel-chromium alloy, stainless steel, etc.;

[0119] The first heating grid 31, the second heating grid 32 and the third heating grid 33 can be a mesh structure woven by thin metal wires to ensure uniform heat.

[0120] Such as Figure 1 When the furnace body 1 shown is placed, the side of the first heating grid 31 facing the material rack 11 is the inner wall of the first heating grid 31, and the side of the first heating grid 31 facing away from the material rack 11 is the outer wall of the first heating grid 31;

[0121] The dimensions of the second heating grid 32 and the third heating grid 33 in the width direction of the furnace body 1 are at least the same as the dimensions of the material rack 11 in the width of the furnace body 1, or greater than the dimensions of the material rack 11 in the width of the furnace body 1;

[0122] Such as Figure 1 When the furnace body 1 shown is placed, the first end 111 and the second end 112 oppositely arranged on the material rack 11 respectively correspond to the upper end and the lower end of the material rack 11; among them, the bottom wall of the second heating grid 32 is fixed to the first end 111, and the top wall of the third heating grid 33 is fixed to the second end 112;

[0123] During specific implementation, during the purification process, the temperature control structure 2 controls the first heating grid 31, the second heating grid 32 and the third heating grid 33 to start simultaneously, and the heating rate, time, etc. of each heating grid are kept synchronous.

[0124] In the present invention, the first heating mesh 31 is sleeved around the material rack 11 to ensure that the rhenium metal on the material rack 11 can be heated evenly. At the same time, the distance between the first heating mesh 31 and the material rack 11 and the distance between the first heating mesh 31 and the heat preservation component 4 are both controlled within the range of 3 mm to 20 mm to reduce the loss of heat during the transfer process and further improve the heating uniformity.

[0125] The second heating mesh 32 and the third heating mesh 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 mesh 31 in different regions, realizing precise heating of the rhenium metal at different positions on the material rack 11 and meeting the specific requirements for temperature distribution during the purification process.

[0126] In some embodiments, refer to Figure 1 , the materials of the first heating mesh 31, the second heating mesh 32 and the third heating mesh 33 are tungsten.

[0127] Specifically, tungsten is a metal with a high melting point (about 3410 °C) and can maintain stable physical and chemical properties at extremely high temperatures. During the process of purifying rhenium metal in the present invention, a relatively high temperature is required to remove impurities, and the heating mesh made of tungsten can more easily cope with such a high-temperature environment to ensure the smooth progress of the purification process. Tungsten not only has high temperature resistance but also has good thermal conductivity, can quickly convert electrical energy into heat energy, and evenly transfer the heat to the rhenium metal 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.

[0128] In some embodiments, refer to Figure 1 , the first heating mesh 31, the second heating mesh 32 and the third heating mesh 33 can all adopt tungsten wire braided tungsten mesh, and among them, the main mesh belt can be 4 - 8 strips. Using a three-phase power supply to heat the tungsten mesh, after being energized and heated, the electrical energy can be quickly converted into heat energy to achieve efficient heating and provide a uniform and stable temperature field to meet the requirements of the heating power.

[0129] It should be noted that a three-phase power supply refers to a system that provides three alternating currents with a phase difference of 120 degrees. Compared with a single-phase power supply, a three-phase power supply can reduce line losses, improve energy utilization efficiency, and has higher stability and reliability when transmitting the same power.

[0130] In some embodiments, refer to Figure 1 , the material rack 11 includes at least one placement plate 113 and a support rod 114;

[0131] The placing plate 113 is sleeved on the support rod 114, and the placing plate 113 is vertically fixed to the support rod 114. The placing plate 113 is used to place at least one of the crucibles.

[0132] It should be noted that the cross-sectional shape of the placing plate 113 can be circular, rectangular, oval, etc.

[0133] The cross-sectional shape of the support rod 114 can be circular, square, etc.

[0134] Such as Figure 1 When the furnace body 1 is placed as shown, the dimension of the support rod 114 in the length direction of the furnace body 1 is greater than the total dimension of the plurality of placing plates 113 in the length of the furnace body 1.

[0135] The dimension of each placing plate 113 in the length direction of the furnace body 1 can be 3 mm to 5 mm; for example, the dimension of each placing plate 113 in the length of the furnace body 1 can be 3 mm, 3.5 mm, 4 mm, 4.5 mm, 5 mm.

[0136] Such as Figure 1 When the furnace body 1 is placed as shown, when the material rack 11 includes more than two placing plates 113, the more than two placing plates 113 are arranged at intervals in the length direction of the support rod 114 on the support rod 114, forming a layered structure from top to bottom on the support rod 114, so as to facilitate placing crucibles containing rhenium metal on each layer of the placing plate 113.

[0137] The material rack 11 can include one placing plate 113, or can include 2, 4, 8, 10, 15, etc.; the number of placing plates 113 included in the material rack 11 can be reasonably set according to the size of the furnace body 1.

[0138] One placing plate 113 can place one crucible, five crucibles, etc.

[0139] The fixing method of the placing plate 113 and the support rod 114 can be welding, bolt connection, snap connection, etc.

[0140] The material of the placing plate 113 needs to be able to withstand high temperatures and the weight of the material, and at the same time also needs to have good thermal conductivity; such as stainless steel, aluminum, copper alloy, high-temperature resistant ceramics, etc.

[0141] By setting the number and position of the placing plates 113 on the material rack 11 in the present invention, the device can adapt to crucibles of different scales and different amounts of materials during use, thereby improving the versatility and utilization rate of the device. The placing plate 113 is vertically fixed to the support rod 114 to ensure stable support of the crucible during the purification process, preventing the crucible from tilting or collapsing due to temperature changes or material reactions during heating, thereby ensuring the safety and reliability of the purification process.

[0142] In some embodiments, referring to Figure 1 , the storage plate 113 can be made of rhenium metal to avoid impurity contamination during the high-temperature and high-vacuum preparation process of high-purity rhenium metal;

[0143] Among them, the storage plate 113 can be set to 5 - 10 layers to increase the processing volume per furnace and improve production efficiency.

[0144] In some embodiments, the crucible can be made of rhenium metal by welding, and its shape can be rectangular or square. The bottom of the crucible can be fully covered with zirconia or alumina padding to avoid adhesion or eutectic melting between high-purity rhenium metal and the crucible under high-temperature conditions.

[0145] In some embodiments, the device can further include a water-cooling component;

[0146] In one case, the water-cooling component can be composed of a fully stainless-steel water distribution main pipe, a water pressure sensor, a main branch pipe stop valve, a water flow monitor, etc.;

[0147] A water-cooling electrode interface 119 can be opened on the furnace body 1. The furnace body 1 can adopt a double-layer jacket water-cooling structure with a polished surface. The furnace body 1 is cooled through the water-cooling system to keep the surface temperature of the furnace body 1 below 30 °C - 50 °C.

[0148] It should be noted that the water-cooling component refers to a component used to reduce the temperature of the furnace body 1 through water circulation;

[0149] The fully stainless-steel water distribution main pipe refers to a water distribution device made of stainless-steel material, 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 total inlet and outlet pipes of the water-cooling component so as to close the water-cooling component or perform maintenance when needed; 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 rate and flow volume to ensure the normal operation of the water-cooling component;

[0150] The double-layer jacket water-cooling structure refers to a structure in which the water-cooling pipes are embedded in the double-layer jacket of the furnace body 1, and the heat generated on the surface of the furnace body 1 is carried away through water circulation to achieve the cooling effect; the surface polishing treatment refers to a process of smoothing the surface of the furnace body 1, which can improve the aesthetic degree and corrosion resistance of the surface of the furnace body 1.

[0151] By introducing a water-cooling component, the present invention adopts a water-cooling system composed of a fully stainless-steel water distribution main pipe, a water pressure sensor, a main branch pipe stop valve, a water flow monitor, etc., which can efficiently take away the heat generated on the surface of the furnace body 1, ensuring that the surface temperature of the furnace body 1 is maintained below 30 °C to 50 °C, thereby improving the stability and safety of the system.

[0152] In some embodiments, referring to Figure 1 , an inflation port 116 is provided on one side of the furnace body 1, and an inflation valve 117 is connected to the inflation port 116. The inflation valve 117 is in a normally closed state.

[0153] It should be noted that the inflation valve 117 refers to a key component used to control and regulate the gas filling into a space in a vacuum state, which can be opened or closed as needed to allow or block the flow of gas.

[0154] In some embodiments, referring to Figure 1 , in one case, when the inflation valve 117 is provided on the furnace body 1, a deflation valve 118 also needs to be provided on the furnace body 1 to discharge the inert gas filled into the furnace body 1.

[0155] When the device provided by the present invention is implemented, the inside of the furnace body 1 is in a high-vacuum state. In order to smoothly take out the purified high-purity rhenium metal, after cooling, the inflation valve 117 is opened to fill the furnace body 1 with inert gas, and then closed after filling to balance the atmospheric pressure inside the furnace body 1, so that devices such as the furnace cover provided on the furnace body 1 can be smoothly opened. Among them, the inert gas can be argon or nitrogen. After taking out the high-purity rhenium metal inside the furnace body 1, the inert gas inside the furnace body 1 can be discharged through the deflation valve 118 again.

[0156] The present invention also provides a method for preparing high-purity rhenium metal by high-temperature and high-vacuum melting suitable for the above-mentioned high-purity rhenium metal high-temperature and high-vacuum melting device. Referring to Figure 2 , the preparation method includes:

[0157] Step S1: Put an appropriate amount of rhenium metal blank into the crucible, and place the crucible containing the blank on the material rack 11;

[0158] Step S2: Start the mechanical pump 51, adjust the vacuum degree inside the furnace body 1 to 10 -1 Pa to 10 Pa, and then start the molecular pump 52. After the molecular pump 52 adjusts the vacuum degree inside the furnace body 1 to 10 -2 Pa to 10 -3 Pa, the temperature control structure 2 controls the heating component 3 to heat the crucible and the blank inside the crucible to 900 °C to 1300 °C for 1 h to 3 h of pre-sintering treatment;

[0159] Step S3: After the pre-sintering treatment, use the molecular pump 52 to adjust the vacuum degree inside the furnace body 1 to 10 -4 Pa~10 -6 Pa, and the temperature control structure 2 controls the heating component 3 to heat the crucible and the blank inside the crucible to 1800 °C~2500 °C for 1 h~3 h of high-temperature sintering treatment. After cooling, high-purity rhenium metal is obtained;

[0160] Among them, the purity of the high-purity rhenium metal is greater than 99.99%.

[0161] It should be noted that the rhenium metal used for purification in the present invention is in a solid state. During the pre-sintering treatment and high-temperature sintering treatment, the rhenium metal remains in a solid state, and the finally purified high-purity rhenium metal is also in a solid state.

[0162] During specific implementation, through the combined use of the mechanical pump 51 and the molecular pump 52, precise control of the vacuum degree inside the furnace body 1 is achieved, providing a good environment for subsequent sintering and avoiding a decrease in purity caused by factors such as oxidation and pollution. During purification, first, a pre-sintering treatment is carried out to preliminarily densify the rhenium metal blank, and then high-temperature sintering is carried out under a high vacuum degree to further remove impurities in the blank and improve the quality of the product. By coupling the vacuum treatment and high-temperature sintering steps, the present invention effectively removes impurities in the rhenium metal, making the purity of the final product reach more than 99.99%, meeting the preparation requirements of high-purity rhenium metal.

[0163] During specific implementation, the pre-sintering treatment can initially remove pores and impurities in the blank, making the blank more dense. At the same time, the pre-sintering can also reduce the thermal stress during the high-temperature sintering process and avoid cracking of the product due to excessive thermal stress. Sintering at different vacuum degrees is to better control oxidation and pollution during the sintering process. At a lower vacuum degree, the air and most impurities inside the furnace body 1 can already be initially removed; while at a higher vacuum degree, the influence of oxygen and other impurities on the sintering process can be further reduced, which can not only ensure the purity of the product but also avoid the step of melting rhenium metal. Compared with the prior art, the purification temperature is greatly reduced, effectively reducing unnecessary energy consumption and improving the economic benefits of the high-temperature and high-vacuum melting and purification process of rhenium metal.

[0164] During specific implementation, in step S2, turn on the mechanical pump 51, and the vacuum degree inside the furnace body 1 can be adjusted to 10 - 1 Pa, 1 Pa, 2 Pa, 3 Pa, 4 Pa, 5 Pa, 6 Pa, 7 Pa, 8 Pa, 9 Pa, 10 Pa;

[0165] 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, 1300 °C, and pre-sintering treatment can be carried out for 1 h, 1.5 h, 2 h, 2.5 h, 3 h;

[0166] 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;

[0167] 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, 2500 °C, and high-temperature sintering treatment can be carried out for 1 h, 1.5 h, 2 h, 2.5 h, 3 h;

[0168] In some embodiments, 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.

[0169] Specifically, in the pre-sintering stage, by controlling the heating rate, it helps to ensure that the blank can be uniformly heated in the pre-sintering stage, enables the blank to quickly reach the ideal temperature and holding time in the pre-sintering stage, thereby effectively removing most of the pores and impurities, reducing the duration of the subsequent high-temperature sintering treatment, and thus reducing energy consumption.

[0170] Specifically, in S2, the temperature control structure 2 can control the heating rate of the heating component 3 to be 8 °C / min, 9 °C / min, 10 °C / min, 11 °C / min, 12 °C / min, 13 °C / min, 14 °C / min, 15 °C / min.

[0171] In some embodiments, 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.

[0172] In specific implementation, during the high-temperature sintering stage, a slower heating rate helps ensure that the blank is heated uniformly and stably throughout the heating process, avoiding local overheating caused by too rapid heating, reducing the risk of thermal stress concentration and blank cracking. A slower heating rate also helps promote the gradual closure of pores inside the blank and the uniform growth of grains, contributing to the formation of a dense sintered body to improve the mechanical properties and purity of the final product. Slow heating also helps reduce the phenomenon of impurity volatilization and redeposition generated during rapid heating in the high-temperature sintering process. Especially in a high-vacuum environment, slow heating can more effectively remove residual gases and volatile impurities in the blank.

[0173] In specific implementation, in S3, the temperature control structure 2 can control the heating rate of the heating component 3 to be 5 °C / min, 6 °C / min, 7 °C / min, 8 °C / min, 9 °C / min, 10 °C / min.

[0174] In some embodiments, in S3, the step of cooling includes:

[0175] The temperature control structure 2 controls the heating component 3 to cool 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 turned off, allowing the crucible and the high-purity rhenium metal inside the crucible to cool naturally to 100 °C to 300 °C.

[0176] In specific implementation, by adjusting the cooling rate, preliminary cooling is first carried out to effectively reduce the thermal stress generated by rapid cooling. Thermal stress is one of the main reasons for material cracking and performance degradation, especially more significant in rhenium metal after high-temperature sintering. Therefore, this step helps protect the integrity of the product and avoid cracks or deformation during the cooling process. Rapid cooling may also cause the redistribution of impurities inside the rhenium metal. By controlling the cooling rate, this situation can be avoided to ensure the high purity of the final product. Then, natural cooling is carried out, which requires no additional energy input and manual operation, and is more conducive to energy conservation and emission reduction. After natural cooling to a lower temperature (100 °C to 300 °C), the residual heat and potential hazards of rhenium metal are greatly reduced, reducing the risk of equipment damage caused by high temperature.

[0177] In specific implementation, the temperature control structure 2 can control the heating component 3 to cool 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 rhenium metal inside the crucible can cool naturally to 100 °C, 150 °C, 200 °C, 250 °C, 300 °C.

[0178] To enable those skilled in the art to understand the present invention more clearly, a high-purity metallic rhenium high-temperature and high-vacuum melting device and a preparation method thereof described in the present invention will be described in detail through the following embodiments.

[0179] Example 1

[0180] Refer to the high-purity metallic rhenium high-temperature and high-vacuum melting device shown as Figure 1 shown.

[0181] (1) Fully cover the bottom of the crucible with zirconia padding and place the metallic rhenium blank in the crucible;

[0182] (2) Place the crucible containing the metallic rhenium blank on the material rack 11 in the order from bottom to top;

[0183] (3) Start the mechanical pump 51 to conduct vacuum treatment on the furnace body 1. When the vacuum degree in the furnace body 1 reaches 10 -1 Pa, open the molecular pump 52 to pump high vacuum;

[0184] (4) Set the temperature control curve in the temperature control structure 2. When the vacuum degree reaches 10 -3 Pa, turn on the three-phase power supply connected to the tungsten mesh. The tungsten mesh converts electrical energy into heat energy and releases it into the furnace body 1. Set the heating rate to 15 °C / min, the sintering temperature to 1300 °C, conduct pre-sintering treatment, and set the sintering time to 1 h;

[0185] (5) After the pre-sintering treatment is completed, when the vacuum degree reaches 10 -4 Pa, start heating. The temperature control structure 2 controls the heating rate on the tungsten mesh to be 10 °C / min, the sintering temperature to be 1800 °C, conduct high-temperature sintering treatment, and set the sintering time to 3 h;

[0186] (6) After the vacuum high-temperature sintering treatment is completed, cool down. 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 materials in the crucible drops to 1000 °C, turn off the temperature control structure 2 and the tungsten mesh, and let the crucible and the materials in the crucible cool down naturally. When the temperature drops below 300 °C, turn off the mechanical pump 51 and the molecular pump 52, stop pumping vacuum, and obtain high-purity metallic rhenium with a purity greater than 99.99% in the crucible.

[0187] Example 2

[0188] Refer to the high-purity metallic rhenium high-temperature and high-vacuum melting device shown as Figure 1 shown.

[0189] (1) Fully cover the bottom of the crucible with alumina padding and place the metallic rhenium blank in the crucible;

[0190] (2) Place the crucible containing the rhenium metal blank on the material rack 11 in the order from bottom to top;

[0191] (3) Start the mechanical pump 51 to conduct 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 pump high vacuum;

[0192] (4) Set the temperature control curve in the temperature control structure 2. When the vacuum degree reaches 10 -2 Pa, turn on the three-phase power supply connected to the tungsten mesh. The tungsten mesh converts electrical energy into heat energy and releases it into the furnace body 1. Set the heating rate to 8 °C / min, set the sintering temperature to 900 °C, conduct pre-sintering treatment, and set the sintering time to 3 h;

[0193] (5) After the pre-sintering treatment is completed, when the vacuum degree reaches 10 -6 Pa, start heating. The temperature control structure 2 controls the heating rate on the tungsten mesh to be 10 °C / min, the sintering temperature is 2500 °C, conduct high-temperature sintering treatment, and set the sintering time to 1 h;

[0194] (6) After the vacuum high-temperature sintering treatment is completed, cool down. 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 materials in the crucible drops to 800 °C, turn off the temperature control structure 2 and the tungsten mesh, and let the crucible and the materials in the crucible cool down naturally. When the temperature drops below 100 °C, turn off the mechanical pump 51 and the molecular pump 52, stop pumping vacuum, and obtain high-purity rhenium metal with a purity greater than 99.99% in the crucible.

[0195] Example 3

[0196] Refer to the Figure 1 high-temperature and high-vacuum melting device for high-purity rhenium metal shown.

[0197] (1) Fully cover the bottom of the crucible with zirconia padding, and place the rhenium metal blank in the crucible;

[0198] (2) Place the crucible containing the rhenium metal blank on the material rack 11 in the order from bottom to top;

[0199] (3) Start the mechanical pump 51 to conduct 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 pump high vacuum;

[0200] (4) Set the temperature control curve in the temperature control structure 2. When the vacuum degree reaches 10 -3 Pa, turn on the three-phase power supply connected to the tungsten mesh. The tungsten mesh converts electrical energy into heat energy and releases it into the furnace body 1. Set the heating rate to 10 °C / min, set the sintering temperature to 1200 °C, conduct pre-sintering treatment, and set the sintering time to 2 h;

[0201] 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 be 8 °C / min, the sintering temperature is 2200 °C, and the high-temperature sintering treatment is carried out. The sintering time is set to 2 h;

[0202] After the vacuum high-temperature sintering treatment is completed, the temperature is decreased. 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 materials in the crucible is decreased to 900 °C, the temperature control structure 2 and the tungsten mesh are turned off, and the crucible and the materials in the crucible are allowed to cool naturally. When the temperature is decreased to below 200 °C, the mechanical pump 51 and the molecular pump 52 are turned off, and the vacuum pumping is stopped. High-purity rhenium metal with a purity greater than 99.99% is obtained in the crucible.

[0203] In summary, a high-purity rhenium metal high-temperature and high-vacuum melting device and preparation method provided by the present invention, compared with the traditional vacuum induction melting equipment, realizes the precise control of the melting temperature under ultra-high vacuum conditions, and has simple operation, can effectively reduce material loss, reduce production energy consumption, and shorten the process flow.

[0204] Each embodiment in this specification is described in a progressive manner. Each embodiment focuses on the differences from other embodiments. The same or similar parts among the embodiments can be referred to each other.

[0205] Although the preferred embodiments of the embodiments of the present application have been described, those skilled in the art can make additional changes and modifications once they know the basic creative concepts. Therefore, the appended claims are intended to be interpreted to include the preferred embodiments and all changes and modifications falling within the scope of the embodiments of the present application.

[0206] Finally, it should also be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the term "comprising", "including" or any other variant thereof is intended to cover non-exclusive inclusion, so that a process, method, article or terminal device including a series of elements not only includes those elements, but also includes other elements not expressly listed, or also includes elements inherent to such process, method, article or terminal device. Without further limitation, an element defined by the statement "including a..." does not exclude the existence of additional identical elements in the process, method, article or terminal device including the said element.

[0207] The above has introduced in detail a high-purity metallic rhenium high-temperature and high-vacuum melting device and a preparation method provided by the present application. Specific examples are used in this article to elaborate on the principle and implementation manner of the present application. The description of the above embodiments is only used to help understand the method and its core idea of the present application; at the same time, for those of ordinary skill in the art, according to the idea of the present application, there will be changes in the specific implementation manner and application scope. In summary, the content of this specification should not be construed as a limitation to the present application.

Claims

1. A high-purity rhenium high-temperature and 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 be 10 -1 Pa~10 Pa; the molecular pump (52) is configured to adjust the vacuum degree inside the furnace body (1) to be 10 -1 Pa~10 Pa when the vacuum degree inside the furnace body (1) is 10 -2 Pa~10 -6 Pa; A temperature control structure (2) is provided on the furnace body (1), and the temperature control structure (2) is configured to control the heating assembly (3) to heat the rhenium metal to 900 °C to 1300 °C when the vacuum degree in the furnace body (1) is 10 -2 Pa to 10 -3 Pa; and, when the vacuum degree in the furnace body (1) is 10 -4 Pa to 10 -6 Pa, control the heating assembly (3) to heat the rhenium metal 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 rhenium high-temperature and high-vacuum melting device according to claim 1, wherein 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 rhenium high-temperature and high-vacuum melting device according to claim 2, wherein, The material of the thermal insulation layer (41) is metal rhenium.

4. The high-purity rhenium high-temperature and high-vacuum melting device according to claim 1, wherein, 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 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 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 rhenium metal by high-temperature and high-vacuum melting, 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. Turn on the mechanical pump (51) and adjust the vacuum degree inside the furnace body (1) to 10 -1 Pa~10 Pa. Then turn on the molecular pump (52). The molecular pump (52) adjusts the vacuum degree inside the furnace body (1) to 10 -2 Pa~10 -3 Pa. After that, the temperature control structure (2) controls the heating component (3) to heat the crucible and the blank inside the crucible to 900 °C~1300 °C for 1h~3 h of pre-sintering treatment; S3. After the pre-sintering treatment, use the molecular pump (52) to adjust the vacuum degree inside the furnace body (1) to 10 -4 Pa to 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 for 1 h to 3 h of high-temperature sintering treatment, and high-purity rhenium metal is obtained after cooling; Wherein, the purity of the high-purity metallic rhenium is greater than 99.99%.

8. The method for preparing high-purity rhenium metal by high-temperature and high-vacuum melting according to claim 7, characterized in that, In the step 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 method for preparing high-purity rhenium metal by high-temperature and high-vacuum melting according to claim 7, characterized in that, In the step 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 method for preparing high-purity rhenium metal by high-temperature and high-vacuum melting according to claim 7, wherein, In S3, the step of cooling down 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 turned off, so that the crucible and the high-purity rhenium metal in the crucible naturally cool down to 100 °C to 300 °C.

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