A metal single crystal ingot preparation device

Abstract

The present application relates to the field of metal single crystal preparation device, in particular to a kind of fast preparation metal single crystal ingot device.The device is mainly composed of vacuum furnace, heating and heat preservation system, large-size single crystal seed preparation system, crucible outer wall heat preservation and air cooling system, single crystal ingot traction system.Its special feature is that first, large-size single crystal seed is prepared by hot continuous casting method;Then, single crystal seed grows freely in inverted conical crucible, gradually expands single crystal radius, until the inner diameter of cylindrical crucible, completes the transformation from single crystal seed to single crystal ingot;Because the diameter of single crystal seed is larger, the heat conduction capacity is significantly enhanced, combined with the auxiliary role of air cooling system cooling of crucible outer wall removed from induction coil, the rapid growth of single crystal ingot is realized.

Description

Technical Field

[0001] This invention relates to the field of metal single crystal preparation apparatus, and more specifically to an apparatus for rapidly preparing metal single crystal ingots. Background Technology

[0002] There are many methods for preparing single crystals. For metals, there are two main methods: the traditional directional solidification method and the OCC method developed by Atsumi Ohno in Japan. The traditional directional solidification method involves pouring molten metal into a mold, where it solidifies directionally within an "S"-shaped seed crystal preparation chamber at the bottom of the mold. During cellular crystal growth within the "S"-shaped seed crystal preparation chamber, individual cellular crystals are eliminated until only one remains in the mold; this single cellular crystal is the prepared seed crystal. The seed crystal continues to grow under a positive temperature gradient, eventually yielding a single crystal ingot. The disadvantage of the traditional directional solidification method is its slow single crystal growth rate. This is because heat is primarily dissipated through the "S"-shaped metal or alloy formed at the bottom, resulting in slow heat dissipation and a slower single crystal growth rate.

[0003] The OCC method for preparing single crystals involves the liquid metal contacting the end of the ingot guide rod, forming a layer of fine equiaxed crystals at the rod's end. When the crystal growth direction is controlled by heat flow, the equiaxed crystals grow in a direction parallel to and opposite to the heat flow, forming cellular crystals. When the solid-liquid interface bulges towards the molten metal, some of the cellular crystals contact the mold wall of the single crystal seed crystallizer and stop growing, leaving only one peritectic crystal within the cast billet to continue growing forward, forming a single crystal. The OCC method allows for arbitrary adjustment of the billet length, potentially reaching infinite lengths, while also providing a relatively fast single crystal growth rate. However, during continuous casting, the heat generated during single crystal growth is primarily dissipated by the ingot guide rod, resulting in a slower growth rate. Furthermore, in the OCC method, the solid-liquid interface is located outside the single crystal seed crystallizer; even slight fluctuations can cause "fire runaway," leading to continuous casting failure. Summary of the Invention

[0004] In view of this, the present invention discloses a metal single crystal ingot preparation apparatus, the specific scheme of which is as follows:

[0005] A metal single crystal ingot preparation apparatus includes a vacuum furnace system, a heating and heat preservation system, a single crystal seed preparation system, a water spray system, and an ingot guide rod;

[0006] The vacuum furnace system includes a vacuum furnace, and a heating and insulation system is disposed inside the vacuum furnace. The heating and insulation system includes a first insulation sleeve, an induction coil, and a crucible. The first insulation sleeve has a cylindrical structure and an insulation cover is provided on the top of the first insulation sleeve. The induction coil is disposed outside the first insulation sleeve. The crucible is disposed inside the first insulation sleeve and has a receiving chamber inside. The receiving chamber inside the crucible includes an insulation part and a single crystal ingot generation part. The insulation part is located above the single crystal ingot generation part and has a cylindrical structure. The single crystal ingot generation part has an inverted conical structure. The lower end of the crucible has an opening communicating with the single crystal ingot generation part.

[0007] The single crystal seed preparation system includes a single crystal seed crystallizer, a first thermocouple, and a second thermocouple. The single crystal seed crystallizer is located below the crucible, and its upper end is connected to the lower opening of the crucible. The first thermocouple is located above the second thermocouple, and the temperature measuring ends of the two thermocouples are located inside the side wall of the single crystal seed crystallizer. The ingot guide rod is located below the single crystal seed crystallizer, and its axis is on the same straight line as the axis of the single crystal seed crystallizer.

[0008] The water spraying system includes a sprayer, which is disposed on the outer periphery of the ingot guide rod and is used to spray cooling water onto the ingot guide rod.

[0009] As a supplement to the technical solution of the present invention, the single crystal seed crystal preparation system further includes a crystallizer sleeve, which is sleeved on the outside of the single crystal seed crystallizer. The first thermocouple and the second thermocouple are both installed on the crystallizer sleeve. Both thermocouples penetrate the side wall of the crystallizer sleeve, and their temperature measuring ends are located inside the side wall of the single crystal seed crystallizer.

[0010] As a supplement to the technical solution of the present invention, a single crystal seed traction mechanism is also included, which is disposed below the vacuum furnace, and the lower end of the ingot guide rod passes through the lower bottom wall of the vacuum furnace and is connected to the single crystal seed traction mechanism; the single crystal seed traction mechanism includes a first motor, a first reducer, a first lead screw, a first guide column, and an ingot guide rod support plate;

[0011] The lower end of the ingot guide rod is connected to the ingot guide rod support plate. The ingot guide rod support plate is provided with a threaded hole. The first lead screw is screwed into the threaded hole on the ingot guide rod support plate. A single crystal ingot traction mechanism is provided below the ingot guide rod support plate. The single crystal ingot traction mechanism includes a support base plate. The first motor and the first reducer are both set on the support base plate. The first motor is connected to the first lead screw through the first reducer and drives the lead screw to rotate, causing the ingot guide rod support plate to rise or fall, thereby driving the ingot guide rod to rise or fall. The first guide post is set on the ingot guide rod support plate. The support base plate is provided with a guide through hole for the first guide post to pass through. The lower part of the first guide post passes through the guide through hole on the support base plate.

[0012] As a supplement to the technical solution of the present invention, the single crystal seed crystal traction mechanism further includes a centering device, which is disposed on the ingot guide rod support plate. The centering device includes a drill chuck and a centering screw. The drill chuck includes a columnar part and a conical part, with the conical part disposed on the lower side of the columnar part. Both are hollow shell structures. The lower part of the ingot guide rod passes through the conical part from top to bottom and is placed inside the columnar part. The side wall of the columnar part is provided with a threaded hole for the centering screw to pass through. The centering screw is screwed into the threaded hole of the columnar part. The centering screw is provided in at least three sets, and each centering screw is uniformly arrayed along the circumference of the columnar part.

[0013] As a supplement to the technical solution of the present invention, the single crystal ingot traction mechanism further includes a second motor, a second reducer, a second lead screw, a third guide column, an ingot guide rod locking mechanism, a guide bracket, and a base plate;

[0014] The guide bracket is installed inside the vacuum furnace and includes a guide plate and a second guide column. The guide plate is located below the sprayer.

[0015] The upper end of the sprayer abuts against the bottom of the crucible, and the lower end of the sprayer abuts against the guide plate. The guide plate has a through hole for the ingot guide rod to pass through, and the upper end of the ingot guide rod passes through the guide plate and is located above the guide plate. The guide plate has a second guide post, which is vertically arranged. The lower bottom wall of the vacuum furnace has a guide through hole through which the second guide post passes, and the lower part of the second guide post passes through the guide through hole on the lower bottom wall of the vacuum furnace to provide guidance for the lifting and lowering movement of the guide bracket.

[0016] The ingot guide rod locking mechanism includes a locking screw. The guide plate is provided with a threaded through hole extending from one end of the guide plate toward the ingot guide rod. The threaded through hole is connected to a through hole on the guide plate for the ingot guide rod to pass through. The locking screw is screwed into the threaded through hole. Tightening the locking screw so that its end presses against the ingot guide rod can lock the ingot guide rod onto the guide plate.

[0017] The support base plate is provided with threaded holes, and the base plate is located below the support base plate. The second lead screw is screwed to the threaded holes on the support base plate. The second motor is connected to the second lead screw through the second reducer, driving the second lead screw to rotate and causing the support base plate to move up and down. The second motor and the second reducer are both mounted on the base plate. The third guide post is mounted on the support base plate, and the base plate is provided with a guide through hole for the third guide post to pass through. The lower part of the third guide post passes through the through hole on the base plate to provide guidance for the lifting and lowering of the support base plate.

[0018] As a supplement to the technical solution of the present invention, it also includes an air-cooling system, which includes an argon cooler, an air cooler, a gas transmission pipe, a gas collection pipe, and a second insulation jacket.

[0019] The second insulation sleeve is located below the first insulation sleeve, and the upper end of the second insulation sleeve abuts against the lower end of the first insulation sleeve. An air cooler is provided on the lower side of the second insulation sleeve. The argon gas cooler is located outside the vacuum furnace. The argon gas cooler is connected to the air cooler through a gas supply pipe. One end of the gas collecting pipe is connected to the argon gas cooler, and the other end is located inside the vacuum furnace.

[0020] As a supplement to the technical solution of the present invention, the spraying system also includes a cooler, a water supply pipe, and a return water pipe;

[0021] The cooler is located outside the vacuum furnace;

[0022] The sprayer includes an inner shell, an outer shell, a top plate, a bottom plate, and a sealing gasket. The outer shell is a tubular structure, with the bottom plate located at the lower end and the top plate at the upper end. Both the bottom and top plates have through holes for the guide rod to pass through. The inner shell is located inside the outer shell, and its upper and lower ends are sealed to the inner wall of the outer shell, forming a water-receiving chamber between them. Spray holes are provided on the inner wall of the inner shell, and one end of a water supply pipe is connected to the water-receiving chamber, while the other end is connected to a cooler.

[0023] The outer shell located below the inner shell and the bottom plate together form a water receiving trough. One end of the return water pipe is connected to the water receiving trough, and the other end is connected to the cooler. The sealing gasket is installed on the bottom of the bottom plate, and a ring-shaped protrusion structure is provided in the central area. The ring-shaped protrusion structure is embedded in the through hole of the bottom plate to fill the gap between the edge of the through hole of the bottom plate and the guide rod.

[0024] As a supplement to the technical solution of the present invention, the heating and heat preservation system further includes an insulation pad, which is disposed at the bottom end of the crucible and located between the crucible and the sprayer.

[0025] As a supplement to the technical solution of the present invention, the spraying system further includes a heat-resistant rubber pad and a pressure plate; the pressure plate is disposed below the heat-resistant rubber pad, and the heat-resistant rubber pad is disposed below the pressure plate, and the heat-resistant rubber pad is in contact with the top plate of the sprayer; the heat-resistant rubber pad has a through hole in the middle for the ingot guide rod to pass through, and the diameter of the through hole in the middle of the heat-resistant rubber pad is smaller than the diameter of the ingot guide rod.

[0026] As a supplement to the technical solution of the present invention, the cone angle of the single crystal ingot generating part of the crucible is 45°~60°.

[0027] This invention utilizes the longitudinal temperature distribution within the single-crystal seed crystallizer to control the outlet temperature below the melting point of the alloy or metal, and the inlet temperature above it, thus creating a temperature gradient from bottom to top within the crystallizer. This temperature gradient causes the solid-liquid interface to shift within the crystallizer, completely resolving the "fire run" phenomenon during OCC continuous casting and successfully producing copper single-crystal rods with a diameter of 20 mm.

[0028] Combining the OCC method with traditional single-crystal ingot preparation methods, this patent applicant proposes a method for preparing a seed crystal within a heated single-crystal seed crystallizer using the OCC method, and then forming a single-crystal ingot within a mold. Because the single-crystal seed crystal has a relatively large diameter and a large heat dissipation area, heat transfer within the mold can be accelerated, thereby speeding up single-crystal growth. Once the single crystal reaches the mold size, auxiliary cooling can be applied to the outside of the mold to further accelerate the single-crystal growth rate.

[0029] In summary, there is an urgent need for a device that can efficiently and precisely control parameters and rapidly prepare large-size metal single crystals to solve the existing technical challenges.

[0030] Beneficial effects:

[0031] 1. The insulation system integrates metal melting and melt temperature control, saving the need for a separate melting furnace and casting process. The insulation around the crucible ensures unidirectional heat transfer quality during seed crystal and single crystal growth.

[0032] 2. The large-size single crystal seed preparation system breaks through the bottleneck of the traditional single crystal seed diameter being very small, and can prepare copper single crystal seed crystals with a diameter of not less than 20mm, providing favorable conditions for the rapid growth of subsequent single crystal ingots.

[0033] 3. After the crucible is removed from the induction coil, the air-cooling system ensures unidirectional heat transfer while accelerating the heat dissipation from the side and below, thus assisting in the rapid growth of single crystal ingots.

[0034] 4. The operation of evacuating and then purging with argon gas can ensure the protection against cooling water leakage and the cleanliness of the melt.

[0035] 5. The cooling water inside the vacuum tank is elastically sealed by a heat-resistant rubber gasket, which ensures that the cooling water will not seep into the vacuum tank when the derrick or guide rod slides relative to it. Attached Figure Description

[0036] Figure 1 This is a three-dimensional structural diagram of the present invention.

[0037] Figure 2 This is a schematic diagram of the heating and heat preservation system of the present invention.

[0038] Figure 3 This is a schematic diagram of the water spray system structure of the present invention.

[0039] Figure 4 This is a schematic diagram of the sprayer structure of the present invention.

[0040] Figure 5 This is a schematic diagram of the sprayer and crucible structure of the present invention.

[0041] Figure 6 This is a schematic diagram of the sealing gasket structure of the present invention.

[0042] Figure 7 This is a schematic diagram of the single crystal seed crystal traction mechanism and the single crystal ingot traction mechanism of the present invention.

[0043] Figure 8 This is a schematic diagram of the guide bracket structure of the present invention.

[0044] Figure 9 This is a schematic diagram of the centering device structure of the present invention.

[0045] Figure 10 This is a top view schematic diagram of the drill chuck structure of the present invention.

[0046] Figure 11 This is a schematic diagram of the air-cooling system structure of the present invention.

[0047] In the diagram: 1. Vacuum furnace, 2. Heating and insulation system, 3. First insulation jacket, 4. Induction coil, 5. Crucible, 6. Insulation section, 7. Single crystal ingot generation section, 8. Single crystal seed crystallizer, 9. First thermocouple, 10. Second thermocouple, 11. Sprayer, 12. Ingot guide rod, 13. Ingot guide rod support plate, 14. First guide post, 15. Centering device, 16. Drill chuck, 17. Centering screw, 18. Columnar section, 19. Conical section, 20. Support base plate, 21. Second guide post, 22. Third guide post, 23. Guide bracket, 24. Locking screw 25. Base plate; 26. Argon cooler; 27. Air cooler; 28. Gas supply pipe; 29. ​​Gas collection pipe; 30. Second insulation sleeve; 31. Cooler; 32. Water supply pipe; 33. Water return pipe; 34. Inner shell; 35. Outer shell; 36. Top plate; 37. Bottom plate; 38. Sealing gasket; 39. Water receiving chamber; 40. Water receiving tank; 41. Insulation pad; 42. Heat-resistant gasket; 43. Pressure plate; 44. Air cooling system; 45. Insulation cover; 46. Crystallizer sleeve; 47. Guide rod; 48. Spray hole; 49. Guide support plate; 50. Positioning clamping bolt. Detailed Implementation

[0048] In the description of this invention, it should be understood that the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0049] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection, an electrical connection, or a connection that allows communication between them; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0050] like Figures 1 to 11 The present invention discloses a metal single crystal ingot preparation apparatus for preparing metal single crystal ingots, comprising a vacuum furnace system, a single crystal seed preparation system, a heating and heat preservation system 2, a water spraying system, and an ingot guide rod 12.

[0051] The vacuum furnace system includes a vacuum furnace 1, and the heating and insulation system 2 is installed inside the vacuum furnace.

[0052] The heating and heat preservation system 2 includes a first heat preservation sleeve 3, an induction coil 4, and a crucible 5.

[0053] The first insulation sleeve 3 is a cylindrical structure with an internal receiving space. An insulation cover 45 is located on the top of the first insulation sleeve 3. The induction coil 4 is fitted around the first insulation sleeve 3 for heating it. The crucible 5 is located inside the first insulation sleeve 3. The crucible 5 is a cylindrical structure with an internal receiving chamber. The receiving chamber includes an insulation section 6 and a single crystal ingot forming section 7. The insulation section 6 is located above the single crystal ingot forming section 7 and is cylindrical. The single crystal ingot forming section 7 is an inverted conical structure. The upper diameter of the single crystal ingot forming section 7 is the same as the diameter of the insulation section 6. The lower end of the crucible 5 has an opening communicating with the single crystal ingot forming section 7, allowing the molten metal to flow into the single crystal seed crystallizer 8 through this opening.

[0054] The single crystal ingot generation section 7 is used for the transition growth from single crystal seed crystal to single crystal.

[0055] The single crystal seed preparation system includes a single crystal seed crystallizer 8, a crystallizer sleeve 46, a first thermocouple 9, and a second thermocouple 10. The single crystal seed crystallizer 8 is positioned below the crucible 5, with its upper end connected to the lower opening of the crucible 5. The single crystal seed crystallizer 8 has a columnar structure and is integrally formed with the crucible 5.

[0056] The crystallizer sleeve 46 is fitted around the outside of the single crystal seed crystallizer 8 to insulate the crystallizer. Both the first thermocouple 9 and the second thermocouple 10 are mounted on the crystallizer sleeve 46. Both thermocouples penetrate the side wall of the crystallizer sleeve 46, with their measuring ends extending into the interior of the side wall of the single crystal seed crystallizer 8. The first thermocouple 9 is located above the second thermocouple 10. The first thermocouple 9 is used to monitor the temperature of the upper part of the single crystal seed crystallizer 8, and the second thermocouple 10 is used to monitor the temperature of the lower part of the single crystal seed crystallizer 8.

[0057] The ingot guide rod 12 is located below the single crystal seed crystallizer 8. The upper end of the ingot guide rod 12 is used to insert into the single crystal seed crystallizer 8 for ingot introduction.

[0058] The water spraying system includes a sprayer 11, which is disposed on the outer periphery of the ingot guide rod 12 and is used to spray cooling water onto the ingot guide rod 12.

[0059] With the above setup, during preparation, the metal raw material is placed in crucible 5, and the vacuum system is activated to evacuate the vacuum furnace 1. After reaching the predetermined vacuum level, the induction coil 4 is activated to melt the metal raw material in crucible 5 and maintain it at a set temperature range. This stabilizes the temperature of the molten metal in crucible 5 and the temperature gradient of the crystallizer sidewall within the set temperature range. Argon gas is pumped into the furnace, and once the set pressure is reached, the water spray system is activated to spray cooling water onto the ingot guide rod 12 to cool it down. The cooling energy is then transferred through the ingot guide rod 12 to the single crystal seed crystallizer 8, ensuring a temperature gradient within the single crystal seed crystallizer 8. This achieves the goal of controlling the crystallizer outlet temperature below the melting point of the alloy or metal and the inlet temperature of the single crystal seed crystallizer 8 above the melting point of the alloy or metal, thus creating a bottom-up temperature gradient within the single crystal seed crystallizer 8. Subsequently, the ingot guide rod 12 is slowly pulled downwards, causing the molten metal to gradually solidify within the single crystal seed crystallizer 8 using the single crystal seed as a substrate, thereby producing a single crystal seed.

[0060] By controlling the temperature gradient within the crystallizer, the solid-liquid interface is transferred to the single-crystal seed crystallizer 8, completely solving the "fire run" phenomenon during OCC continuous casting. By first preparing a single-crystal seed crystal, and then allowing it to grow freely into the inverted conical single-crystal ingot generation section 7, gradually increasing the single-crystal radius until reaching the heat-insulating section 6 within the crucible 5, the transformation from single-crystal seed crystal to single-crystal ingot is completed. Due to the larger diameter of the single-crystal seed crystal, its thermal conductivity is significantly enhanced, enabling rapid growth of the single-crystal ingot. In the above technical solution, the design of the single-crystal ingot generation section 7 can significantly increase the overall diameter of the single-crystal ingot.

[0061] As a supplement to the above technical solution, the cone angle of the single crystal ingot generation section 7 is 45°~60°, specifically the angle between the side wall of the crucible 5 at the location of the single crystal ingot generation section 7 and the horizontal plane. When the cone angle is less than 45°, it is easy to cause a large transition from single crystal seed to single crystal preparation, resulting in the formation of multiple seed crystals, which ultimately affects the preparation of single crystal ingots. When the cone angle is greater than 60°, under the condition of a fixed heat preservation section 6 of the crucible 5, it will cause the height of the entire single crystal ingot generation section 7 to increase, reducing production efficiency.

[0062] As a preferred embodiment of the present invention, a single crystal seed traction mechanism is also included, which is disposed below the vacuum furnace 1. The lower end of the ingot guide rod 12 passes through the lower bottom wall of the vacuum furnace 1 and is connected to the single crystal seed traction mechanism. The single crystal seed traction mechanism includes a first motor, a first reducer, a first lead screw, a first guide column 14, and an ingot guide rod support plate 13 (the first motor, the first reducer, and the first lead screw are not shown in the figure). The lower end of the ingot guide rod 12 is connected to the ingot guide rod support plate 13. The ingot guide rod support plate 13 is provided with a threaded hole. The first lead screw is screwed into the threaded hole on the ingot guide rod support plate 13. The rotation of the first lead screw drives the ingot guide rod support plate 13 to drive the ingot guide rod 12 to move up and down. A single-crystal ingot traction mechanism is located below the ingot guide rod support plate 13. This mechanism includes a support base plate 20, which is positioned below the ingot guide rod support plate 13. A first motor and a first reducer are both mounted on the support base plate 20, and the first motor is connected to a first lead screw via the first reducer, driving the lead screw to rotate. A first guide post 14 is mounted on the ingot guide rod support plate 13, and the support base plate 20 has a guide hole through which the first guide post 14 passes. The first guide post 14 guides the lifting and lowering movement of the ingot guide rod support plate 13. The ingot guide rod 12 is raised and lowered via the single-crystal seed traction mechanism. Lowering the ingot guide rod 12 accelerates the formation of the single-crystal seed, improving production efficiency.

[0063] Preferably, the ingot guide rod 12 includes an ingot guide rod and a guide rod 47. The ingot guide rod is disposed at the upper end of the guide rod 47. The ingot guide rod is used to guide the ingot, and the guide rod 47 is used to connect with the single crystal seed crystal traction mechanism. The ingot guide rod is driven to rise and fall accordingly by the raising and lowering of the guide rod 47.

[0064] As a preferred technical solution of the present invention, the single crystal seed crystal traction mechanism further includes a centering device 15, which is disposed on the ingot guide rod support plate 13. The centering device 15 includes a drill chuck 16 and a centering screw 17. The drill chuck 16 includes a columnar part 18 and a conical part 19. The conical part 19 is disposed on the lower side of the columnar part 18. Both are hollow shell structures. The lower part of the ingot guide rod 12 passes through the conical part 19 from top to bottom and is located inside the columnar part 18. The side wall of the columnar part 18 is provided with a threaded hole through which the centering screw 17 passes. The centering screw 17 is screwed into the threaded hole of the columnar part 18. There are at least three sets of centering screws 17, and each centering screw 17 is uniformly arrayed along the circumference of the columnar part 18. By tightening and adjusting each centering screw 17, the position of the ingot guide rod 12 is adjusted so that the axis of the ingot guide rod 12 is on the same vertical line as the axis of the single crystal seed crystallizer 8. After the centering of the ingot guide rod 12 is completed, the lower part of the ingot guide rod 12 is fixed on the ingot guide rod support plate 13.

[0065] The ingot guide rod support plate 13 is provided with an annular base. The annular base is provided with a groove for the lower end of the ingot guide rod 12 to be inserted. The side wall of the annular base is provided with a screw hole. The positioning clamping bolt 50 is screwed into the screw hole on the annular base so that the end of the positioning clamping bolt 50 presses against the ingot guide rod 12, and the lower end of the ingot guide rod 12 is fixed in the annular base.

[0066] As a preferred embodiment of the present invention, the single crystal ingot traction mechanism further includes a second motor, a second reducer, a second lead screw, a third guide column 22, an ingot guide rod locking mechanism, a guide bracket 23, and a base plate 25. (The second motor, the second reducer, and the second lead screw are not shown in the figure).

[0067] The guide bracket 23 is disposed inside the vacuum furnace 1 and includes a guide plate 49 and a second guide column 21. The guide plate 49 is located below the sprayer 11 and is used to support the sprayer 11. The guide plate 49 is provided with a through hole for the ingot guide rod 12 to pass through. The guide plate 49 is provided with a second guide column 21, which is vertically arranged. The bottom wall of the vacuum furnace 1 is provided with a guide through hole through which the second guide column 21 passes. The second guide column 21 passes through the guide through hole on the bottom wall of the vacuum furnace 1 to provide guidance for the lifting and lowering movement of the guide bracket 23.

[0068] The ingot guide rod locking mechanism is used to lock the ingot guide rod 12 onto the guide bracket 23. It includes a locking screw 24. The guide plate 49 is provided with a threaded through hole from one end of the guide plate 49 toward the ingot guide rod 12. The threaded through hole is connected to the through hole on the guide plate 49 through which the ingot guide rod 12 passes. The locking screw 24 is screwed into the threaded through hole. By tightening the locking screw 24, the ingot guide rod 12 can be locked onto the guide plate 49, so that when the ingot guide rod 12 moves downward, it drives the guide bracket 23 to move downward together.

[0069] The locking screw 24 can be rotated by a motor via gear transmission or by direct drive, thereby enabling the locking screw 24 to rotate the guide rod 12.

[0070] The support base plate 20 has threaded holes, and the base plate 25 is located below the support base plate 20. The second lead screw is screwed into the threaded holes on the support base plate 20, and the second motor is connected to the second lead screw via a second reducer. Both the second motor and the second reducer are mounted on the base plate 25. The rotation of the second motor drives the second lead screw to rotate, thereby driving the lifting and lowering of the support base plate 20. The third guide post 22 is mounted on the support base plate 20, and the base plate 25 has guide holes for the third guide post 22 to pass through. The third guide post 22 provides guidance for the lifting and lowering movement of the support base plate 20.

[0071] After the preparation of the single crystal seed is completed, the ingot guide rod 12 is locked onto the guide bracket 23 by the ingot guide rod locking mechanism. At this time, the first motor is turned off to prevent it from rotating by self-locking. The second motor is turned on to drive the support base plate 20 to descend. At this time, the support base plate 20 can drive the ingot guide rod support plate 13 to descend together, so that the ingot guide rod 12 drives the guide bracket 23 to move down. Through the guide bracket 23, the sprayer 11 and the crucible 5 are driven down together, so that the lower part of the crucible 5 is moved out of the first heat insulation sleeve 3 first, while the crucible 5 inside the first heat insulation sleeve 3 is still in the heating state of the induction coil 4, so that the crucible 5 forms a temperature gradient from bottom to top, thus completing the preparation of the single crystal.

[0072] As a preferred embodiment of the present invention, the spraying system includes a sprayer 11, a cooler 31, a water supply pipe 32, and a return water pipe 33. The cooler 31 is located outside the vacuum furnace 1. The cooler 31 is connected to the sprayer 11 through the water supply pipe 32, which delivers cooling water to the sprayer 11. The sprayer 11 sprays the cooling water onto the surface of the ingot guide rod 12 to cool the ingot guide rod 12. Then, the sprayer 11 recovers the cooling water and delivers it back to the cooler 31 through the return water pipe 33, completing the water circulation.

[0073] The sprayer 11 includes an inner shell 34, an outer shell 35, a top plate 36, a bottom plate 37, and a sealing gasket 38.

[0074] The outer shell 35 is a tubular structure, with a bottom plate 37 located at the lower end and a top plate 36 located at the upper end. Both the bottom plate 37 and the top plate 36 have through holes for the guide rod 12 to pass through. The inner shell 34 is located inside the outer shell 35, with its upper and lower ends sealed to the inner wall of the outer shell 35, forming a water-receiving chamber 39 between them. Spray holes 48 are provided on the inner wall of the inner shell 34, and a water supply pipe 32 communicates with the water-receiving chamber 39. Cooling water supplied by the water supply pipe 32 enters the water-receiving chamber 39 and is sprayed onto the surface of the guide rod 12 through the spray holes 48. The water supply pipe 32 is connected to the water receiving chamber 39 at the lower part of the water receiving chamber 39. It can ensure that the spray holes 48 opened on the inner side wall of the inner shell 34 can spray cooling water through water pressure control, so as to ensure the cooling effect of the ingot guide rod 12.

[0075] Preferably, the upper end of the inner shell 34 is sealed to the top plate 36, so that a water-containing chamber 39 is formed between the inner shell 34, the top plate 36 and the outer shell 35.

[0076] The outer shell 35, located below the inner shell 34, forms a water collection tank 40 with the base plate 37. The water collection tank 40 collects the cooling water sprayed onto the surface of the ingot guide rod 12. The return water pipe 33 is connected to the water collection tank 40, and the water in the water collection tank 40 flows back to the cooler 31 through the return water pipe 33. The sealing gasket 38 is installed at the bottom of the base plate 37, and its central area has an annular protrusion structure. This annular protrusion structure is embedded in the through hole of the base plate 37 to fill the gap between the edge of the through hole of the base plate 37 and the ingot guide rod 12, ensuring that the ingot rod or guide rod 47 slides relative to it, effectively preventing cooling water from leaking out from the through hole of the base plate 37.

[0077] Through the above-described configuration, the spray system cools the ingot guide rod 12, creating a temperature gradient from bottom to top within the single crystal seed crystallizer 8, thus promoting the formation of the single crystal seed. After the single crystal seed is prepared, the single crystal ingot traction mechanism pulls the crucible 5 downwards, while the spray system continues to operate, transferring cooling energy through the ingot guide rod 12 into the crucible 5, accelerating the formation of the temperature gradient within the crucible 5.

[0078] As a preferred embodiment of the present invention, it also includes an air-cooling system 44, which includes an argon cooler 26, an air cooler 27, a gas delivery pipe 28, a gas collection pipe 29, and a second insulation jacket 30.

[0079] The second insulation sleeve 30 is located below the first insulation sleeve 3 and is fitted over the outside of the crucible. The upper end of the second insulation sleeve 30 abuts against the lower end of the first insulation sleeve 3. An air cooler 27 is provided on the lower side of the second insulation sleeve 30. The argon gas cooler 26 is located outside the vacuum furnace 1 and is connected to the air cooler 27 via a gas supply pipe 28. The air cooler 27 is used to cool the crucible 5. One end of the gas collecting pipe 29 is connected to the argon gas cooler 26, and the other end is located inside the vacuum furnace 1. The argon gas blown out by the air cooler 27 flows back to the argon gas cooler 26 through the gas collecting pipe 29, is cooled in the argon gas cooler 26, and then is transported to the air cooler 27 through the gas supply pipe 28. The air cooler 27 blows the argon gas onto the surface of the crucible 5 to cool the crucible 5.

[0080] In the above technical solution, under the drive of the guide bracket 23, the crucible 5 gradually moves downward. The crucible 5 located above the second insulation sleeve 30 is heated by the induction coil 4 and is in a heat preservation state, while the crucible 5 located below the second insulation sleeve 30 is cooled by the air cooler 27 and is in a cooling state, so that a temperature gradient is formed inside the crucible 5, which accelerates the heat dissipation of the crucible 5 located below and assists the rapid growth of the single crystal ingot inside the crucible 5.

[0081] In addition to accelerating the rapid growth of single crystal ingots, the air-cooling system 44 can also introduce argon gas into the vacuum furnace 1 during the preparation of single crystal seed crystals. Since the cold air blown out by the air-cooling system 44 acts on the sprayer 11, it can cool the side wall of the sprayer 11 and simultaneously introduce argon gas into the vacuum furnace 1. This prevents the cooling water from flowing into the vacuum furnace 1 through the heat-resistant pad 42 due to the negative pressure environment, and also isolates the air to ensure the cleanliness of the melt.

[0082] As a preferred embodiment of the present invention, the heating and heat preservation system 2 further includes a heat insulation pad 41, which is disposed at the bottom end of the crucible 5 and located between the crucible 5 and the sprayer 11. The heat insulation pad 41 is used to insulate the heat from the sprayer 11, so that heat can only be transferred through the ingot guide rod 12.

[0083] As a preferred embodiment of the present invention, the spraying system further includes a heat-resistant rubber pad 42 and a pressure plate 43. The pressure plate 43 is disposed below the heat insulation pad 41, and the heat-resistant rubber pad 42 is disposed below the pressure plate 43, with the heat-resistant rubber pad 42 in contact with the top plate 36 of the sprayer 11. The heat-resistant rubber pad 42 has a through hole in the middle through which the ingot guide rod 12 passes, and the diameter of the through hole in the middle of the heat-resistant rubber pad 42 is smaller than the diameter of the ingot guide rod 12 to prevent cooling water on the ingot guide rod 12 from seeping into the crucible 5.

[0084] As a preferred technical solution of the present invention, the vacuum furnace system further includes a control system, which is connected to the first thermocouple 9, the second thermocouple 10, the chiller of the water spray system, the argon cooler 26 of the air cooling system 44, the first motor of the single crystal seed crystal traction mechanism, and the second motor of the single crystal ingot traction mechanism, respectively, for controlling each device and mechanism.

[0085] The present invention also discloses a method of using the above-mentioned metal single crystal ingot preparation apparatus, comprising the following steps:

[0086] S1. The upper end of the ingot guide rod 12 driven by the first motor of the single crystal seed crystal traction mechanism is inserted into the single crystal seed crystal crystallizer 8, the lower part of the crucible 5 is sealed, the metal raw material is placed in the crucible, the vacuum furnace is evacuated, and the crucible is heated by the inductive coil 4, so that the metal raw material melts into liquid metal in the crucible.

[0087] S2. Argon gas is introduced into the vacuum furnace through the air-cooling system. After reaching the set pressure, the single crystal seed preparation system and water spray system are turned on to cool the ingot guide rod 12, so that the liquid metal solidifies in the single crystal seed crystallizer 8. By controlling the spray water volume of the water spray system, and cooperating with the first thermocouple 9 and the second thermocouple 10 to monitor the temperature in the single crystal seed crystallizer 8, the temperature of the single crystal seed crystallizer 8 is made to reach the set range and the set longitudinal temperature gradient. The single crystal seed traction mechanism is turned on to lower the ingot guide rod 12, ensuring that the outlet temperature of the single crystal seed crystallizer 8 is controlled below the melting point temperature of the alloy or metal, and the inlet temperature of the single crystal seed crystallizer 8 is controlled above the melting point temperature of the alloy or metal. That is, a temperature gradient is formed from bottom to top in the crystallizer. This temperature gradient causes the solid-liquid interface to transfer into the crystallizer, solving the "fire run" phenomenon and realizing the preparation of single crystal seeds.

[0088] S3. After the single crystal seed crystallizer 8 stably generates an ingot with a single crystal seed, the first motor controls the first lead screw to not rotate, while the locking screw 24 is tightened so that its end presses against the ingot guide rod 12. The second motor and air cooling system of the single crystal ingot traction mechanism are turned on, so that the ingot guide rod 12 and the guide bracket 23 move downward together, and the sprayer 11 and the crucible 5 move downward together, so that the crucible 5 slowly descends from the crucible, allowing the single crystal seed to grow freely in the single crystal ingot generation part 7 of the crucible 5 and gradually expand the single crystal radius until it reaches the heat preservation part 6 inside the crucible 5, thus completing the transformation from single crystal seed to single crystal ingot. In the above process, the temperature of the melt inside the crucible located inside the first insulation sleeve 3 is controlled by the induction coil 4, and the temperature inside the crucible located outside the first insulation sleeve 3 is transferred to the bottom of the crucible 5 through the sprayer 11 and the ingot guide rod 12. At the same time, the cooling capacity is transferred to the outer surface of the crucible 5 through the air cooling system. This comprehensive approach achieves overall temperature control of the crucible 5 in the longitudinal direction, forming a temperature gradient and ensuring the smooth preparation of single crystal ingots.

[0089] This device breaks through the bottleneck of the traditional single crystal seed crystal having a very small diameter, and can produce copper single crystal seed crystals with a diameter of not less than 20 mm, which provides favorable conditions for the rapid growth of subsequent single crystal ingots.

[0090] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A metal single crystal ingot preparation apparatus, characterized in that, The system comprises a vacuum furnace system, a heating and heat preservation system (2), a single crystal seed crystal preparation system, a water spraying system, and an ingot guide rod (12). The vacuum furnace system comprises a vacuum furnace (1), and the heating and heat preservation system (2) is arranged in the vacuum furnace. The heating and heat preservation system (2) comprises a first heat preservation sleeve (3), an induction coil (4), and a crucible (5). The first heat preservation sleeve (3) is in a columnar structure, and a heat preservation cover (45) is arranged at the top of the first heat preservation sleeve (3). The induction coil (4) is arranged outside the first heat preservation sleeve (3). The crucible (5) is arranged in the first heat preservation sleeve (3) and is provided with an accommodating cavity. The accommodating cavity in the crucible (5) comprises a heat preservation part (6) and a single crystal ingot generation part (7). The heat preservation part (6) is in a cylindrical structure and is located on the upper side of the single crystal ingot generation part (7). The single crystal ingot generation part (7) is in an inverted conical structure. The lower end of the crucible (5) is provided with an opening in communication with the single crystal ingot generation part (7). The single crystal seed crystal preparation system comprises a single crystal seed crystal crystallizer (8), a first thermocouple (9), and a second thermocouple (10). The single crystal seed crystal crystallizer (8) is arranged below the crucible (5), and the upper end of the single crystal seed crystal crystallizer (8) is in communication with the opening at the lower end of the crucible (5). The first thermocouple (9) is located on the upper side of the second thermocouple (10), and the temperature measuring ends of the two thermocouples are located inside the side wall of the single crystal seed crystal crystallizer (8). The ingot guide rod (12) is located below the single crystal seed crystal crystallizer (8). The water spraying system comprises a sprayer (11) arranged around the ingot guide rod (12) and used for spraying cooling water on the ingot guide rod (12). The single crystal seed crystal preparation system further comprises a crystallizer sleeve (46) arranged outside the single crystal seed crystal crystallizer (8). The first thermocouple (9) and the second thermocouple (10) are both mounted on the crystallizer sleeve (46). The two thermocouples both penetrate the side wall of the crystallizer sleeve (46) and have temperature measuring ends located inside the side wall of the single crystal seed crystal crystallizer (8). The system further comprises a single crystal seed crystal traction mechanism arranged below the vacuum furnace (1). The lower end of the ingot guide rod (12) penetrates the lower bottom wall of the vacuum furnace (1) and is connected with the single crystal seed crystal traction mechanism. The single crystal seed crystal traction mechanism comprises a first motor, a first speed reducer, a first lead screw, a first guide column (14), and an ingot guide rod support plate (13). The lower end of the dummy bar guide rod (12) is connected with a dummy bar guide rod support plate (13), the dummy bar guide rod support plate (13) is provided with a threaded hole, a first screw rod is screwed with the threaded hole on the dummy bar guide rod support plate (13), a single crystal ingot pulling mechanism is arranged below the dummy bar guide rod support plate (13), the single crystal ingot pulling mechanism comprises a support base plate (20), a first motor and a first speed reducer are arranged on the support base plate (20), the first motor is connected with the first screw rod through the first speed reducer, and driving the screw rod to rotate makes the dummy bar guide rod support plate (13) connected to perform a lifting action; the first guide column (14) is arranged on the dummy bar guide rod support plate (13), the support base plate (20) is provided with a guide through hole for the first guide column (14) to pass through, and the lower part of the first guide column (14) passes through the guide through hole on the support base plate (20); The single crystal ingot pulling mechanism further comprises a second motor, a second speed reducer, a second screw rod, a third guide column (22), a dummy bar guide rod locking mechanism, a guide bracket (23) and a base plate (25); The guide bracket (23) is arranged in the vacuum furnace (1) and comprises a guide bracket (49) and a second guide column (21), and the guide bracket (49) is located below the sprayer (11); The upper end of the sprayer (11) abuts against the bottom of the crucible (5), the lower end of the sprayer (11) abuts against the guide bracket (49), the guide bracket (49) is provided with a through hole for the dummy bar guide rod (12) to pass through, the upper end of the dummy bar guide rod (12) passes through the guide bracket (49) and is located above the guide bracket (49); the guide bracket (49) is provided with the second guide column (21), the second guide column (21) is vertically arranged, the lower bottom wall of the vacuum furnace (1) is provided with a guide through hole for the second guide column (21) to pass through, and the lower part of the second guide column (21) passes through the guide through hole on the lower bottom wall of the vacuum furnace (1), so as to provide guidance for the lifting movement of the guide bracket (23); The dummy bar guide rod locking mechanism comprises a locking screw (24), the guide bracket (49) is provided with a threaded through hole extending from one end of the guide bracket (49) towards the dummy bar guide rod (12), the threaded through hole is in communication with the through hole on the guide bracket (49) for the dummy bar guide rod (12) to pass through, and the locking screw (24) is screwed in the threaded through hole; and the end of the locking screw (24) is tightly pressed against the dummy bar guide rod (12) by being screwed, so that the dummy bar guide rod (12) can be locked on the guide bracket (49). The support base plate (20) is provided with a threaded hole, the base plate (25) is located below the support base plate (20), the second screw rod is screwed with the threaded hole on the support base plate (20), the second motor is connected with the second screw rod through the second speed reducer, and the second screw rod is driven to rotate to make the support base plate (20) perform a lifting action; the second motor and the second speed reducer are arranged on the base plate (25); the third guide column (22) is arranged on the support base plate (20), and the base plate (25) is provided with a guide through hole for the third guide column (22) to pass through, and the lower part of the third guide column (22) passes through the through hole on the base plate (25), so that the lifting of the support plate base is guided.

2. The apparatus for preparing a single-crystal ingot of metal according to claim 1, wherein The single crystal seed pulling mechanism further comprises a centering device (15) arranged on the dummy bar guide rod support plate (13), the centering device (15) comprises a drill chuck (16) and a centering screw rod (17), the drill chuck (16) comprises a cylindrical part (18) and a tapered part (19), the tapered part (19) is arranged on the lower side of the cylindrical part (18), both are hollow shell structures, the lower part of the dummy bar guide rod (12) passes through the tapered part (19) from top to bottom and is arranged in the cylindrical part (18), and a threaded hole for the centering screw rod (17) to pass through is arranged on the side wall of the cylindrical part (18), the centering screw rod (17) is screwed in the threaded hole of the cylindrical part (18), and the centering screw rod (17) is provided with at least three groups, and each centering screw rod (17) is uniformly arranged along the circumference of the cylindrical part (18).

3. The apparatus for preparing a single-crystal ingot of metal according to claim 1, wherein Further comprising a forced air cooling system (44) comprising an argon cooler (26), an air cooler (27), a gas conveying pipe (28), a gas collecting pipe (29) and a second heat preservation sleeve (30); The second heat preservation sleeve (30) is located below the first heat preservation sleeve (3), the upper end of the second heat preservation sleeve (30) is in abutment with the lower end of the first heat preservation sleeve (3), the lower side of the second heat preservation sleeve (30) is provided with the air cooler (27), the argon cooler (26) is located outside the vacuum furnace (1), the argon cooler (26) is connected with the air cooler (27) through the gas conveying pipe (28), and one end of the gas collecting pipe (29) is in communication with the argon cooler (26) and the other end is located in the vacuum furnace (1).

4. The apparatus for preparing a single crystal ingot of metal according to claim 1, wherein The spraying system further comprises a cooler (31), a water conveying pipe (32) and a water return pipe (33); The cooler (31) is located outside the vacuum furnace (1). The sprayer (11) comprises an inner shell (34), an outer shell (35), a top plate (36), a bottom plate (37), and a sealing rubber pad (38). The outer shell (35) is in a tubular structure. The bottom plate (37) is arranged at the lower end of the outer shell (35), and the top plate (36) is arranged at the upper end of the outer shell (35). The bottom plate (37) and the top plate (36) are both provided with through holes for the ingot guide rod (12) to pass through. The inner shell (34) is arranged inside the outer shell (35). The upper end and the lower end of the inner shell (34) are sealingly connected to the inner side wall of the outer shell (35), so as to form a water containing chamber (39) between the inner shell (34) and the outer shell (35). The inner side wall of the inner shell (34) is provided with a spraying hole (48). One end of the water delivery pipe (32) is in communication with the water containing chamber (39), and the other end is in communication with the cooling machine (31). The outer shell (35) below the inner shell (34) and the bottom plate (37) enclose a water receiving groove (40). One end of the water return pipe (33) is in communication with the water receiving groove (40), and the other end is in communication with the cooling machine (31). The sealing rubber pad (38) is installed at the bottom of the bottom plate (37). The middle region of the sealing rubber pad (38) is provided with an annular protruding structure, which is embedded in the through hole of the bottom plate (37) and used to fill the gap between the through hole edge of the bottom plate (37) and the ingot guide rod (12).

5. The apparatus for preparing a single crystal ingot of metal according to claim 4, wherein The heating and heat preservation system (2) further comprises a heat insulation pad (41), which is arranged at the lower bottom end of the crucible (5) and located between the crucible (5) and the sprayer (11).

6. The apparatus according to claim 4, wherein The spraying system further comprises a heat-resistant rubber pad (42) and a pressing plate (43). The pressing plate (43) is arranged below the heat insulation pad (41). The heat-resistant rubber pad (42) is arranged below the pressing plate (43) and in contact with the top plate (36) of the sprayer (11). The heat-resistant rubber pad (42) is provided with a through hole in the middle for the ingot guide rod (12) to pass through. The diameter of the through hole in the middle of the heat-resistant rubber pad (42) is smaller than the diameter of the ingot guide rod (12).

7. The apparatus according to claim 1, wherein The taper angle of the single crystal ingot generation part (7) of the crucible (5) is 45°~60°.

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