An apparatus and method for preparing a high utilization rate ingot of a niobium-silicon based alloy

Abstract

The application relates to an equipment and method for preparing a high-utilization-rate ingot of a niobium-silicon-based alloy, and relates to the field of alloy preparation. The application is used for solving the problems of low utilization rate, uneven composition and excessive impurity content in the preparation of the existing niobium-silicon-based alloy ingot. The application controls the solidification speed of the niobium-silicon-based alloy ingot in the solidification process through the cooperation of a cooling system and an induction coil, increases the contact area of raw materials and heat sources by uniformly paving the raw materials on a water-cooled crucible, and intervenes in the impurities in the metal liquid under the action of a decontamination system. The ingot former can ensure that the niobium-silicon-based alloy metal liquid in the ingot is cooled at an extremely slow speed in the solidification process, so that the solute in the metal liquid is fully diffused, and the composition uniformity of the niobium-silicon-based alloy ingot is improved. The addition of the solid refining agent improves the purity of the ingot and reduces the inclusion content in the niobium-silicon-based alloy ingot, so that the utilization rate of the ingot is improved. The application is used for the preparation of alloys.

Description

TECHNICAL FIELD

[0001] The present application relates to a kind of high-temperature alloy ingot solidification equipment and method, specifically to a kind of equipment and method for preparing niobium silicon base alloy high utilization rate ingot, belong to alloy preparation technical field. BACKGROUND

[0002] With the development of aviation industry, the thrust-to-weight ratio and thermal efficiency of aircraft are significantly improved, which means higher requirements for the temperature resistance of aircraft gas turbine engine hot section components. Niobium silicon base alloy can withstand working temperature above 1200 DEG C, so it is considered as the candidate material of next generation of aircraft engine turbine blade. Ingot metallurgy, as a method commonly used in industrial production and experimental test to prepare niobium silicon alloy ingot, has many advantages such as simple operation, so it is widely used.

[0003] But in prior art, the niobium silicon base alloy ingot prepared generally has the problems of low utilization rate, uneven composition and excessive impurity content, which will greatly increase the preparation cost, cause raw material waste, and at the same time affect the service life or the accuracy of experiment. The reasons for the above problems in the existing equipment are as follows: 1) lack of filling control during ingot solidification process; 2) large temperature gradient during ingot solidification process, and the solidification process greatly deviates from the equilibrium solidification state; 3) uneven heating of raw materials during smelting process, and small contact area with heat source; 4) lack of device for improving the purity of ingot in the equipment.

[0004] In summary, the preparation of existing niobium silicon base alloy ingot has the problems of low utilization rate, uneven composition and excessive impurity content. SUMMARY

[0005] The present application aims to solve the problems of low utilization rate, uneven composition and excessive impurity content in the preparation of existing niobium silicon base alloy ingot. And a kind of equipment and method for preparing niobium silicon base alloy high utilization rate ingot is provided.

[0006] The technical scheme of the present application is: a device for preparing high-utilization-rate ingot of niobium-silicon-based alloy comprises an air extraction control assembly, a water cooling circulation system, a decontamination system, a furnace body, an ingot former and a water-cooled crucible body; the air extraction control assembly is installed outside the furnace body and extends into the furnace body, and extracts high-concentration oxygen in the furnace body to prevent the niobium-silicon-based alloy raw material from reacting with oxygen during smelting; the water cooling circulation system comprises a cooling system, a copper base, an induction coil and an induction coil power supply; the water-cooled crucible body is located at the lower part of the furnace body and is connected with the copper base; the niobium-silicon-based alloy raw material is uniformly laid on the water-cooled crucible body; the induction coil is sleeved on the water-cooled crucible body and is connected with the induction coil power supply located outside the furnace body; the induction coil serves as a heat source to heat the niobium-silicon-based alloy raw material; the cooling system is installed on the water-cooled crucible body; the reaction speed of the niobium-silicon-based alloy raw material is adjusted through the induction coil and the cooling system; the ingot former is vertically installed on the upper part of one side of the niobium-silicon-based alloy raw material; the decontamination system is installed outside the furnace body and is connected with the upper part of the ingot former to remove oxidized impurities in the niobium-silicon-based alloy liquid; and the upper end bottom surface of the ingot former is chamfered at two corners.

[0007] Further, the air extraction control assembly comprises an air storage tank, an air extraction device, an air charging valve and an air extraction mechanism controller; the air extraction device extends into the furnace body through a pipeline; the air extraction mechanism controller is installed on the pipeline; and the air storage tank is connected with the pipeline through the air charging valve.

[0008] Further, the air extraction control assembly further comprises a gas delivery pipe; one end of the gas delivery pipe is connected with the pipeline extending into the furnace body; the other end of the gas delivery pipe is upwardly bent, and the gas outlet of the gas delivery pipe faces downward; and a space is left between the gas outlet end of the gas delivery pipe and the upper end surface of the niobium-silicon-based alloy raw material.

[0009] Preferably, the space between the gas outlet end of the gas delivery pipe and the upper end surface of the niobium-silicon-based alloy raw material is 8 cm.

[0010] Further, the cooling system comprises a water inlet plug, a water outlet plug, a water inlet pipe, a water outlet pipe, a water inlet plug plate and a water outlet plug plate; the water inlet plug plate, the water inlet pipe and the water inlet plug are sequentially connected and then extend into the water-cooled crucible body; and the water outlet plug plate, the water outlet pipe and the water outlet plug are sequentially connected and then extend into the water-cooled crucible body.

[0011] Further, it further comprises a heat preservation coil and a heat preservation coil controller; the heat preservation coil is sleeved on the ingot former; and the heat preservation coil is connected with the heat preservation coil controller.

[0012] Further, the impurity removing system comprises a screen, a conveying pipe, a gas transmission pipe, a gas exhaust pipe, a sealing baffle, a connector, a push rod, a sealing ring, a solid refining agent, a sealing baffle and a gas exhaust collecting tank, the connector is installed on the upper part of the ingot former, the screen is installed on the upper end face of the ingot former, one end of the conveying pipe is covered on the screen, the other end of the conveying pipe is connected with the upper part of the gas exhaust collecting tank, the upper part of the gas exhaust collecting tank is horizontally provided with a sealing baffle, the lower part of the push rod extends downward through the sealing ring, and the solid refining agent is installed in the cavity formed between the conveying pipe and the lower end face of the push rod; one end of the gas transmission pipe is connected with the upper end of the ingot former through the gas exhaust pipe, the other end of the gas transmission pipe is connected with the gas exhaust collecting tank, the lower part of the gas exhaust collecting tank is provided with a plurality of sealing baffles, and the outer side of the lower part of the gas exhaust collecting tank is provided with a gas outlet.

[0013] Preferably, the solid refining agent is ZnCl2.

[0014] The application further provides a preparation method of the equipment for preparing the high-utilization ingot of the niobium-silicon-based alloy.

[0015] Step one: inspection;

[0016] Step one: check whether the connector is connected normally, and adjust in time if loosening occurs;

[0017] Step two: check whether the water circulation of the water cooling circulation system is normal, and adjust if not normal;

[0018] Step three: check whether the pressure indication on the furnace body is normal;

[0019] Step two: lay the niobium-silicon-based alloy raw material;

[0020] Place the niobium-silicon-based alloy raw material in the water-cooled crucible, and uniformly lay it during placement to ensure that the contact surface between the niobium-silicon-based alloy raw material and the water-cooled crucible is large enough; after the above actions are completed, close the furnace door on the furnace body;

[0021] Step three: perform vacuumizing treatment on the equipment interior;

[0022] Step three: open the air exhaust mechanism controller while paying attention to the pressure indication, immediately close the air exhaust mechanism controller when the vacuum degree in the furnace body is 0.1 MPa, open the gas filling valve at the same time, make the inert gas argon fill into the furnace body, and pay attention to the pressure indication again, and keep the vacuum degree in the furnace body at 0.03 MPa;

[0023] Step four: heat the niobium-silicon-based alloy raw material to melting;

[0024] Turn on the induction coil power supply, and observe the niobium-silicon-based alloy raw material through the observation window on the furnace body, and wait for the niobium-silicon-based alloy raw material to completely melt before proceeding to the next step;

[0025] Step five: observe the liquid level in the ingot former 35;

[0026] Open the gas filling valve again, and continuously fill the inert gas argon into the furnace body, and observe whether the liquid level in the ingot former continuously rises slowly through the observation window, and if there is no rise or the rising speed is too fast, adjust the gas filling valve in time; at the same time, open button 1 on the heat preservation coil controller to ensure the normal flow of the niobium-silicon-based alloy liquid metal;

[0027] Step six: slow solidification of the niobium-silicon-based alloy liquid metal;

[0028] When the liquid level in the ingot former is 2.5 cm away from the upper end surface of the connector, adjust the gas filling valve again to ensure that the liquid level height does not change; at the same time, close button 1 on the heat preservation coil controller and open button 2 on the heat preservation coil controller to slow down the solidification of the niobium-silicon-based alloy liquid metal in the ingot former;

[0029] Step seven: push the solid refining agent into the ingot former by operating the push rod;

[0030] Step eight: observe the solidification of the niobium-silicon-based alloy liquid metal through the observation window, and after the niobium-silicon-based alloy liquid metal is completely solidified, sequentially close button 2 on the heat preservation coil controller, the induction coil power supply and the gas filling valve;

[0031] Step nine: after the niobium-silicon-based alloy is cooled, open the furnace door, remove the connector, separate the impurity removal system and the ingot former, and then take out the niobium-silicon-based alloy high-utilization ingot.

[0032] Preferably, the composition of the niobium-silicon-based alloy raw material is Nb-16Si-20Ti alloy.

[0033] Compared with the prior art, the present application has the following effects:

[0034] The present application controls the solidification speed of the niobium-silicon-based alloy ingot during the solidification process through the cooperation of the induction heating and cooling system, increases the contact area of the raw material and the heat source and the impurity intervention measures, designs a smooth ingot forming process and a unique ingot shape, and effectively solves the problems of low utilization rate, uneven composition and excessive impurities of the niobium-silicon-based alloy ingot with a new equipment structure, which is helpful to promote the further application and development of the niobium-silicon-based alloy in the field of aero-engine.

[0035] The gas control system of the present invention controls the flow of argon during equipment operation. This system has three functions: 1) It acts as a protective gas to expel oxygen from the furnace, preventing the niobium-silicon alloy raw material from reacting with oxygen during the smelting process; 2) It acts as a gas flux to expel hydrogen from the niobium-silicon alloy molten metal, improving the purity of the ingot; and 3) It controls the furnace pressure to slowly press the niobium-silicon alloy molten metal into the ingot former, resulting in a dense ingot with a smooth surface. However, due to limitations in the existing equipment structure, the protective gas used only helps expel oxygen from the furnace and does not improve the quality of the resulting ingot.

[0036] 2. The entire upper surface of the water-cooled crucible designed in the present invention can be used as a heat source to heat the niobium-silicon alloy feedstock thereon, greatly increasing the contact area between the niobium-silicon alloy feedstock and the heat source (specifically, the niobium-silicon alloy feedstock 16 is evenly placed on the upper surface to maximize the contact area between the niobium-silicon alloy feedstock 16 and the heat source). This allows the niobium-silicon alloy feedstock to be heated more evenly during the smelting process, further improving the compositional uniformity and utilization rate of the resulting ingot. In contrast, ingots obtained using existing techniques often suffer from uneven heating, resulting in localized unmelted elements, significantly reducing the ingot's utilization rate.

[0037] 3. The present invention combines induction heating with a crucible water-cooling system, so that during the solidification process, the ingot first contacts the surface of the water-cooled copper crucible to produce quenching, resulting in a large number of fine grains. Simultaneously, due to the uniform induction heating, the fine grains obtained have no distinct growth direction (i.e., there are no temperature conditions for columnar crystal growth), thereby preventing the growth of columnar crystals and ensuring the uniformity of the microstructure of each part of the niobium-silicon-based alloy ingot. This significantly improves the microstructure uniformity and density of the resulting ingot, thereby increasing the utilization rate of the ingot. In contrast, ingots obtained using existing technologies typically have three distinct grain zones: a surface fine-grained zone, a columnar crystal zone, and a central equiaxed crystal zone. During the use of the ingot, the fine-grained zone produced by rapid cooling is usually discarded, significantly reducing the utilization rate of the ingot.

[0038] 4. The ingot former provided by the present invention ensures that the niobium-silicon alloy liquid metal within it cools at an extremely slow rate during solidification, allowing sufficient diffusion of solutes within the liquid metal, thereby improving the compositional uniformity of the niobium-silicon alloy ingot. In contrast, in existing technologies, the ingot cools at an extremely high rate during solidification, resulting in inadequate atomic diffusion and poor compositional uniformity in the resulting ingot, leading to low utilization rates.

[0039] 5、The application further improves the purity of the ingot, reduces the inclusion content in the ingot, and improves the utilization rate of the ingot. In the prior art, due to the limitations of the equipment structure design and the types of refining agents, the ingot is rarely optimized by adding solid refining agents during the generation process, so it has a high inclusion content and low purity. BRIEF DESCRIPTION OF DRAWINGS

[0040] Figure 1 is a front view of the equipment for preparing the high-utilization ingot of the niobium-silicon-based alloy;

[0041] Figure 2 is a top view of the equipment for preparing the high-utilization ingot of the niobium-silicon-based alloy;

[0042] Figure 3 is a structural schematic diagram of the ingot former and the impurity removal system;

[0043] Figure 4 is an edge microstructure diagram of the niobium-silicon-based alloy ingot prepared by the application;

[0044] Figure 5 is an edge microstructure diagram of the niobium-silicon-based alloy ingot prepared by the prior art;

[0045] Figure 6 is an organization diagram of the niobium-silicon-based alloy ingot prepared by the prior art, in which the metal elements are not completely melted;

[0046] Figure 7 is a mechanical property comparison diagram of the left side, the middle and the right side of the niobium-silicon-based alloy ingot prepared by the application;

[0047] Figure 8 is a mechanical property comparison diagram of the left side, the middle and the right side of the niobium-silicon-based alloy ingot prepared by the prior art. DETAILED DESCRIPTION

[0048] The technical solution of the application is not limited to the following specific embodiments, and any reasonable combination of the specific embodiments is also included.

[0049] Specific embodiment one: combination Figures 1 to 2The embodiment includes a gas extraction control assembly, a water cooling circulation system, a system for removing impurities, a furnace body 21, an ingot forming device 35 and a water-cooled crucible body 5. The gas extraction control assembly is installed outside the furnace body 21 and extends into the furnace body 21, and extracts high-concentration oxygen in the furnace body 21 to prevent the niobium-silicon-based alloy raw material 16 from reacting with oxygen during the melting process. The water cooling circulation system includes a cooling system, a copper base 12, an induction coil 13 and an induction coil power supply 14. The water-cooled crucible body 5 is located at the lower part of the furnace body 21 and is connected with the copper base 12. The niobium-silicon-based alloy raw material 16 is uniformly laid on the water-cooled crucible body 5. The induction coil 13 is sleeved on the water-cooled crucible body 5 and is connected with the induction coil power supply 14 located outside the furnace body 21. The induction coil 13 serves as a heat source to heat the niobium-silicon-based alloy raw material 16. The cooling system is installed on the water-cooled crucible body 5. The reaction speed of the niobium-silicon-based alloy raw material 16 is adjusted by the induction coil 13 and the cooling system. The ingot forming device 35 is vertically installed on the upper part of one side of the niobium-silicon-based alloy raw material 16. The system for removing impurities is installed outside the furnace body 21 and is connected with the upper part of the ingot forming device 35 to remove oxidized impurities in the niobium-silicon-based alloy liquid. The upper end of the ingot forming device 35 is subjected to a sharpness-removing treatment.

[0050] Specific implementation method two: combined with Figure 1 and Figure 2 The gas extraction control assembly of the embodiment includes a gas tank 4, a gas extraction device 1, a gas filling valve 3 and a gas extraction mechanism controller 2. The gas extraction device 1 extends into the furnace body 21 through a pipeline. The gas extraction mechanism controller 2 is installed on the pipeline. The gas tank 4 is connected with the pipeline through the gas filling valve 3. The other components and connection relationships are the same as those in the specific implementation method one.

[0051] The gas extraction device 1 in the embodiment extends into the furnace body 21 through a pipeline and communicates with the furnace body 21. The gas extraction mechanism controller 2 is located on the right side of the gas extraction device 1 and controls the gas extraction operation of the equipment during the operation of the equipment. The purpose is to extract the gas containing high-concentration oxygen in the furnace body to prevent the niobium-silicon-based alloy raw material 16 from reacting with oxygen during the melting process. The gas filling valve 3 is located on the gas tank 4 and is connected in series with the pipeline and is located below the pipeline. The gas filling valve 3 controls the gas filling operation during the operation of the equipment. The type of the gas filled is argon. The gas filling valve 3 needs to be adjusted multiple times during the operation of the equipment to control the gas pressure in the furnace body 21. The change of the gas pressure in the furnace body 21 is used to control the process of inputting the niobium-silicon-based alloy liquid into the ingot forming device 35. The gas conveying pipe 15 is located 8 cm above the niobium-silicon-based alloy raw material 16. The argon uniformly acts on the surface of the niobium-silicon-based alloy raw material 16 through the gas conveying pipe 15, and simultaneously changes the gas pressure in the entire furnace body 21.

[0052] Specific implementation method three: combined with Figure 1In this embodiment, the argon gas control assembly further comprises a gas delivery pipe 15, one end of which is connected to a pipe extending into the furnace body 21, and the other end of which is bent upwards with the gas outlet facing downwards, and the end of the gas outlet of the gas delivery pipe 15 is spaced apart from the upper end surface of the niobium-silicon based alloy raw material 16. In this way, the argon gas valve 3 controls the argon gas in the gas tank 4 to fill the inside of the furnace body 21, and the argon gas, as a protective gas, can expel oxygen during the filling process, preventing the niobium-silicon based alloy raw material 16 from being oxidized and contaminated. At the same time, since the gas delivery pipe 15 is located directly above the water-cooled crucible body 5 and the upper end surface of the water-cooled crucible body 5 is flat, the argon gas can not only act as a protective gas but also dissolve into the niobium-silicon based alloy liquid as a gas flux, expelling hydrogen in the niobium-silicon based alloy liquid and improving the purity of the niobium-silicon based alloy ingot. In addition, the argon gas valve 3 can be adjusted multiple times during the operation of the equipment, allowing the niobium-silicon based alloy liquid to be slowly and smoothly filled into the ingot former 35, which ensures the compactness of the structure of the niobium-silicon based alloy ingot and the smoothness of its surface. The other components and connection relationships are the same as those in the first or second embodiment.

[0053] Specific embodiment four: combination Figure 1 In this embodiment, the spacing between the end of the gas outlet of the gas delivery pipe 15 and the upper end surface of the niobium-silicon based alloy raw material 16 is 8 cm. The other components and connection relationships are the same as those in any one of the first to third embodiments.

[0054] Specific embodiment five: combination Figure 1 In this embodiment, the cooling system comprises a water inlet pipe 6, a water outlet pipe 7, a water inlet pipe 10, a water outlet pipe 11, a water inlet plate 8 and a water outlet plate 9; the water inlet plate 8, the water inlet pipe 10 and the water inlet pipe 6 are connected in sequence and extend into the water-cooled crucible body 5, and the water outlet plate 9, the water outlet pipe 11 and the water outlet pipe 7 are connected in sequence and extend into the water-cooled crucible body 5. The other components and connection relationships are the same as those in any one of the first to fourth embodiments.

[0055] The upper parts of the water inlet pipe 6 and the water outlet pipe 7 in this embodiment are connected to the water inlet plate 8 and the water outlet plate 9; both the water inlet pipe 6 and the water outlet pipe 7 are vertically installed in the water-cooled crucible body 5. During the operation of the equipment, the above-mentioned water cooling system needs to be turned on to prevent the equipment from being damaged due to overheating. The water-cooled crucible body 5 is located at the lower part of the furnace body 21 and is connected to the copper base 12 in an up-down manner, and the niobium-silicon based alloy raw material 16 is evenly placed on its upper surface, which aims to maximize the contact area between the niobium-silicon based alloy raw material 16 and the heat source, which will be beneficial to the uniform heating of the niobium-silicon based alloy raw material 16, thereby promoting the uniformity of the composition of the niobium-silicon based alloy ingot. The induction coil 13 is located around the water-cooled crucible body 5 and is operated by the induction coil power supply 14, which acts as a heat source to heat the niobium-silicon based alloy raw material 16 during the operation of the equipment.

[0056] The induction coil 13 in the embodiment cooperates with the water cooling circulation system to adjust the cooling speed of the niobium-silicon based alloy raw material 16 during solidification, ensuring the uniformity of the microstructure of the obtained ingot, improving the microstructure uniformity and compactness of the obtained ingot, and reducing the removal of parts during use of the niobium-silicon based alloy ingot.

[0057] Specific embodiment six: in combination with Figure 1 and Figure 3 This embodiment is described, and the embodiment further includes a heat preservation coil 19 and a heat preservation coil controller 20. The heat preservation coil 19 is sleeved on the ingot former 35, and the heat preservation coil 19 is connected with the heat preservation coil controller 20. The other components and connection relationships are the same as any one of the specific embodiments one to five.

[0058] The ingot former 35 in the embodiment is the final forming area of the niobium-silicon based alloy ingot during operation of the equipment. The heat preservation coil 19 is installed on the ingot former 35, and the purpose is to slow down the cooling speed of the niobium-silicon based alloy ingot, so that the niobium-silicon based alloy ingot can approach equilibrium solidification. The upper part of the ingot former 35 is the last solidification area of the niobium-silicon based alloy ingot, which increases the contact area of the ingot former 35 and the niobium-silicon based alloy liquid with a unique cuboid structure (four bottom corners of the cuboid are cut off), prevents the niobium-silicon based alloy liquid from not being able to be timely feeding during solidification, and further improves the quality and utilization rate of the obtained niobium-silicon based alloy ingot.

[0059] The heat preservation coil 19 in the embodiment is controlled by the heat preservation coil controller 20. The button 1 of the heat preservation coil controller 20 controls the lower part of the ingot former 35, which ensures good flowability of the niobium-silicon based alloy liquid during operation of the equipment. The button 2 of the heat preservation coil controller 20 controls the upper part of the ingot former 35, which ensures that the niobium-silicon based alloy liquid has a gentle cooling speed during operation of the equipment, so that the atoms in the niobium-silicon based alloy liquid can fully diffuse, thereby improving the composition uniformity and utilization rate of the niobium-silicon based alloy ingot.

[0060] Specific embodiment seven: in combination with Figure 1 and Figure 3In this embodiment, the impurity removal system comprises a screen 29, a conveying pipe 31, a gas transmission pipe 32, a gas discharge pipe 33, a sealing partition 34, a connector 36, a push rod 24, a sealing ring 25, a solid refining agent 23, the sealing partition 34 and an exhaust gas collection tank 26. The connector 36 is installed on the upper part of the ingot former 35, the screen 29 is installed on the upper end surface of the ingot former 35, one end of the conveying pipe 31 is covered on the screen 29, the other end of the conveying pipe 31 is connected with the upper part of the exhaust gas collection tank 26, the upper part of the exhaust gas collection tank 26 is horizontally provided with a sealing partition 34, the lower part of the push rod 24 extends downward after passing through the sealing ring 25, and the solid refining agent 23 is installed in the cavity formed between the conveying pipe 31 and the lower end surface of the push rod 24. One end of the gas transmission pipe 32 is connected with the upper end of the ingot former 35 through the gas discharge pipe 33, the other end of the gas transmission pipe 32 is connected with the exhaust gas collection tank 26, the lower part of the exhaust gas collection tank 26 is installed with a plurality of sealing partitions 34, and the lower part of the exhaust gas collection tank 26 is provided with a gas outlet 22.

[0061] In this embodiment, the screen 29 is located at the end of the conveying pipe 31, which performs the screening operation on the solid refining agent 23 during the operation of the equipment, and excludes the solid refining agent 23 with large particle volume, so that the solid refining agent 23 with small volume passes through the screen 29 to play a role at the bottom of the niobium-silicon-based alloy liquid. The solid refining agent 23 is conveyed inwardly through the push rod 24, and the sealing ring 25 is installed on both sides of the push rod 24 for sealing. The push rod 24 needs to be slowly pushed into during use to prevent the solid refining agent 23 from being blocked due to excessive pushing force. The impurity gas 26 generated in the ingot former 35 is transmitted to the exhaust gas collection tank 26 through the gas transmission pipe 32, and is discharged through the gas outlet 22 after the operation of the equipment is completed. The sealing partition 34 is located at the upper end of the exhaust gas collection tank 26, and the upper end surface thereof is in contact with the solid refining agent 23.

[0062] Specific embodiment eight: Figure 1 and Figure 3 In this embodiment, the solid refining agent 23 is ZnCl2. In this way, the solid refining agent 23 in this embodiment selects ZnCl2. Since the Nb element is more active than the Zn element, the reaction is relatively violent when the solid refining agent 23 acts. The addition amount of the solid refining agent 23 is 0.2% of the mass of the alloy. Since the solid refining agent 23 is prone to deliquescence after absorbing water in the air, the furnace door 28 needs to be closed in time after the use of the equipment to prevent too much air from entering. The solid refining agent 23 in this embodiment can assist in removing hydrogen inside the niobium-silicon-based alloy liquid and removing oxide inclusions in the niobium-silicon-based alloy liquid during the solidification process of the niobium-silicon-based alloy liquid, so as to improve the purity of the niobium-silicon-based alloy ingot. The other components and connection relationship are the same as any one of the specific embodiments one to seven.

[0063] DETAILED DESCRIPTION NINE: COMBINATION Figures 1 to 3 To illustrate this embodiment, the preparation method of this embodiment includes the following steps:

[0064] Step one: inspection work;

[0065] Step one: check if the connector 36 is connected normally, if loose, adjust in time;

[0066] Step two: check if the water circulation of the water-cooled circulating system is normal, if not, adjust;

[0067] Step three: check if the pressure gauge 18 on the furnace body 21 is normal;

[0068] Step two: lay the niobium-silicon-based alloy raw material 16;

[0069] Put the niobium-silicon-based alloy raw material 16 into the water-cooled crucible 5, and place it evenly to ensure that the contact surface between the niobium-silicon-based alloy raw material 16 and the water-cooled crucible 5 is large enough. After the above operation is completed, close the furnace door 28 on the furnace body 21;

[0070] Step three: vacuumize the inside of the equipment;

[0071] Step three: open the air extraction mechanism controller 2 while paying attention to the pressure gauge 18, when the vacuum degree in the furnace body 1 is 0.1 MPa, immediately close the air extraction mechanism controller 2, and open the gas filling valve 3 to fill the inert gas argon into the furnace body 1, and then pay attention to the pressure gauge 18 again, and keep the vacuum degree in the furnace body 1 at 0.03 MPa;

[0072] Step four: heat the niobium-silicon-based alloy raw material 16 to melt;

[0073] Turn on the induction coil power supply 14, and at the same time, observe the niobium-silicon-based alloy raw material 16 through the observation window 17 on the furnace body 1, and after the niobium-silicon-based alloy raw material 16 is completely melted, proceed to the next step;

[0074] Step five: observe the liquid level in the ingot former 35;

[0075] Open the gas filling valve 3 again to continuously fill the inert gas argon into the furnace body 1, and through the observation window 17, observe whether the liquid level in the ingot former 35 continues to rise slowly, if not or the rising speed is too fast, adjust the gas filling valve 3 in time; at the same time, open the button 1 on the heat preservation coil controller 20 to ensure the normal flow of the niobium-silicon-based alloy metal liquid;

[0076] Step six: slowly solidify the niobium-silicon-based alloy metal liquid;

[0077] When the liquid surface in the ingot former 35 is 2.5 cm away from the upper end surface of the connector 26, the air charging valve 3 is adjusted again to ensure that the liquid level does not change again; at the same time, button 1 on the heat preservation coil controller 20 is turned off, and button 2 on the heat preservation coil controller 20 is turned on, so that the niobium-silicon-based alloy liquid in the ingot former 35 slowly solidifies;

[0078] Step seven: operate the push rod 24 to push the solid refining agent 23 into the ingot former 35;

[0079] Step eight: observe the solidification of the niobium-silicon-based alloy liquid through the observation window 17, and after waiting for the niobium-silicon-based alloy liquid to solidify, turn off button 2 on the heat preservation coil controller 20, the induction coil power supply 14 and the air charging valve 3 in sequence;

[0080] Step nine: after waiting for the niobium-silicon-based alloy to cool down, open the furnace door 28, remove the connector 36, separate the impurity removal system and the ingot former 35, and then take out the niobium-silicon-based alloy high-utilization ingot.

[0081] Specific implementation method ten: combined Figure 1 and Figure 8 This embodiment is described, and the composition of the niobium-silicon-based alloy raw material 16 in this embodiment is Nb-16Si-20Ti alloy. In this way, the alloy system of this embodiment covers high-temperature alloys, and the preferred composition of the high-temperature alloy is Nb-16Si-20Ti high-temperature alloy. Other compositions and connection relationships are the same as any one of specific implementation methods one to seven.

[0082] The alloy system of this embodiment covers niobium-silicon-based alloys, and the specific example of the niobium-silicon-based alloy composition in the example is Nb-16Si-22Ti alloy.

[0083] combined Figures 4 to 8 to illustrate the inventive effect of this embodiment. By using Figure 4 and Figure 5 For comparison: the edge microstructure of the Nb-16Si-22Ti alloy ingot prepared by using the present application has no obvious chilling zone, the structure is dense and uniform, and the NbSS phase and the Nb5Si3 phase are uniformly distributed; while the edge microstructure of the Nb-16Si-22Ti alloy ingot prepared by using the prior art has a obvious chilling zone, which is caused by the too fast cooling speed of the Nb-16Si-22Ti alloy ingot during solidification, and this part often needs to be removed during use, thereby greatly reducing the utilization rate of the niobium-silicon-based alloy ingot. Figure 6The figure shows the microstructure of the Nb-Si based alloy ingot prepared by the prior art, the highlighted part in the figure is the un-dissolved Nb element, which needs to be removed during the use of the Nb-Si based alloy ingot, otherwise it will affect the service life and the accuracy of the experiment of the Nb-Si based alloy, thus reducing the utilization rate of the Nb-Si based alloy ingot. Figure 7 and Figure 8 By comparison: the room temperature fracture toughness of the left side, the middle and the right side of the Nb-16Si-22Ti alloy ingot prepared by the present application is almost the same, which shows that the Nb-16Si-22Ti alloy ingot prepared by the present application is uniform in composition and high in purity, the atoms in the alloy are fully diffused during the solidification process, so the part to be removed during the use process is very small, thus greatly improving the utilization rate of the Nb-16Si-22Ti alloy ingot; while the room temperature fracture toughness of the left side, the middle and the right side of the Nb-16Si-22Ti alloy ingot prepared by the prior art has obvious difference, because the microstructure of the two sides of the ingot is abnormally refined due to the chilling effect during the solidification process, which needs to avoid the abnormal microstructure of the two sides during the use process, which will not be conducive to the full use of the Nb-16Si-22Ti alloy ingot, thus reducing the utilization rate of the Nb-Si based alloy ingot.

[0084] The above examples are only used to illustrate the technical solutions of the present application, but not to limit it; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that they can still modify the technical solutions recorded in the foregoing examples, or make equivalent replacement for part of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. An apparatus for preparing high-utilization-rate ingots of niobium-silicon-based alloys, characterized by: It includes an exhaust control component, a water cooling circulation system, an impurity removal system, a furnace body (21), an ingot former (35), a water-cooled crucible body (5), a heat preservation coil (19) and a heat preservation coil controller (20); The exhaust control assembly is installed on the outside of the furnace body (21) and extends into the furnace body (21), and extracts high-concentration oxygen inside the furnace body (21) to prevent the niobium-silicon based alloy raw material (16) from reacting with oxygen during the smelting process; The water-cooled circulation system includes a cooling system, a copper base (12), an induction coil (13) and an induction coil power supply (14); the water-cooled crucible body (5) is located at the lower part of the furnace body (21) and is connected to the copper base (12); the niobium-silicon-based alloy raw material (16) is evenly laid on the water-cooled crucible body (5); the induction coil (13) is mounted on the water-cooled crucible body (5) and is connected to the induction coil power supply (14) located outside the furnace body (21); the induction coil (13) serves as a heat source to heat the niobium-silicon-based alloy raw material (16); the cooling system is installed on the water-cooled crucible body (5); and the reaction speed of the niobium-silicon-based alloy raw material (16) is adjusted by the induction coil (13) and the cooling system; The ingot former (35) is vertically mounted on the upper side of the niobium-silicon-based alloy raw material (16); the impurity removal system is mounted outside the furnace body (21) and connected to the upper portion of the ingot former (35) to remove oxidized impurities in the niobium-silicon-based alloy liquid metal; and the two corners of the upper bottom surface of the ingot former (35) are de-sharpened. The insulation coil (19) is mounted on the ingot former (35), and the insulation coil (19) is connected to the insulation coil controller (20); The impurity removal system includes a screen (29), a conveying pipe (31), a gas transmission pipe (32), an exhaust gas pipe (33), a sealing partition (34), a connector (36), a push rod (24), a sealing ring (25), a solid refining agent (23), a sealing partition (34) and an exhaust gas collection tank (26). A connector (36) is mounted on the upper portion of the ingot former (35), a screen (29) is mounted on the upper end surface of the ingot former (35), one end of the conveying pipe (31) is covered on the screen (29), the other end of the conveying pipe (31) is connected to the upper portion of the exhaust gas collecting tank (26), a sealing partition (34) is horizontally provided on the upper portion of the exhaust gas collecting tank (26), the lower portion of the push rod (24) passes through the sealing ring (25) and extends downward, and a solid refining agent (23) is installed in a chamber formed between the conveying pipe (31) and the lower end surface of the push rod (24); One end of the gas transmission pipe (32) is connected to the upper end of the ingot former (35) through the exhaust gas pipe (33), and the other end of the gas transmission pipe (32) is connected to the exhaust gas collection tank (26). A plurality of sealing partitions (34) are installed at the lower part of the exhaust gas collection tank (26), and a venting port (22) is provided on the outer side of the lower part of the exhaust gas collection tank (26).

2. The device for preparing a niobium-silicon-based alloy high-utilization ingot according to claim 1, characterized in that: The air extraction control assembly comprises an air storage tank (4), an air extraction device (1), an air charging valve (3), and an air extraction mechanism controller (2). The air extraction device (1) extends into the furnace body (21) through a pipeline, the air extraction mechanism controller (2) is installed on the pipeline, and the air storage tank (4) is connected to the pipeline through the air charging valve (3).

3. The device for preparing a niobium-silicon based alloy high-utilization ingot according to claim 2, characterized in that: The exhaust control assembly further includes an air delivery pipe (15), one end of which is connected to a pipeline extending into the furnace body (21), and the other end of which is bent upward with the air outlet facing downward, and a distance is left between the end of the air outlet of the air delivery pipe (15) and the upper end surface of the niobium-silicon-based alloy raw material (16).

4. The apparatus for preparing a niobium-silicon based alloy high-utilization ingot according to claim 3, characterized in that: The distance between the gas outlet end of the gas delivery pipe (15) and the upper end surface of the niobium-silicon based alloy raw material (16) is 8 cm.

5. The device for preparing a niobium-silicon based alloy high-utilization ingot according to claim 4, characterized in that: The cooling system includes a water inlet insert (6), a water outlet insert (7), a water inlet pipe (10), a water outlet pipe (11), a water inlet insert plate (8) and a water outlet insert plate (9); The water inlet plug plate (8), the water inlet pipe (10) and the water inlet plug pipe (6) are connected in sequence and then extended into the water-cooled crucible body (5); the water outlet plug plate (9), the water outlet pipe (11) and the water outlet plug pipe (7) are connected in sequence and then extended into the water-cooled crucible body (5).

6. The device for preparing a niobium-silicon based alloy high-utilization ingot according to claim 5, characterized in that: The solid refining agent (23) is ZnCl2.

7. A method for preparing a high-utilization-rate niobium-silicon alloy ingot using the apparatus according to any one of claims 1 to 6, characterized in that: It includes the following steps: Step 1: Check the work; Step 11: Check whether the connector (36) is connected properly. If it is loose, adjust it in time; Step 1 and 2: Check whether the water circulation of the water cooling system is normal. If not, adjust it. Step 13: Check whether the pressure gauge (18) on the furnace body (21) shows normal readings; Step 2: Laying niobium-silicon based alloy raw material (16); Place the niobium-silicon-based alloy raw material (16) into the water-cooled crucible body (5), and spread it evenly to ensure that the contact surface between the niobium-silicon-based alloy raw material (16) and the water-cooled crucible body (5) is large enough. After completing the above steps, close the furnace door (28) on the furnace body (21); Step 3: Vacuum the inside of the equipment; Step 31: Turn on the pumping mechanism controller (2) while paying attention to the indication of the pressure gauge (18). When the vacuum degree in the furnace body (21) is 0.1 MPa, immediately turn off the pumping mechanism controller (2) and open the charging valve (3) at the same time to allow the inert gas argon to be charged into the furnace body (21). Pay attention to the indication of the pressure gauge (18) again to maintain the vacuum degree in the furnace body (21) at 0.03 MPa. Step 4: heating the niobium-silicon based alloy raw material (16) until it is melted; Turn on the induction coil power supply (14), and observe the niobium-silicon-based alloy raw material (16) through the observation window (17) on the furnace body (21), and wait for the niobium-silicon-based alloy raw material (16) to be completely melted before proceeding to the next step; Step 5: Observe the liquid level in the ingot forming device (35); Open the charging valve (3) again to allow the inert gas argon to continue to be charged into the furnace body (21), and observe through the observation window (17) whether the liquid level in the ingot former (35) continues to rise slowly. If it does not rise or rises too fast, adjust the charging valve (3) in time; at the same time, turn on the button 1 on the insulation coil controller (20) to ensure the normal flow of the niobium-silicon based alloy metal liquid; Step 6: The niobium-silicon based alloy liquid metal slowly solidifies; When the liquid level in the ingot former (35) is 2.5 cm away from the upper end surface of the connector (36), the inflation valve (3) is adjusted again to ensure that the liquid level does not change; at the same time, the button 1 on the insulation coil controller (20) is closed, and the button 2 on the insulation coil controller (20) is opened to allow the niobium-silicon based alloy metal liquid in the ingot former (35) to slowly solidify; Step 7: Operate the push rod (24) to push the solid refining agent (23) into the ingot forming device (35); Step 8: Observe the solidification of the niobium-silicon-based alloy metal liquid through the observation window (17). After the solidification of the niobium-silicon-based alloy metal liquid is completed, turn off the button 2 on the insulation coil controller (20), the induction coil power supply (14) and the inflation valve (3) in sequence; Step 9: After the niobium-silicon alloy is cooled, the furnace door (28) is opened, the connector (36) is removed, the impurity removal system and the ingot former (35) are separated, and the niobium-silicon alloy high-utilization ingot is taken out.

8. The preparation method according to claim 7, characterized in that: The composition of the niobium-silicon based alloy raw material (16) is Nb-16Si-20Ti alloy.

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