A solidification device and method for preparing ultra-fine high-temperature alloy with multi-angle enhanced nucleation rate

Abstract

The application relates to a solidification device and method for preparing superfine high-temperature alloy by multi-angle promoting nucleation rate, and relates to alloy comprehensive mechanical property measurement. In order to solve the problems of obvious directionality and element segregation of the existing Nb-Si-based high-temperature alloy when the arc melting is adopted, the application cooperates the double-gun-head arc gun design with the established arc gun operation angle, operation direction, operation sequence and operation frequency, forcibly generates convection in the high-temperature alloy liquid, effectively reduces the composition segregation of the high-temperature alloy and improves the nucleation rate of the high-temperature alloy by using the convection effect. The laser shot peening treatment is creatively carried out on the upper end surface of the oil-water mixed liquid cold copper crucible, a large number of nanoscale micro recesses are formed as non-uniform nucleation points, and the nucleation rate of the high-temperature alloy is improved. The structure of the ingot turning spoon and the monitoring system is improved, the modifier introduced has a synergistic effect with the convection effect, and the nucleation rate of the high-temperature alloy is also effectively improved. The application is used for the preparation of high-temperature alloy.

Description

TECHNICAL FIELD

[0001] The present application relates to a solidification device and method for preparing ultra-fine high-temperature alloy, in particular to a solidification device and method for preparing ultra-fine high-temperature alloy by multi-angle improving nucleation rate, and belongs to the technical field of alloy preparation. BACKGROUND

[0002] As the main material of the aero-engine, the high-temperature alloy material has a proportion of up to 40%-60%, and is applied in the combustion chamber, guide vane, turbine vane, turbine disc, four large heat section parts, casing, ring, afterburner and tail nozzle of the aero-engine, and has a huge application prospect.

[0003] As one of the methods for preparing large-size high-temperature alloy in industrial production, the ingot metallurgy has many advantages such as low cost, and is widely used. However, under the existing technology, the prepared high-temperature alloy generally has problems of coarse organization, obvious directionality and serious element segregation. Taking the Nb-Si-based high-temperature alloy as an example, under the existing technology, due to the addition of a large amount of alloying elements, the organization will be obviously coarse, and the elements will be seriously segregated, which is not conducive to the overall performance of the Nb-Si-based high-temperature alloy material, thereby greatly reducing the application range thereof.

[0004] The reason why the existing solidification device has the above problems is that it lacks control of the nucleation rate of the high-temperature alloy in the solidification process. Increasing the nucleation rate in the solidification process of the high-temperature alloy can effectively refine the organization, reduce the directionality in the grain growth process of the high-temperature alloy, that is, hinder the growth in the columnar crystal mode and promote the growth in the equiaxed crystal mode, and reduce the element segregation in the solidification process of the high-temperature alloy. On the other hand, the higher the nucleation rate, the finer the grain, according to the fine-grain strengthening principle, it can simultaneously improve the strength and toughness of the high-temperature alloy, thereby taking into account the overall performance of the high-temperature alloy material. At the same time, the structural design of the existing solidification device is not conducive to taking into account the overall performance of the high-temperature alloy.

[0005] In summary, the existing Nb-Si-based high-temperature alloy has problems of coarse alloy organization, obvious directionality and element segregation when arc melting is used. SUMMARY

[0006] The purpose of the present application is to solve the problems of coarse alloy organization, obvious directionality and element segregation of the existing Nb-Si-based high-temperature alloy when arc melting is used. Further, a solidification device and method for preparing ultra-fine high-temperature alloy by multi-angle improving nucleation rate are provided.

[0007] The technical scheme of the present application is: a solidification equipment for preparing ultra-fine high-temperature alloy with multi-angle improved nucleation rate comprises an electric arc current control cabinet, a pressure gauge, an electric arc current control line, an air extraction device, an air extraction mechanism opening device, an argon tank, an air filling valve, a sight mirror, a right double-gun head electric arc gun device, a left double-gun head electric arc gun device, a turning ingot spoon with a modifier releasing function, a crucible temperature monitoring and furnace picture real-time monitoring integrated device, a vacuum electric arc furnace and an oil-water mixed liquid cooling system; the upper portion of the vacuum electric arc furnace is provided with the sight mirror, the pressure gauge is installed on the upper end face of the vacuum electric arc furnace through a pressure gauge seat, the turning ingot spoon with the modifier releasing function is movably installed on the upper end face of the vacuum electric arc furnace, and the turning ingot spoon with the modifier releasing function realizes lifting operation, rotating operation and modifier releasing operation; the oil-water mixed liquid cooling system is installed inside the vacuum electric arc furnace and cools the crucible by inputting oil-water mixed liquid; the right double-gun head electric arc gun device and the left double-gun head electric arc gun device are rotatably installed on the upper end face of the vacuum electric arc furnace, the lower portions of the right double-gun head electric arc gun device and the left double-gun head electric arc gun device extend into the vacuum electric arc furnace, and the electric arc current control cabinet is connected with the right double-gun head electric arc gun device and the left double-gun head electric arc gun device through the electric arc current control line; the crucible temperature monitoring and furnace picture real-time monitoring integrated device is installed directly above the vacuum electric arc furnace body; the sight mirror is located at the right upper portion of the vacuum electric arc furnace body; the air extraction device is connected with the vacuum electric arc furnace through a pipeline and realizes vacuumizing operation of the vacuum electric arc furnace through the air extraction mechanism opening device arranged on the pipeline; the argon tank is connected with the pipeline, and the air filling valve is installed on the output pipe of the argon tank.

[0008] Further, the vacuum electric arc furnace comprises a body, a furnace door and a sealing gasket, the sealing gasket is installed on the furnace door, and the furnace door is openably connected with the body.

[0009] Further, the right double-gun head electric arc gun device and the left double-gun head electric arc gun device are the same in structure, the left double-gun head electric arc gun device comprises a rotating wheel disc, a bellows, a protective sleeve, a lifting rod and double-tungsten electrode, the double-tungsten electrode is installed at the lower portion of the lifting rod through positioning bolts, the protective sleeve is sleeved on the lifting rod, the bellows is installed at the upper portion of the lifting rod, a support rod is installed at the upper end portion of the bellows, and the rotating wheel disc is installed at the upper end portion of the support rod.

[0010] Further, the turning ingot spoon with the modifier releasing function comprises a turning ingot spoon head, a cylindrical storage rod, a modifier, a double-sided pulling device and a control rod, the double-sided pulling device is installed on the left and right sides of the cylindrical storage rod and extends downward along the outer sidewall of the cylindrical storage rod, the cylindrical storage rod is sealingly connected with the vacuum electric arc furnace and extends into the vacuum electric arc furnace, and the control rod is installed at the upper portion of the cylindrical storage rod and located outside the vacuum electric arc furnace.

[0011] Further, the crucible temperature monitoring and real-time furnace picture monitoring integrated device comprises a threaded double-cylinder glass window, an infrared temperature detector, a temperature display, an infrared high-definition optical fiber transmission camera, a transceiver one, an optical fiber signal transmission line, a fusion box, a transceiver two, a switch and a hard disk video recorder; the infrared temperature detector is connected to the threaded double-cylinder glass window on the upper end of the vacuum arc furnace through threads, the infrared temperature detector is connected with the temperature display; the infrared high-definition optical fiber transmission camera is located on the right side of the infrared temperature detector and is connected to the threaded double-cylinder glass window through threads, the measured picture data is transmitted to the transceiver one through the optical fiber signal transmission line, and the data is sequentially transmitted to the fusion box, the transceiver two, the switch and the hard disk video recorder which are electrically connected with each other.

[0012] Further, the oil-water mixture cooling system comprises a smelting pit with nano-level micro recesses subjected to laser shot peening treatment, a copper crucible body, a copper shell, a copper base, an oil-water mixture inlet pipe, an oil-water mixture outlet pipe, an oil-water mixture inlet pipe, an oil-water mixture outlet pipe, an oil-water mixture inlet plate and an oil-water mixture outlet plate; the copper base is installed in the vacuum arc furnace, the smelting pit with nano-level micro recesses subjected to laser shot peening treatment is installed on the copper base and located in the copper shell, the upper parts of the oil-water mixture inlet pipe and the oil-water mixture outlet pipe are inclined to one side, the oil-water mixture inlet pipe and the oil-water mixture outlet pipe are vertically installed in the oil-water mixture cooling copper crucible body, one end of the oil-water mixture inlet pipe and the oil-water mixture outlet pipe is respectively inserted into the oil-water mixture inlet pipe and the oil-water mixture outlet pipe, and the other end of the oil-water mixture inlet pipe and the oil-water mixture outlet pipe is respectively connected with the oil-water mixture inlet plate and the oil-water mixture outlet plate.

[0013] The application also provides a preparation method of a solidification equipment for preparing ultra-fine high-temperature alloy by using multi-angle promotion nucleation rate, which comprises the following steps:

[0014] Step one: inspection work;

[0015] The copper crucible body is polished and cleaned with alcohol and sandpaper; whether there is smelting residual metal on the double-tungsten electrode is observed, if there is, the double-tungsten electrode is polished in time by an angle grinder and is replaced, the double-tungsten electrode is placed in the nut, the positioning bolt with a hole is installed, the lifting rod and the double-tungsten electrode are connected, and whether the oil-water mixture cooling system is normal is checked.

[0016] Step two: the high-temperature alloy elements with a proper proportion are placed in the oil-water mixture cooling copper smelting pit with nano-level micro recesses subjected to laser shot peening treatment on the upper end face, the position of the ingot turning ladle with modification agent releasing function is adjusted to be directly above the oil-water mixture cooling copper smelting pit with nano-level micro recesses subjected to laser shot peening treatment on the upper end face, and the furnace door is closed after the above-mentioned actions are completed;

[0017] Step 3: Turn on the vacuum pumping device.

[0018] First, turn on the air extraction mechanism and observe the reading on the pressure gauge. When the vacuum degree in the electric arc furnace reaches 0.1 MPa, turn off the air extraction mechanism. At the same time, open the inflation valve to allow the inert gas argon to fill into the furnace. Then, observe the reading on the pressure gauge again and maintain the vacuum degree in the furnace at 0.05 Mpa.

[0019] Step 4: Control the left double-gun head electric arc gun device and the right double-gun head electric arc gun device.

[0020] Rotate the wheel disc to adjust the left double-gun head electric arc gun device and the right double-gun head electric arc gun device so that the center point of the connection line between the two gun heads of the double tungsten electrodes is 1 - 2 mm above the superalloy raw material.

[0021] Step 5: Turn on the integrated device for crucible temperature monitoring and real-time monitoring of the furnace interior.

[0022] After turning it on, check whether the reading displayed on the infrared thermometer is correct. At the same time, check whether the signal transmission of the infrared high-definition fiber optic transmission camera is stable.

[0023] Step 6: Turn on the arc current control component and observe the reading on the infrared thermometer in real-time. At the same time, start to control the left double-gun head electric arc gun device and the right double-gun head electric arc gun device to make them arc.

[0024] The operating angles of the left double-gun head electric arc gun device and the right double-gun head electric arc gun device are: the double tungsten electrodes of the left double-gun head electric arc gun device and the right double-gun head electric arc gun device form an angle of 45° with respect to the direction perpendicular to the ground.

[0025] The operating directions of the left double-gun head electric arc gun device and the right double-gun head electric arc gun device are: passing through the center of gravity of the copper crucible body, and the plane formed by the movement direction of the double-gun head electric arc gun and the center point of the connection line between the two gun heads needs to be always perpendicular to the plane of the copper crucible body.

[0026] The movement sequence is that the left double-gun head electric arc gun device first makes a complete movement trajectory in the established direction, and then the right double-gun head electric arc gun device makes a complete movement trajectory in the established direction, and so on repeatedly.

[0027] Until the reading on the infrared thermometer reaches the melting point of the superalloy, immediately stop increasing the arc current. If the specific melting point of the alloy is not clear, the reading on the infrared thermometer shall not be higher than the melting point of the main element in the alloy composition. Then, maintain this arc current until the superalloy is completely melted.

[0028] Step 7: Pull the pulling devices on both sides of the ingot turning spoon with the function of releasing the modifier to partially release the modifier. After partial release, return the bilateral pulling devices.

[0029] Step eight: observe the opening of the crucible temperature monitoring and real-time monitoring of the picture integration device;

[0030] Observe the reading of the infrared temperature measuring instrument to room temperature, and the fiber transmission picture displays the solidification of the high-temperature alloy in the furnace, at this time, the ingot is turned over by using the ingot turning ladle with modification agent releasing function;

[0031] Step nine: repeat the operation of step six, step seven and step eight, so that the ingot is repeatedly remelted 5-10 times, and the melting times are determined according to the alloy composition, and thus the preparation of the high-temperature alloy is completed.

[0032] Further, the high-temperature alloy elements with a proportion prepared in step two are Nb-16Si-20Ti high-temperature alloy.

[0033] Further, the copper crucible body is made of T2 purple copper material.

[0034] Compared with the prior art, the present application has the following effects:

[0035] The present application solves the problems of coarse organization, obvious direction and serious element segregation of high-temperature alloy after solidification by using a new structure design, full range, multi-angle and micro-fine, which has important positive significance for the preparation of aero-engine materials.

[0036] 1、The present application utilizes the unique double-gun head arc gun design and the established arc gun operation angle, operation direction, operation sequence and operation frequency to cooperate, to manufacture forced convection in the high-temperature alloy liquid, effectively reduce the composition segregation of the high-temperature alloy and improve the nucleation rate of the high-temperature alloy by using the convection effect. In the prior art, most of them are single arc gun design, and a few of them are double arc gun design, and in the double arc gun design, generally single gun head design, which cannot achieve the above forced convection effect.

[0037] 2、The present application is provided with infrared thermometer and infrared high-definition optical fiber transmission camera, the former can timely observe the real-time temperature of the alloy in the crucible, control the temperature not to exceed the melting point of the alloy or the melting point of the main element in the alloy composition, can effectively prevent the superheat of the superalloy liquid, reduce the superheat degree can avoid the already formed crystal nucleus to be melted again and when the superheat degree is larger, the concave curved surface becomes a plane, the number of non-uniform nucleation core is reduced, because the superalloy overheating control can greatly improve the number of crystal nucleus, improve the nucleation rate of superalloy. The latter can monitor and record the solidification process throughout, effectively improve the real-time degree of operation personnel to the situation inside the vacuum arc furnace, reduce the operation error of the operation personnel due to the unclear situation in the furnace, improve the operability and easy-to-use of the equipment; From the melting results of high-temperature alloy from a large sample, the real-time degree of operation personnel to the situation inside the vacuum arc furnace is improved, and the quality of the high-temperature alloy obtained by melting is also generally improved, and the melting cost of the high-temperature alloy is reduced; And the recorded solidification process can objectively evaluate the whole solidification process, which is convenient for finding problems and comparative discussion, can improve the material performance through improving the solidification operation details, greatly reduce the trial and error cost. The prior art does not have accurate temperature monitoring and picture monitoring system, and the high-temperature alloy is often melted by excessive arc current, which leads to overheating of the high-temperature alloy, thereby causing problems of coarse organization and low nucleation rate. The cooperation of the former and the latter, that is, the cooperation of temperature data and high-temperature alloy melting picture in the furnace, improves the degree of operation personnel to the high-temperature alloy organization form, greatly improves the problem that the high-temperature alloy is overheated due to the melting of the high-temperature alloy by the excessive arc current in the prior art, thereby causing the problems of coarse organization and low nucleation rate. Based on this, the whole solidification process can be objectively evaluated, which is convenient for finding problems and comparative discussion, and the material performance can be improved through improving the solidification operation details, greatly reducing the trial and error cost. The prior art does not have accurate temperature monitoring and picture monitoring system, and the high-temperature alloy is often melted by excessive arc current, which leads to overheating of the high-temperature alloy, thereby causing problems of coarse organization and low nucleation rate.

[0038] 3、Laser peening technology in the field of high-temperature alloy is usually used as a surface strengthening means of finished product, and the present application creatively applies it to the melting process of high-temperature alloy, and creatively performs laser peening treatment on the upper end face of oil-water mixed liquid copper crucible, so that a large number of nanoscale micro concave are formed on the surface. According to the solidification principle of high-temperature alloy, the concave interface base has the strongest nucleation ability, which greatly improves the nucleation rate of high-temperature alloy. At the same time, the surface roughness increases after laser peening treatment, which provides more non-uniform nucleation points for high-temperature alloy solidification, so that the nucleation process is more easy to carry out, and the nucleation rate of high-temperature alloy is also effectively improved.

[0039] 4、The present application improves the water cooling system, and uses oil-water mixture to reduce the cooling speed of the crucible, but still makes the high-temperature alloy liquid supercooling reach the effective nucleation supercooling. According to the solidification principle of high-temperature alloy, if the high-temperature alloy liquid supercooling reaches the effective nucleation supercooling, too much supercooling will not improve the nucleation rate, but will increase the temperature gradient in front of the solidification interface, causing the high-temperature alloy to grow in columnar crystals. During the columnar crystal growth process, solute is discharged, causing the liquidus of the alloy to drop, thereby reducing the high-temperature alloy nucleation rate. The present application innovatively adjusts the ratio of oil-water mixture: 24% of mineral oil, 73% of water, 1% of surfactant, 1% of cooling accelerator, and 1% of antioxidant. The prior art is mostly 1:10 or 1:15. The present application increases the proportion of mineral oil, aiming to reach the effective nucleation temperature of high-temperature alloy while slowing down the cooling speed, thereby avoiding overheating of the high-temperature alloy liquid caused by excessive effective nucleation temperature, preventing the high-temperature alloy from growing in columnar crystals caused by the increase of the temperature gradient in front of the solidification interface, and improving the reduction of the high-temperature alloy nucleation rate caused by the drop of the liquidus of the alloy.

[0040] 5、The present application innovatively improves the structure of the existing ingot turning spoon, which has the functions of general ingot turning spoon and modification agent storage and release. The existing technology cannot add modification agent due to the need for sealing during the melting of high-temperature alloy in a vacuum arc furnace, but the present application effectively and low-costly solves this problem, thereby further refining the high-temperature alloy structure and improving the comprehensive mechanical properties of the high-temperature alloy. At the same time, this innovation point is matched with the unique double-gun head arc gun design, the established arc gun operation angle, direction, sequence, and frequency designed by the present application, making the modification agent action range more uniform and the effect better. The strong convection effect is also better due to the addition of modification agent. Therefore, the purpose of mutual promotion is truly achieved. BRIEF DESCRIPTION OF DRAWINGS

[0041] Figure 1 is the overall structure schematic diagram of the high-temperature alloy preparation equipment of the present application;

[0042] Figure 2 is the top view of the vacuum arc furnace;

[0043] Figure 3 is the structure schematic diagram of the right double-gun head arc gun device 9 or the left double-gun head arc gun device 10;

[0044] Figure 4 is the structure schematic diagram of the ingot turning spoon 11 with modification agent release function;

[0045] Figure 5 is the schematic diagram of the crucible temperature monitoring and furnace picture real-time monitoring integrated device 12.

[0046] Figure 6 is a schematic diagram of the upper end surface of a laser peening treated oil-water mixed liquid copper crucible with nanoscale micro-concave;

[0047] Figure 7 is a schematic diagram of the intended direction of operation when melting superalloys using the right double gun head arc gun device 9 and the left double gun head arc gun device 10;

[0048] Figure 8 is a sample organization picture prepared using the prior art equipment;

[0049] Figure 9 is a sample organization picture prepared using the present application;

[0050] Figure 10 is a comparison bar chart of the room temperature fracture toughness of a sample prepared using the prior art equipment and the room temperature fracture toughness of a sample prepared using the present application;

[0051] Figure 11 is a comparison bar chart of the high temperature strength of a sample prepared using the prior art equipment and the high temperature strength of a sample prepared using the present application.

[0052] Figure 12 is a fracture photograph of a Nb-Si based superalloy prepared using the present application;

[0053] Figure 13 is a fracture photograph of a Nb-Si based superalloy prepared using the prior art. DETAILED DESCRIPTION

[0054] The technical solutions of the present application are not limited to the following specific embodiments, and any reasonable combination of the specific embodiments is also included.

[0055] Specific embodiment one: combining Figure 1 and Figure 2This embodiment describes an implementation that includes an arc current control cabinet 1, a pressure gauge 2, an arc current control line 3, a vacuum device 4, an open vacuum mechanism 5, an argon tank 6, a filling valve 7, a sight glass 8, a right double-headed arc lance device 9, a left double-headed arc lance device 10, a tilting spoon with a modifier release function 11, an integrated device for crucible temperature monitoring and real-time furnace internal monitoring 12, a vacuum arc furnace 13, and an oil-water mixture cooling system 14. A sight glass 8 is installed on the upper part of the vacuum arc furnace 13. The pressure gauge 2 is mounted on the upper surface of the vacuum arc furnace 13 via a pressure gauge base. The tilting spoon 11 with a modifier release function is movably mounted on the upper surface of the vacuum arc furnace 13, and the tilting spoon 11 with the modifier release function can perform lifting, rotating, and modifier release operations. The oil-water mixture cooling system 14 is installed inside the vacuum arc furnace 13. The crucible is cooled by introducing an oil-water mixture. The right double-headed arc gun device 9 and the left double-headed arc gun device 10 are rotatably mounted on the upper surface of the vacuum arc furnace 13, with the lower parts of the right double-headed arc gun device 9 and the left double-headed arc gun device 10 extending into the vacuum arc furnace 13. The arc current control cabinet 1 is connected to the right double-headed arc gun device 9 and the left double-headed arc gun device 10 respectively through the arc current control line 3. The crucible temperature monitoring and furnace interior real-time monitoring integrated device 12 is installed directly above the furnace body of the vacuum arc furnace 13. The sight glass 8 is located on the upper right side of the furnace body of the vacuum arc furnace 13. The evacuation device 4 is connected to the vacuum arc furnace 13 through a pipe, and the vacuum furnace 13 is evacuated by the evacuation mechanism 5 set on the pipe. The argon tank 6 is connected to the pipe, and the output pipe of the argon tank 6 is equipped with an inflation valve 7.

[0056] In this embodiment, the operation of the right double-headed arc gun device 9 and the left double-headed arc gun device 10 needs to be performed according to predetermined arc gun operating angles, operating directions, operating sequences, and operating frequencies: the operating angles of the right double-headed arc gun device 9 and the left double-headed arc gun device 10 are as follows: Figure 7 As shown in (b), the cylindrical tungsten electrode portions of the left double-headed arc gun device 10 and the right double-headed arc gun device 9 form a 45° angle with respect to the direction perpendicular to the ground; the operating directions of the left double-headed arc gun device 10 and the right double-headed arc gun device 9 are... Figure 7(b), that is, the plane formed by the center point of the line connecting the two gun heads and the movement direction of the double gun head arc furnace passing through the center of the crucible must be perpendicular to the plane of the crucible; the movement sequence of the double gun head arc furnace device 10 and the right double gun head arc furnace device 9 is that the left double gun head arc furnace device 10 first moves along a complete trajectory in a predetermined direction, and then the right double gun head arc furnace device 9 moves along a complete trajectory in a predetermined direction, and so on; the movement frequency of the double gun head arc furnace device 10 and the right double gun head arc furnace device 9 is determined according to the flow trend of the metal liquid in the crucible, that is, after the left double gun head arc furnace device 10 moves in a predetermined direction, it needs to wait for the completion of the forced convection of the metal liquid caused by it (after the circular arc metal liquid movement trajectory is formed), and then the right double gun head arc furnace device 9 is operated, and after the operation of the right double gun head arc furnace device 9 is completed, it also needs to wait for the completion of the forced convection of the metal liquid caused by it (after the circular arc metal liquid movement trajectory is formed), and then the left double gun head arc furnace device 10 is operated, and so on. As shown in FIG. 2. Figure 7 (a), the liquid flow in the crucible caused by the left double gun head arc furnace device 10 is indicated by a small arrow, the liquid flow in the crucible caused by the right double gun head arc furnace device 9 is indicated by a large arrow, and the two flows form opposite flow trends in the same crucible to induce convection. This effectively reduces the composition segregation of the high-temperature alloy and improves the nucleation rate of the high-temperature alloy by utilizing the convection effect.

[0057] By using the unique double gun head arc furnace design and the cooperation of the predetermined arc furnace operation angle, operation direction, operation sequence, and operation frequency, melting, timely observation of the real-time temperature and picture of the alloy in the crucible, the manufacture of a large number of nanoscale micro recesses on the upper end surface of the oil-water mixed liquid cooled copper crucible, the use of oil-water mixed liquid cooling to reduce the cooling speed of the crucible but still make the high-temperature alloy liquid supercooling degree reach the effective nucleation supercooling degree, and other innovative technologies, the Nb-Si-based high-temperature alloy or Ti-Al high-temperature alloy is melted, the nucleation rate during the solidification process of the high-temperature alloy is greatly improved, and the comprehensive mechanical properties of the high-temperature alloy are greatly improved, that is, the strength and toughness of the high-temperature alloy are improved, and the application range, safety factor, and service life of the melted material are greatly improved.

[0058] Specific implementation method two: combined with Figure 2 In this embodiment, the vacuum arc furnace 13 includes a body, a furnace door 16, and a sealing gasket 17, the sealing gasket 17 is installed on the furnace door 16, and the furnace door 16 is in openable connection with the body. In this way, auxiliary observation can be performed while the crucible temperature monitoring and real-time monitoring of the furnace picture integrated device is running, which serves as part of the observation function and ensures normal use of the equipment in the event of power failure or failure of the crucible temperature monitoring and real-time monitoring of the furnace picture integrated device. The other components and connection relationships are the same as those in the first specific embodiment.

[0059] The sealing rubber ring is installed around the furnace door, and the vacuum silica gel is applied to prevent the furnace door from leaking, so as to prevent the vacuum furnace from being polluted by external gas and the smelting material.

[0060] Specific embodiment three: combination Figure 3 and Specific embodiment three: combination Figure 7 The right double gun head arc gun device 9 and the left double gun head arc gun device 10 of the embodiment are the same in structure, and the left double gun head arc gun device 10 comprises a rotating wheel disc 19, a bellows 20, a protective sleeve 21, a lifting rod 22, and a double tungsten electrode 23. The double tungsten electrode 23 is installed at the lower part of the lifting rod 22 through positioning bolts. The protective sleeve 21 is sleeved on the lifting rod 22. The bellows 20 is installed at the upper part of the lifting rod 22. A support rod is installed at the upper end of the bellows 20. The rotating wheel disc 19 is installed at the upper end of the support rod, and is used for controlling the lifting operation and the arc striking operation of the left double gun head arc gun device 10 and the right double gun head arc gun device 9. In this way, the double gun head arc gun device is simple and efficient to operate, and is easy to use. At the same time, the double tungsten electrode can be effectively protected, so that the wear of the double tungsten electrode is avoided, and the service life of the double tungsten electrode is greatly prolonged. The other components and connection relationships are the same as those in the first or second embodiment.

[0061] The specific structure of the double tungsten electrode 23 of the embodiment is shown in Figure 3 The specific structure of the double tungsten electrode 23 of the embodiment is shown in Figure 7 The specific structure of the double tungsten electrode 23 of the embodiment is shown in Figure 7When two liquid flows in opposite directions meet, strong convection is caused in the crucible, which breaks the dendrites formed in the liquid of the superalloy during solidification and forms equiaxed grains, thereby greatly increasing the nucleation rate. At the same time, the convection in the solidification process of the superalloy makes the modifier released by the ingot turning spoon 11 with modifier releasing function fully contact with the liquid, thereby promoting the refining effect of the modifier and increasing the nucleation rate of the superalloy during solidification. In terms of composition segregation, strong convection will affect the solute distribution at the front of the solidification interface and the redistribution of solute atoms, so as to reduce the composition segregation of the superalloy during solidification. The double tungsten electrode 23 of the present embodiment cooperates with the unique structure and the established operation method to generate two liquid flows in opposite directions in the superalloy liquid, so as to cause forced convection of the superalloy liquid. The general single tungsten electrode design in the prior art cannot generate liquid convection by regulating the movement trajectory of the tungsten electrode due to the limitation of its own structure, and thus cannot increase the nucleation rate by forced convection of the superalloy liquid.

[0062] The left double gun head arc gun device 10 and the right double gun head arc gun device 9 are operated in the device operation, i.e. the superalloy melting process, and the movement trajectories of the left double gun head arc gun device 10 and the right double gun head arc gun device 9 are operated in the manner shown in Figure 7 As shown in Figure 7 The mixed liquid flow caused by the left double gun head arc gun device 10 is indicated by small arrows to show the flow direction, and the mixed liquid flow caused by the right double gun head arc gun device 9 is indicated by large arrows to show the flow direction, which are opposite to each other, and can effectively generate forced convection in the superalloy liquid. This technical means can skillfully use liquid convection to replace the traditional stirring process, effectively reduce the process complexity while improving the refining effect, i.e. reduce the composition segregation of the superalloy, and at the same time, increase the nucleation rate of the superalloy by using the convection effect.

[0063] Specific implementation four: combine Figure 1 and Figure 4 to illustrate the present embodiment. The ingot turning spoon 11 with modifier releasing function of the present embodiment includes an ingot turning spoon head 24, a cylindrical storage rod 25, a modifier 26, a double-sided pulling device 27 and a control rod 28. The double-sided pulling device 27 is installed on the left and right sides of the cylindrical storage rod 25 and extends downward tightly along the outer side wall of the cylindrical storage rod 25. The cylindrical storage rod 25 is sealingly connected with the vacuum arc furnace 13 and extends into the vacuum arc furnace 13. The control rod 28 is installed on the upper part of the cylindrical storage rod 25 and located outside the vacuum arc furnace 13. In this way, Figure 4The local enlarged portion is an enlarged view of the bottom of the cylindrical material storing rod 25. The multi-functional design of the embodiment solves the problem that the modification agent cannot be added in the vacuum arc furnace to improve the grain size of the high-temperature alloy. According to the principle of fine-grain strengthening, the smaller the grain size, the higher the strength, plasticity and toughness of the high-temperature alloy, thereby improving the comprehensive mechanical properties of the high-temperature alloy. The other components and connection relationships are the same as any one of the first to third embodiments.

[0064] The ingot turning spoon 11 with the modification agent releasing function in the embodiment can achieve the effect of mutual promotion when releasing the modification agent in cooperation with the third embodiment. That is, due to the forced convection of the high-temperature alloy liquid caused by the third embodiment, the modification agent has a more uniform range of action and a better effect. The strong convection effect caused by the third embodiment is also better due to the release of the modification agent in the embodiment.

[0065] The fifth embodiment is combined with the first to fourth embodiments. Figure 5 The embodiment is described. The crucible temperature monitoring and real-time monitoring integrated device 12 includes a threaded double-cylinder glass skylight 29, an infrared temperature measuring instrument 30, a temperature display 38, an infrared high-definition optical fiber transmission camera 31, a transceiver one 32, an optical fiber signal transmission line 34, a fusion box 35, a transceiver two 33, a switch 36 and a hard disk video recorder 37.

[0066] The infrared temperature measuring instrument 30 is connected to the threaded double-cylinder glass skylight 29 on the upper end of the vacuum arc furnace 13 through threads, and the infrared temperature measuring instrument 30 is connected to the temperature display 38. The infrared high-definition optical fiber transmission camera 31 is located on the right side of the infrared temperature measuring instrument 30 and is connected to the threaded double-cylinder glass skylight 29 through threads. The measured implementation picture data is transmitted to the transceiver one 32 through the optical fiber signal transmission line 34, and the data is sequentially transmitted through the fusion box 35, the transceiver two 33, the switch 36 and the hard disk video recorder 37 which are electrically connected to each other. The other components and connection relationships are the same as any one of the first to fourth embodiments.

[0067] The infrared temperature measuring instrument 30 in the embodiment can timely observe the real-time temperature of the alloy in the crucible (referring to the copper crucible body 41), prevent the high-temperature alloy from being overheated too much during the melting process, and control the temperature to be not more than the melting point of the alloy or the melting point of the main element in the alloy composition according to the general law of the alloy melting point. Such design can effectively avoid a series of problems caused by overheating, such as melting the already formed crystal nucleus again, changing the concave surface of the grain nucleation to a plane, reducing the number of non-uniform nucleation cores, etc., thereby effectively improving the nucleation rate of the high-temperature alloy during the vacuum arc furnace melting process, and further improving the comprehensive mechanical properties of the high-temperature alloy.

[0068] The infrared high-definition optical fiber transmission camera 31 in the embodiment can monitor and record the solidification process in real time, effectively improves the real-time control of the operator on the situation inside the vacuum arc furnace, reduces the operation errors caused by the operator's unclear understanding of the situation inside the furnace, and improves the operability and ease of use of the equipment. From the melting results of high-temperature alloys with large samples, the improvement of the operator's real-time control of the situation inside the vacuum arc furnace also generally improves the quality of the high-temperature alloy obtained by melting, and reduces the melting cost of the high-temperature alloy.

[0069] The infrared temperature measuring instrument and the infrared high-definition optical fiber transmission camera in the embodiment cooperate, that is, the temperature data and the high-temperature alloy melting picture in the furnace cooperate, which improves the operator's control of the high-temperature alloy organization form, and greatly improves the problem of the high-temperature alloy overheating caused by the high arc current melting of the high-temperature alloy in the prior art, which leads to the problem of coarse organization and low nucleation rate.

[0070] Specific implementation method six: combined Figure 1 In this embodiment, the oil-water mixture cooling system 14 includes a melting pit 15 with nanoscale micro-depressions treated by laser shot peening, a copper crucible body 41, a copper shell 42, a copper base 40, an oil-water mixture inlet pipe 43, an oil-water mixture outlet pipe 44, an oil-water mixture inlet pipe 45, an oil-water mixture outlet pipe 46, an oil-water mixture inlet plate 47, and an oil-water mixture outlet plate 48;

[0071] Copper base 40 is installed in vacuum arc furnace 13, and the smelting pit 15 with nanoscale micro concave processed by laser shot peening is installed on the copper base 40 and located in the copper shell 42. The upper part of the oil-water mixture inlet pipe 43 and the oil-water mixture outlet pipe 44 is a pipe opening inclined to one side. The oil-water mixture inlet pipe 43 and the oil-water mixture outlet pipe 44 are vertically installed in the oil-water mixture cold copper crucible body 41. One end of the oil-water mixture inlet pipe 45 and the oil-water mixture outlet pipe 46 is respectively inserted into the oil-water mixture inlet pipe 43 and the oil-water mixture outlet pipe 44. The other end of the oil-water mixture inlet pipe 45 and the oil-water mixture outlet pipe 46 is respectively connected with the oil-water mixture inlet and outlet plug plate 47 and the oil-water mixture outlet and inlet plug plate 48. In this way, the oil-water mixture needs to add a surfactant to achieve uniform mixing, that is, one end of the surfactant molecule is an oil-loving group that can effectively enter the oil inside, and the other end is a water-soluble group with good solubility in water. The purpose of the technical solution is to make the supercooling degree of the high-temperature alloy during the vacuum furnace melting and cooling process reach the effective nucleation supercooling degree without exceeding the effective nucleation supercooling degree too much, thereby reducing the temperature gradient. According to the metal solidification principle, an increase in the temperature gradient will lead to columnar growth of the high-temperature alloy during the solidification process. The solute will be discharged during the columnar crystal growth process, resulting in a decrease in the liquidus line of the alloy, thereby reducing the supercooling degree at the same temperature, thereby reducing the nucleation rate of the high-temperature alloy, and further improving the nucleation rate of the high-temperature alloy during the solidification process, and further improving the overall mechanical properties of the high-temperature alloy material. The other components and connection relationships are the same as any one of the first to fifth embodiments.

[0072] The selection of the medium material in the embodiment is a copper crucible that does not react with the high-temperature alloy at high temperature. The size of the crucible can be processed in multiple sizes according to the volume of the material.

[0073] The oil-water mixture ratio of the embodiment is about 1:4, the mineral oil accounts for 24%, the water accounts for 73%, the surfactant accounts for 1%, the refrigerant accounts for 1%, and the antioxidant accounts for 1%. The existing technology is mostly 1:10 or 1:15. The present application increases the proportion of mineral oil, aiming to achieve the effective nucleation temperature of high-temperature alloy while slowing down the cooling speed, thereby avoiding overheating of the high-temperature alloy liquid caused by excessive effective nucleation temperature, preventing the increase of the temperature gradient in front of the solidification interface, improving the nucleation rate of the high-temperature alloy caused by the decrease of the liquidus line of the alloy. The surfactant is used to realize uniform mixing. One end of the surfactant molecule is an oil-loving group that can effectively enter the oil inside; the other end is a water-soluble group with good solubility in water.

[0074] The oil-water mixed solution cooled copper crucible of the embodiment has its upper end face subjected to laser shot peening treatment, and the laser shot peening treatment is usually used as a strengthening means for finished products in the high-temperature alloy field and is applied in the smelting process of the high-temperature alloy, so that a large number of nanoscale micro recesses appear on the surface of the crucible. According to the solidification principle of the high-temperature alloy, the base of the recess interface has the strongest nucleation ability because the critical crystal nucleus volume required for solidification is the smallest, thereby greatly improving the nucleation rate of the high-temperature alloy.

[0075] The surface roughness of the oil-water mixed solution cooled copper crucible of the embodiment is increased after the laser shot peening treatment, and more non-uniform nucleation points are provided for the solidification of the high-temperature alloy, so that the nucleation process is more easily performed, and the nucleation rate of the high-temperature alloy is also effectively improved.

[0076] Specific implementation method seven: combination Figures 1 to 7 The preparation method of the embodiment is characterized in that it comprises the following steps:

[0077] Step one: inspection work;

[0078] The copper crucible body 41 is polished and cleaned with alcohol and sandpaper; it is observed whether there is smelting residual metal on the double-tungsten-electrode electrode 23, if there is, the double-tungsten-electrode electrode 23 is polished in time with an angle grinder and is replaced, the nut is removed, the double-tungsten-electrode electrode 23 is put into the nut, the middle hole positioning bolt is installed to connect the lifting rod and the double-tungsten-electrode electrode 23, and it is checked whether the oil-water mixed solution cooling system 14 is normal.

[0079] Step two: the high-temperature alloy elements with the prepared proportion are put into the oil-water mixed solution cooled copper smelting recess 15 with the nanoscale micro recesses on the upper end face subjected to the laser shot peening treatment, the position of the ingot turning ladle 11 with the modification agent releasing function is adjusted to be directly above the oil-water mixed solution cooled copper smelting recess 15 with the nanoscale micro recesses on the upper end face subjected to the laser shot peening treatment, and after the above-mentioned actions are completed, the furnace door is closed;

[0080] Step three: open the vacuum pumping device.

[0081] First, the air pumping mechanism 4 is opened, and the reading on the pressure gauge 2 is observed. When the vacuum degree in the electric arc furnace is 0.1 MPa, the air pumping mechanism 5 is closed, and the gas filling valve 7 is opened, so that the inert gas argon is filled into the furnace. The reading on the pressure gauge 2 is observed again, and the vacuum degree in the furnace is kept at 0.05 MPa.

[0082] Step four: control the left double-gun-head electric arc gun device 10 and the right double-gun-head electric arc gun device 9.

[0083] The rotating wheel disc 19 is rotated, and the left double-gun-head electric arc gun device 10 and the right double-gun-head electric arc gun device 9 are adjusted so that the center point of the line connecting the two gun heads of the double-tungsten-electrode electrode 23 is 1-2 mm above the high-temperature alloy raw material.

[0084] Step five: turn on the crucible temperature monitoring and real-time monitoring of the picture inside the furnace integration device 12;

[0085] After turning on, check whether the infrared thermometer display 30 is correct, and at the same time check whether the infrared high-definition optical fiber transmission camera 31 signal transmission is stable;

[0086] Step six: turn on the electric arc current control component and observe the infrared thermometer display in real time, and start the left double gun head arc gun device 10 and the right double gun head arc gun device 9 to make it arc. The operating angle of the left double gun head arc gun device 10 and the right double gun head arc gun device 9 is as shown in Figure 7 (b), that is, the cylindrical tungsten electrode part of the left double gun head arc gun device 10 and the right double gun head arc gun device 9 has a 45° angle relative to the vertical ground direction; the operating direction of the left double gun head arc gun device 10 and the right double gun head arc gun device 9 is Figure 7 (b), that is, the plane formed by the center point of the double gun head arc gun movement direction and the line connecting the two gun heads should always be perpendicular to the crucible plane; the movement sequence is that the left double gun head arc gun device 10 first makes a complete movement trajectory according to the predetermined direction, and then the right double gun head arc gun device 9 makes a complete movement trajectory according to the predetermined direction, and so on; the movement frequency is determined according to the metal liquid flow trend in the crucible, that is, after the left double gun head arc gun device 10 moves in the predetermined direction, it needs to wait for the completion of the forced convection of the metal liquid caused by it (after showing a circular arc metal liquid movement trajectory), and then the right double gun head arc gun device 9 is operated, and after the operation of the right double gun head arc gun device 9 is completed, it also needs to wait for the completion of the forced convection of the metal liquid caused by it (after showing a circular arc metal liquid movement trajectory), and then the left double gun head arc gun device 10 is operated, and so on. Gradually increase the electric arc current of the left double gun head arc gun device 10 and the right double gun head arc gun device 9. Until the infrared thermometer display reaches the melting point of the high-temperature alloy, immediately stop increasing the electric arc current. If the specific melting point of the alloy is not clear, the infrared thermometer display should not be higher than the melting point of the main element in the alloy composition to prevent overheating of the high-temperature alloy. Then maintain this electric arc current until the high-temperature alloy is completely melted;

[0087] Step seven: pull the pulling device 27 on both sides of the ingot turning spoon 11 with the function of releasing the modifier to release part of the modifier, and then return the double-sided pulling device 27 to its original position;

[0088] Step eight: observe the opening of the crucible temperature monitoring and real-time monitoring of the picture inside the furnace integration device 12;

[0089] Observe the infrared thermometer 30 display to room temperature, and the optical fiber transmission picture shows that the high-temperature alloy in the furnace has been solidified. At this time, use the ingot turning spoon 11 with the function of releasing the modifier to turn over the solidified high-temperature alloy ingot;

[0090] Step nine: repeat the operation of step six, step seven, step eight, so that the ingot is repeatedly remelted 5-10 times, the number of melting times is determined according to the alloy composition, thus, the preparation of the high-temperature alloy is completed.

[0091] Specific embodiment eight: in combination with Figure 1 , Figure 8 and Figure 9 This embodiment is described, and the proportioned high-temperature alloy elements in step two of this embodiment are Nb-16Si-20Ti high-temperature alloy. In this way, the alloy system of this embodiment covers high-temperature alloy, and the preferred high-temperature alloy composition is Nb-16Si-20Ti high-temperature alloy. Other compositions and connections are the same as any one of embodiments one to seven.

[0092] Specific embodiment nine: in combination with Figure 1 and Figure 6 This embodiment is described, and the copper crucible body 41 of this embodiment is made of T2 red copper material. Other compositions and connections are the same as embodiment one.

[0093] The application initiatively uses a unique double-gun-head arc gun design and a given arc gun operation angle, operation direction, operation sequence, and operation frequency to cooperate with each other to generate forced convection in the high-temperature alloy liquid, effectively reduces the composition segregation of the high-temperature alloy, and improves the nucleation rate of the high-temperature alloy by using the convection effect.

[0094] The application initiatively improves the structure of the commonly used ingot turning ladle in the prior art, so that the ingot turning ladle has the functions of the general ingot turning ladle and additionally has the functions of storing and releasing the modifier. The release of the modifier and the convection effect complement each other and promote each other, further improving the nucleation rate caused by the strong convection and the refining effect of the modifier.

[0095] The application initiatively sets an integrated device for monitoring the temperature of the crucible and real-time monitoring the picture in the furnace. The former effectively prevents a series of occurrences of the deterioration of the high-temperature alloy organization, such as overheating of the high-temperature alloy, reduction of the number of non-uniform nucleation cores, etc. The latter can monitor and record the solidification process in real time throughout the process, effectively improves the real-time control degree of the operator on the situation inside the vacuum arc furnace, and improves the quality of the high-temperature alloy obtained by melting. The real-time control degree of the operator on the situation inside the vacuum arc furnace is also improved, thereby reducing the melting cost of the high-temperature alloy. At the same time, the solidification process can be monitored and recorded throughout the process. Based on this, the entire solidification process can be objectively evaluated, which is convenient for finding problems and comparative discussion. When the entire detection system works together, that is, the temperature data and the melting picture of the high-temperature alloy in the furnace cooperate with each other, the control degree of the operator on the organization form of the high-temperature alloy is improved, and the problem of the overheating of the high-temperature alloy caused by the excessively large arc current to cause the coarse organization and the excessively low nucleation rate under the prior art is greatly improved.

[0096] The present application improves the prior art which generally uses a water cooling system, and utilizes oil-water mixture cooling to reduce the cooling speed of the crucible, and initiatively adjusts the proportion of the oil-water mixture: 24% of mineral oil, 73% of water, 1% of surfactant, 1% of cooling accelerator, and 1% of antioxidant; the prior art is mostly 1:10 or 1:15, and the present application increases the proportion of mineral oil, so that the supercooling degree of the high-temperature alloy liquid reaches the effective nucleation supercooling degree without being too much, thereby avoiding the ejection of solute during the columnar crystal growth process to reduce the nucleation rate of the high-temperature alloy.

[0097] The present application initiatively performs laser shot peening treatment on the upper end surface of the oil-water mixture cooled copper crucible, and applies the high-temperature alloy field as a finished product strengthening method in the smelting process of the high-temperature alloy, so that a large number of nanoscale micro recesses appear on the surface of the crucible, the nucleation rate of the high-temperature alloy is greatly improved, and the surface roughness is increased, so that the nucleation process is more easily performed.

[0098] Combining Figures 8 to 11 It is shown that the effect of the present application is exhibited. Figure 8 and Figure 9 By comparison: the microstructure of the Nb-16Si-20Ti high-temperature alloy prepared by using the prior art is coarse, is in a fishbone shape, the NbSS phase, the Nb3Si phase and the Nb5Si3 phase grains are relatively coarse, element segregation is serious, and the distribution of each phase is also uneven; and the microstructure of the Nb-16Si-20Ti high-temperature alloy prepared by the solidification equipment for preparing ultra-fine high-temperature alloy with multi-angle nucleation rate improvement is obviously refined, is mostly fine equiaxed crystal structure, and the distribution of each phase is very uniform.

[0099] By comparison: Figure 10 and Figure 11 It can be seen that the high-temperature compression yield strength and the room temperature fracture toughness of the Nb-16Si-20Ti high-temperature alloy prepared by using the present application are obviously improved, and the room temperature fracture toughness is increased by nearly 50%. Compared with the prior art, under the same composition, the tensile test is performed, Figure 12 and Figure 13The fracture photos of the Nb-Si based high-temperature alloy prepared by the application and the Nb-Si based high-temperature alloy prepared by the prior art are respectively shown in the figures, the Nb-Si based high-temperature alloy prepared by the application has obvious plastic deformation before fracture, the fracture morphology presents dark gray fibrous shape, and the fracture presents ductile fracture, while the Nb-Si based high-temperature alloy prepared by the prior art has not strong plastic deformation before fracture, and the fracture presents a small part of bright crystalline shape in addition to the dark gray fibrous shape; in terms of the fracture elongation, compared with the prior art, the same composition is increased by 45%; in terms of the tensile strength, compared with the prior art, the same composition is increased by 27%.

[0100] The application creates a solidification equipment and method for preparing ultra-fine high-temperature alloy with multi-angle promotion of nucleation rate based on the solidification principle of high-temperature alloy and solid theoretical basis, and the application points of the application have strong synergistic effect, and all the application points aim to improve the nucleation rate in the solidification process of high-temperature alloy, and excellent technical effect is achieved in the improvement of the nucleation rate of high-temperature alloy.

[0101] The above examples are only used to illustrate the technical solutions of the application, but not limit the application; although the application is described in detail with reference to the foregoing examples, those skilled in the art should understand that the technical solutions recorded in the foregoing examples can be modified, or some technical features can be replaced equivalently; and the modification or replacement does not make the essence of the corresponding technical solution deviate from the spirit and scope of the technical solutions of the embodiments of the application.

Claims

1. A solidification apparatus for preparing ultrafine high-temperature alloys by multi-angle enhancement of nucleation rate, characterized in that: It includes an arc current control cabinet (1), a pressure gauge (2), an arc current control line (3), a gas extraction device (4), a gas extraction mechanism (5), an argon tank (6), a gas filling valve (7), a sight glass (8), a right double-headed arc gun device (9), a left double-headed arc gun device (10), a tilting spoon with a modifier release function (11), an integrated device for crucible temperature monitoring and real-time monitoring of the furnace interior (12), a vacuum arc furnace (13), and an oil-water mixture cooling system (14). A sight glass (8) is installed on the upper part of the vacuum arc furnace (13). A pressure gauge (2) is installed on the upper surface of the vacuum arc furnace (13) through a pressure gauge seat. A tilting spoon (11) with a degrading agent release function is movably installed on the upper surface of the vacuum arc furnace (13). The tilting spoon (11) with a degrading agent release function realizes lifting operation, rotation operation and degrading agent release operation. An oil-water mixture cooling system (14) is installed inside the vacuum arc furnace (13) and cools the crucible by introducing an oil-water mixture. The right double-headed arc lance device (9) and the left double-headed arc lance device (10) are rotatably mounted on the upper surface of the empty arc furnace (13), and the lower parts of the right double-headed arc lance device (9) and the left double-headed arc lance device (10) extend into the vacuum arc furnace (13). The arc current control cabinet (1) is connected to the right double-headed arc lance device (9) and the left double-headed arc lance device (10) respectively through the arc current control line (3); crucible temperature monitoring and furnace drawing The integrated real-time monitoring device (12) is installed directly above the furnace body of the vacuum arc furnace (13); the viewing mirror (8) is located on the upper right side of the furnace body of the vacuum arc furnace (13); the vacuum pump (4) is connected to the vacuum arc furnace (13) through a pipe, and the vacuum furnace (13) is vacuumed through the vacuum pump mechanism (5) set on the pipe; the argon tank (6) is connected to the pipe, and the output pipe of the argon tank (6) is equipped with a filling valve (7); The tilting spoon (11) with the function of releasing the deteriorating agent includes a tilting spoon head (24), a cylindrical storage rod (25), a deteriorating agent (26), a double-sided pull-out device (27), and a control lever (28). The double-sided pull-out device (27) is installed on the left and right sides of the cylindrical storage rod (25) and extends downward close to the outer side wall of the cylindrical storage rod (25); the cylindrical storage rod (25) is sealed to the vacuum arc furnace (13) and extends into the vacuum arc furnace (13); the operating lever (28) is installed on the upper part of the cylindrical storage rod (25) and located outside the vacuum arc furnace (13); The oil-water mixture cooling system (14) includes smelting pits (15) with nanoscale micro-depressions treated by laser shot peening.

2. The solidification equipment for preparing ultrafine high-temperature alloys by multi-angle enhancement of nucleation rate according to claim 1, characterized in that: The vacuum electric arc furnace (13) includes a body, a furnace door (16) and a sealing gasket (17). The sealing gasket (17) is installed on the furnace door (16), and the furnace door (16) is openably connected to the body.

3. The solidification equipment for preparing ultrafine high-temperature alloys by multi-angle enhancement of nucleation rate according to claim 2, characterized in that: The right double-headed arc gun device (9) and the left double-headed arc gun device (10) have the same structure. The left double-headed arc gun device (10) includes a rotary disc (19), a bellows (20), a protective sleeve (21), a lifting rod (22), and a double tungsten electrode (23). The dual tungsten electrode (23) is installed on the lower part of the lifting rod (22) by positioning bolts. The protective sleeve (21) is fitted on the lifting rod (22). The upper part of the lifting rod (22) is equipped with a bellows (20). The support rod is installed on the upper part of the bellows (20). The turntable (19) is installed on the upper end of the support rod.

4. The solidification equipment for preparing ultrafine high-temperature alloys by multi-angle enhancement of nucleation rate according to claim 3, characterized in that: The integrated device for crucible temperature monitoring and real-time monitoring of the furnace interior (12) includes a threaded double cylindrical glass skylight (29), an infrared thermometer (30), a temperature display (38), an infrared high-definition fiber optic transmission camera (31), a transceiver I (32), a fiber optic signal transmission line (34), a fusion splice box (35), a transceiver II (33), a switch (36), and a hard disk recorder (37). The infrared thermometer (30) is connected to the threaded double cylindrical glass skylight (29) at the top of the vacuum electric arc furnace (13) by a thread. The infrared thermometer (30) is connected to the temperature display (38). The infrared high-definition fiber optic transmission camera (31) is located to the right of the infrared thermometer (30) and is connected to the threaded double cylindrical glass skylight (29) by a thread. The measured real-time image data is transmitted to transceiver one (32) through fiber optic signal transmission line (34). The data is then transmitted sequentially through the fusion splice box (35), transceiver two (33), switch (36), and hard disk recorder (37) that are electrically connected to each other.

5. The solidification equipment for preparing ultrafine high-temperature alloys by multi-angle enhancement of nucleation rate according to claim 4, characterized in that: The oil-water mixture cooling system (14) also includes a copper crucible body (41), a copper outer shell (42), a copper base (40), an oil-water mixture inlet pipe (43), an oil-water mixture outlet pipe (44), an oil-water mixture inlet pipe (45), an oil-water mixture outlet pipe (46), an oil-water mixture inlet and outlet plate (47), and an oil-water mixture outlet plate (48). A copper base (40) is installed inside a vacuum electric arc furnace (13). A smelting pit (15) with nanoscale micro-depressions, which has been treated by laser shot peening, is installed on the copper base (40) and located inside the copper shell (42). The upper part of the oil-water mixture inlet pipe (43) and the oil-water mixture outlet pipe (44) are pipe openings that are tilted to one side. The oil-water mixture inlet pipe (43) and the oil-water mixture outlet pipe (44) are both installed vertically inside the oil-water mixture cooling copper crucible body (41). One end of the oil-water mixture inlet pipe (45) and the oil-water mixture outlet pipe (46) are respectively inserted into the oil-water mixture inlet pipe (43) and the oil-water mixture outlet pipe (44). The other end of the oil-water mixture inlet pipe (45) and the oil-water mixture outlet pipe (46) are respectively connected to the oil-water mixture inlet / outlet plate (47) and the oil-water mixture outlet / outlet plate (48).

6. A method for preparing a solidification apparatus for preparing ultrafine high-temperature alloys using a multi-angle enhancement nucleation rate method as described in claim 5, characterized in that: It includes the following steps: Step 1: Inspection work; Use alcohol and sandpaper to polish and clean the copper crucible body (41); Observe the double tungsten electrode (23) to see if there is any residual metal from smelting. If so, grind the double tungsten electrode (23) with an angle grinder and replace it. Remove the nut and put the double tungsten electrode (23) into it. Install the center hole positioning bolt to connect the lifting rod and the double tungsten electrode (23). At the same time, check whether the oil-water mixture cooling system (14) is normal. Step 2: Place the high-temperature alloying elements in the correct proportion into the cold copper smelting pit (15) of the oil-water mixture with nano-scale micro-depressions on the upper surface, which has been treated by laser shot peening. Adjust the position of the ingot-turning spoon (11) with the modifier release function to be directly above the cold copper smelting pit (15) of the oil-water mixture with nano-scale micro-depressions on the upper surface, which has been treated by laser shot peening. After completing the above actions, close the furnace door. Step 3: Turn on the vacuum pump; First, turn on the evacuation mechanism (5) and observe the reading on the pressure gauge (2). When the vacuum degree in the electric arc furnace is 0.1 MPa, turn off the evacuation mechanism (5) and open the charging valve (7) at the same time to allow the inert gas argon to be charged into the furnace. Observe the reading on the pressure gauge (2) again to keep the vacuum degree in the furnace at 0.05 MPa. Step 4: Operate the left double-headed arc gun device (10) and the right double-headed arc gun device (9). Rotate the rotary wheel (19) and adjust the left double-headed arc gun device (10) and the right double-headed arc gun device (9) so that the center point of the line connecting the two heads of the double tungsten electrode (23) is 1-2 mm above the high-temperature alloy material. Step 5: Turn on the integrated device for crucible temperature monitoring and real-time monitoring of the furnace interior (12). After turning it on, check whether the display of the infrared thermometer (30) is correct, and at the same time check whether the signal transmission of the infrared high-definition fiber optic transmission camera (31) is stable. Step 6: Turn on the arc current control component and observe the reading of the infrared thermometer in real time. At the same time, start the operation of the left double-headed arc gun device (10) and the right double-headed arc gun device (9) to make it start the arc. The operating angles of the left double-headed arc gun device (10) and the right double-headed arc gun device (9) are as follows: the double tungsten electrodes (23) of the left double-headed arc gun device (10) and the right double-headed arc gun device (9) form an angle of 45° with respect to the direction perpendicular to the ground. The operating directions of the left double-headed arc gun device (10) and the right double-headed arc gun device (9) are: passing through the center of gravity of the copper crucible body (41) and the plane formed by the direction of movement of the double-headed arc gun and the center point of the line connecting the two gun heads must always be perpendicular to the plane of the copper crucible body (41). The sequence of motion is as follows: the left double-headed arc gun device (10) first makes a complete motion trajectory in the predetermined direction, and then the right double-headed arc gun device (9) makes a complete motion trajectory in the predetermined direction, and so on. Stop increasing the arc current as soon as the reading of the infrared thermometer (30) reaches the melting point of the high-temperature alloy. If the specific melting point of the alloy is not known, the reading of the infrared thermometer (30) must not be higher than the melting point of the main component in the alloy composition. Then maintain this arc current until the high-temperature alloy is completely melted. Step 7: Pull the pull devices (27) on both sides of the flipping spoon (11) with the function of releasing the deteriorating agent, so that the deteriorating agent is partially released and then returned to the pull devices (27) on both sides after partial release. Step 8: Observe and turn on the integrated device for real-time monitoring of crucible temperature and furnace interior (12). Observe the reading of the infrared thermometer (30) until the room temperature, and at the same time, the fiber optic transmission screen shows that the high-temperature alloy in the furnace has solidified. At this time, use the ingot flipping spoon (11) with the function of releasing modifier to flip the solidified high-temperature alloy ingot. Step Nine: Repeat steps Six, Seven, and Eight to remelt the ingot 5-10 times. The number of remelting times depends on the alloy composition. This completes the preparation of the high-temperature alloy.

7. The preparation method according to claim 6, characterized in that: The high-temperature alloying elements prepared in step two are Nb-16Si-20Ti high-temperature alloy.

8. The preparation method according to claim 7, characterized in that: The copper crucible body (41) is made of T2 copper.

Images