WO2014176778A1 - 一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法 - Google Patents

一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法 Download PDF

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Publication number
WO2014176778A1
WO2014176778A1 PCT/CN2013/075110 CN2013075110W WO2014176778A1 WO 2014176778 A1 WO2014176778 A1 WO 2014176778A1 CN 2013075110 W CN2013075110 W CN 2013075110W WO 2014176778 A1 WO2014176778 A1 WO 2014176778A1
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Prior art keywords
energy beam
casting
vacuum chamber
head
melting
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PCT/CN2013/075110
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English (en)
French (fr)
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李碚
张森
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深圳市赛迈特悬浮冶金科技有限公司
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Priority to PCT/CN2013/075110 priority Critical patent/WO2014176778A1/zh
Publication of WO2014176778A1 publication Critical patent/WO2014176778A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/06—Crucible or pot furnaces heated electrically, e.g. induction crucible furnaces with or without any other source of heat
    • F27B14/061—Induction furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details peculiar to crucible or pot furnaces
    • F27B14/14—Arrangements of heating devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D11/00—Arrangement of elements for electric heating in or on furnaces
    • F27D11/06—Induction heating, i.e. in which the material being heated, or its container or elements embodied therein, form the secondary of a transformer
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D99/00—Subject matter not provided for in other groups of this subclass
    • F27D99/0001—Heating elements or systems
    • F27D99/0006—Electric heating elements or system
    • F27D2099/003—Bombardment heating, e.g. with ions or electrons
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the present invention relates to a method of melting and casting refractory metals and alloys thereof in combination with cold head induction melting technology and energy beam technology.
  • Refractory metals generally refer to metals with melting points between 1800 and 3400 ° C, such as tungsten, ruthenium, osmium, molybdenum, niobium, tantalum, vanadium, chromium, zirconium, etc. Sometimes, titanium with a melting point of 1660 ° C is also Belonging to this category.
  • metal tungsten is used for electric light source and tube components, metallurgical, welded electrodes, and hard alloys and hardfacing layers; tungsten copper and tungsten silver alloys are used as electrical contact materials; tungsten and nickel, iron, copper and other elements High-specific gravity alloys are used in the manufacture of gyroscope rotors, guides and shock absorbers for aerospace and spacecraft, mechanically produced die-casting molds, tool holders, masts and automatic watch weights, as well as armor-piercing bullets and weapons for weapons. Radiation shield.
  • Metal molybdenum is used in the manufacture of electronic equipment and electrodes, as well as in alloy steels and high temperature superalloys for aerospace and aerospace applications; molybdenum alloys are used in atomic energy, aerospace and aerospace technologies.
  • Metal ruthenium is mainly used for capacitors, tubes and high-temperature alloys, as well as corrosion-resistant equipment in the chemical and atomic industries, tantalum-tungsten alloys and tantalum-tungsten-rhenium alloys for corrosion-resistant materials in the chemical industry, high-temperature structural materials for the aerospace industry, and rocket nozzles. And spacecraft parts.
  • Tantalum and niobium alloys are used as high-temperature structural materials for spacecraft, structural materials for atomic reactors, and acid-resistant equipment in the chemical industry. They are also used to make high-strength low-alloy steels and high-temperature resistant superalloys, similar to titanium and tin. Zirconium, aluminum, and niobium alloys are superconductors.
  • Zirconium and zirconium alloys are used as core construction materials for nuclear reactors, hydrogen storage materials and corrosion resistant materials, and ballistic resistant alloy steels.
  • Chromium is used to make surface modification layers of stainless steel, superalloys, electrothermal alloys, alloy structural steels and steels, and high hardness chrome-cobalt alloys are used to make cutting tools.
  • Vanadium is mainly used in the manufacture of stainless steel, structural steel, spring steel, tool steel, armor steel and rails. It is also used in the manufacture of superalloys, vanadium gallium. Alloys are important superconducting materials.
  • the first type is high-temperature vacuum sintering technology.
  • the process includes: forming a metal into a powder of suitable particle size, press-forming a mixture of powders, and increasing the density of the blank in an isostatic pressing device at a temperature lower than the melting point of the material.
  • the billet is sintered or hot pressed into a relatively high density material under vacuum conditions.
  • a product such as a plate, a rod, a belt, a wire or the like
  • the disadvantage of this technique is that there are pores in the material, the compactness is not ideal, the gas content is relatively high, and the process flow is relatively long.
  • the second type is vacuum energy beam cold head melting technology, where the energy beam refers to an arc beam, a plasma beam, an electron beam, a laser beam, and the like.
  • vacuum arc melting technology that is, vacuum non-consumable arc melting technology is more common.
  • Such techniques achieve particularly high temperatures by employing the various energy beams described above. Since ceramic materials react strongly with metal melts at such high temperatures, these techniques use water-cooled copper matte. It should be noted that the coldness mentioned here is a water-cooling flaw that is not separated.
  • This technology One The disadvantage is that the energy beam is concentrated and the charge melts in its focus position, but when the energy beam is transferred to other locations to melt the charge, under the conditions of intense water cooling, the previously melted charge immediately solidifies.
  • the third category is vacuum cold head induction melting technology (hereinafter referred to as cold head induction melting technology), which is one of the most advanced melting techniques in the modern era.
  • the existing vacuum cold head induction melting equipment consists of a cold head 11 ', an induction coil 12 ', and a vacuum chamber 13 ', high frequency or intermediate frequency induction power supply 14 ', vacuum - argon-filled system 15 ', control cabinet 16 'and cooling system 17 '.
  • the charge (not shown) is placed in the cold head 11 ', and the induction coil 14 ' is sent to the induction coil 12
  • the electromagnetic field generated by the high-frequency or intermediate-frequency current passes through the crucible wall to heat the charge to produce a smelting action.
  • Cold heading 11 ' generally made of copper, the reason why the electromagnetic field can pass through the metal wall is that it has a number of slits parallel to the axis. In order to make it cold 11 'It does not melt at the melting temperature, and the wall is cooled by water. Cooling water is passed through each of the flaps.
  • the electromagnetic field as a heating source has an integral range of action on the charge, and can generate a strong stirring action. Therefore, the charge is integrally melted, suspended, and agitated as a whole. This condition is necessary to obtain a product that is accurate, uniform, and dense in composition.
  • the temperature of the charge is difficult to reach a high temperature of 2000 °C or higher.
  • the technical problem to be solved by the invention is that it overcomes the disadvantage that the material is partially melted and the uniformity of the composition is difficult to be ensured when the refractory metal and the alloy are melted by the energy beam melting technique such as vacuum non-consumable arc melting, and a disadvantage is proposed.
  • the smelting process melts the refractory metal and the alloy as a whole, and the finished product has a new technology of good composition uniformity. With this new technology, various casting operations can be performed on refractory metals and alloys.
  • the present invention proposes the following technical solution: a method of melting and casting a refractory metal and an alloy thereof combined with a cold head induction melting technique and an energy beam technique, which requires application of a device including a vacuum chamber a truss, a cold head, an induction coil, a high frequency or intermediate frequency induction power source, an energy beam emitting head, an energy beam generator, and a casting mold;
  • the vacuum chamber is an inner closed container
  • the truss is installed in the vacuum chamber
  • the cold head is installed in the vacuum chamber, and the cold head is mounted on the truss, the cold head is made of dense copper, and the cold head is composed of a plurality of ridges, and the gap between the ridges is parallel to the cold ⁇ Axis
  • the induction coil is installed inside the vacuum chamber, and the induction coil is circumferentially mounted on the outside of the cold chamber;
  • the high frequency or intermediate frequency induction power source is installed outside the vacuum chamber, and the high frequency or intermediate frequency induction power source is connected to the induction coil and supplies power to the induction coil;
  • the energy beam emitting head is mounted at a top end of the vacuum chamber, above the cold head, and the energy beam emitted from the energy beam emitting head reaches the cold head;
  • the energy beam generator is mounted outside the vacuum chamber, the energy beam generator is coupled to the energy beam emitting head, the energy beam generator capable of generating an energy beam and transmitting to the energy beam emitting head;
  • the casting mold is installed obliquely below the cold head
  • the energy beam generator is a non-consumable arc generating device, and the energy beam emitted by the energy beam emitting head is an arc beam; or the energy beam generator is a plasma beam emitting device, and the energy beam emitted by the energy beam emitting head is a plasma beam Or the energy beam generator is an electron beam emitting device, and the energy beam emitted by the energy beam emitting head is an electron beam; or the energy beam generator is a laser emitting device, and the energy beam emitted by the energy beam emitting head is a laser beam;
  • the energy beam emitting head is vacuum-tightly mounted on the top of the vacuum chamber, and can swing within a certain angle range, and the swinging of the emitting head can enlarge the local molten pool formed by the energy beam to a certain extent;
  • a heat-insulating baffle made of a high-melting ceramic material with a hole in the center is arranged on the upper end surface of the cold head.
  • the diameter of the central hole is larger than the diameter of the energy beam.
  • the heat-insulating baffle can prevent energy beam bombardment. Go to the cold side wall and reduce the radiant heat loss of the molten pool to speed up the melting process of the charge;
  • the method includes the following steps:
  • Step 1 Smelting: During the smelting process, the induction power source is controlled to generate an electromagnetic field in the induction coil. Controlling the energy beam generator such that the energy beam emits an energy beam N from the hair, and the energy beam N causes the local charge in the cold head to reach a high temperature and melt to form a local molten pool, and the electromagnetic field B The furnace material is integrally heated to expand the local molten pool and obtain electromagnetic stirring until all the metal charge forms a uniform molten pool;
  • Step 2 Tumble casting: After the smelting is finished, the energy beam generator is controlled so that the energy beam emitting head stops emitting the energy beam. Control the inductive power supply so that the induction coil continues to work to maintain the electromagnetic field B. The electromagnetic field B continues to heat the molten pool, while removing the thermal barrier, tilting the cold, and pouring the refractory metal melt into the casting mold.
  • the apparatus for melting and casting the refractory metal and the alloy thereof further comprises a vacuum - An argon-filling system, a cooling system, a control cabinet, the vacuum-filling argon system is installed outside the vacuum chamber, the vacuum - An argon-filling system fills the vacuum chamber with argon; the cooling system is used to cool the cold head; the control cabinet is connected to the vacuum chamber, the high frequency or intermediate frequency induction power source, and the vacuum - Fill the argon system, cool the system, and control them.
  • the casting mold is a water-cooled copper mold or a non-metal mold prepared from zirconia, boron nitride, or magnesium oxide materials.
  • the casting mold is made of silicon carbide and graphite, and the inner surface of the casting mold has a coating of zirconia, boron nitride, or magnesium oxide material.
  • the present invention proposes the following technical solution: a method for melting and casting a refractory metal and an alloy thereof in combination with a cold head induction melting technique and an energy beam technique, which applies a device including a vacuum chamber a truss, a cold head, an induction coil, a high frequency or intermediate frequency induction power source, an energy beam emitting head, an energy beam generator, a casting mold, a plug and a tie rod;
  • the vacuum chamber is an inner closed container
  • the truss is installed in the vacuum chamber
  • the cold head is installed in the vacuum chamber, and the cold head is mounted on the truss, the cold head is made of dense copper, and the cold head is composed of a plurality of ridges, and the gap between the ridges is parallel to the cold ⁇ Axis
  • the cold heading includes a bottom plate having a bottom casting opening at the center thereof;
  • the induction coil is installed inside the vacuum chamber, and the induction coil is circumferentially mounted on the outside of the cold chamber;
  • the high frequency or intermediate frequency induction power source is installed outside the vacuum chamber, and the high frequency or intermediate frequency induction power source is connected to the induction coil and supplies power to the induction coil;
  • the energy beam emitting head is mounted at a top end of the vacuum chamber, above the cold head, and an energy beam is emitted from the energy beam emitting head to reach the cold head;
  • the energy beam generator is mounted outside the vacuum chamber, the energy beam generator is coupled to the energy beam emitting head, the energy beam generator capable of generating an energy beam and transmitting to the energy beam emitting head;
  • the casting mold is installed in the vacuum chamber directly under the cold head, and an opening is formed in the bottom of the casting mold;
  • the plug is connected to the top end of the pull rod, and the pull rod is inserted into the opening of the casting mold;
  • the energy beam generator is a non-consumable arc generating device, and the energy beam emitted by the energy beam emitting head is an arc beam; or the energy beam generator is a plasma beam emitting device, and the energy beam emitted by the energy beam emitting head is a plasma beam Or the energy beam generator is an electron beam emitting device, and the energy beam emitted by the energy beam emitting head is an electron beam; or the energy beam generator is a laser emitting device, and the energy beam emitted by the energy beam emitting head is a laser beam;
  • the energy beam emitting head is vacuum-tightly mounted on the top of the vacuum chamber, and can swing within a certain angle range, and the swinging of the emitting head can enlarge the local molten pool formed by the energy beam to a certain extent;
  • a heat-insulating baffle made of a high-melting ceramic material with a hole in the center is arranged on the upper end surface of the cold head.
  • the diameter of the central hole is larger than the diameter of the energy beam.
  • the heat-insulating baffle can prevent energy beam bombardment. Go to the cold side wall and reduce the radiant heat loss of the molten pool to speed up the melting process of the charge;
  • the method includes the following steps:
  • Step 1 Smelting: During the smelting process, the induction power source is controlled to generate an electromagnetic field in the induction coil. Controlling the energy beam generator such that the energy beam emits an energy beam N from the hair, and the energy beam N causes the local charge in the cold head to reach a high temperature and melt to form a local molten pool, and the electromagnetic field B The furnace material is integrally heated to expand the local molten pool and obtain electromagnetic stirring until all the metal charge forms a uniform molten pool;
  • Step 2 Bottom casting: After the smelting is finished, the induction power supply and the energy beam generator are controlled, so that the induction coil continues to generate electromagnetic fields. And the energy beam emitting head continues to emit the energy beam N while opening the bottom casting port at the bottom of the cold head, so that the melt is injected into the casting mold through the bottom casting port.
  • the apparatus for melting and casting the refractory metal and the alloy thereof further comprises a vacuum - An argon-filling system, a cooling system, a control cabinet, the vacuum-filling argon system is installed outside the vacuum chamber, the vacuum - An argon-filling system fills the vacuum chamber with argon; the cooling system is used to cool the cold head; the control cabinet is connected to the vacuum chamber, the high frequency or intermediate frequency induction power source, and the vacuum - Fill the argon system, cool the system, and control them.
  • the casting mold is a water-cooled copper mold or a non-metal mold prepared from zirconia, boron nitride, or magnesium oxide materials.
  • the casting mold is made of silicon carbide and graphite, and the inner surface of the casting mold has a coating of zirconia, boron nitride, or magnesium oxide material.
  • the above technical solution is further defined by adding a feeder at the top of the vacuum chamber, adding a casting chamber below the vacuum chamber, placing the casting mold in the casting chamber, and installing a first valve between the vacuum chamber and the casting chamber.
  • a second valve is mounted on the side wall of the casting chamber.
  • the invention overcomes the disadvantage that in the energy beam melting technology, the charge can only form a local molten pool, and it is difficult to obtain agitation, so that the charge can be integrally melted and fully electromagnetically stirred, so the product
  • the composition is accurate and uniform. This advantage is particularly important for the preparation of alloys of refractory metals.
  • the refractory metal and its alloy In the energy beam melting technology, it is difficult for the refractory metal and its alloy to melt integrally, which poses an important difficulty for the casting process. Even if there is a large molten pool, the energy beam emission is terminated during the casting process, which leads to the melt. The temperature is lowered, so the yield is low and the casting quality is poor.
  • the invention forms an integral molten pool during the smelting process, in which the electromagnetic field and the energy beam can continue to be heated together, at least the electromagnetic field can be further heated, so that the molten metal maintains a relatively high temperature during the casting process. Therefore, in the present invention, the casting process has a high finished product rate, and the structure of the casting is uniform and the material is dense.
  • the technology of the present invention can also adopt other special casting methods such as centrifugal casting, pressure casting, vacuum suction casting, etc. in the casting process to further improve the quality of the casting.
  • high production efficiency can be obtained by using a continuous drawing technique, and a directional crystal material of a refractory metal and its alloy, or even a single crystal, or a refractory metal can be prepared by using a directional solidification technique. And its alloys are purified.
  • the specifications of the energy beam melting equipment are generally small, and the equipment of the invention can reach several tens of kilograms / furnace to several hundred kilograms / The size of the furnace. Therefore, with the technique of the present invention, production efficiency can be greatly improved, and large-sized refractory metals and alloy products can be produced.
  • Figure 1 is a schematic diagram of the basic structure of a conventional vacuum cold head sensing device.
  • FIG. 2 is a schematic view of a cold head vacuum induction melting apparatus with an energy beam assisted heat source of the present invention.
  • Figure 3 shows a vacuum seal - a bellows - KF interface device that allows the emitter to sway.
  • Figure 4 shows the state of the charge when the metal or alloy is smelted using the apparatus of the present invention.
  • Figure 5 is a schematic illustration of tilt casting in the apparatus of the present invention.
  • Figure 6 is a schematic illustration of bottom casting in the apparatus of the present invention.
  • Figure 7 shows a schematic of the equipment for the feeder and the bottom casting chamber.
  • Figure 8 is a schematic illustration of continuous feed and continuous draw in the apparatus of the present invention.
  • Figure 9 is a schematic illustration of directional solidification performed in the apparatus of the present invention.
  • the present invention provides a first embodiment of an apparatus for melting and casting a refractory metal and an alloy thereof, which comprises a vacuum chamber 1, a truss 3, a cold raft 5, and an induction Circle 7 , a high frequency or intermediate frequency induction power supply 9 , an energy beam emitting head 11 , an energy beam generator 13 , a vacuum - an argon charging system 15 , a cooling system 17 , a control cabinet 19 , a casting mold twenty one .
  • the vacuum chamber 1 is an internal closed container.
  • the truss 3 is installed in the vacuum chamber 1.
  • the cold head 5 is installed in the vacuum chamber 1, and the cold head 5 is mounted on the truss 3.
  • the cold heading 5 is made of dense copper, which is cold 5 It consists of a number of flaps (not shown), the gap between the flaps being parallel to the axis of the cold head 5. Cooling water is introduced into each of the lobes for sufficient cooling.
  • the induction coil 7 is mounted inside the vacuum chamber 1, and the induction coil 7 is circumferentially mounted outside the cold head 5.
  • the high frequency or intermediate frequency induction power supply 9 is mounted outside the vacuum chamber 1, and the high frequency or intermediate frequency induction power supply 9 is connected to the induction coil. And supplying power to the induction coil 7.
  • the energy beam emitting head 11 is mounted at the inner top end of the vacuum chamber 1 above the cold head 5 from the energy beam emitting head 11
  • the energy beam N is emitted to reach the cold head 5, and the refractory metal charge located in the cold head 5 is heated.
  • the energy beam emitted by the above energy beam emitting head 11 It can be an arc beam, a plasma beam melting technique, an electron beam melting technique or a laser beam.
  • the energy beam generator 13 is mounted outside the vacuum chamber 1.
  • the energy beam generator 13 is connected to the energy beam emitting head 11 .
  • the energy beam generator 13 is capable of generating an energy beam and transmitting it to the energy beam emitting head 11.
  • the energy beam generator 13 It may be a non-consumable arc generating device, or a plasma beam emitting device, or an electron beam emitting device, or a laser emitting device.
  • the energy beam emitting head 11 is combined with the top of the vacuum chamber 1 by a vacuum seal in the vacuum chamber 1 A KF interface 112 is mounted on the top, then a stainless steel bellows 114 is installed, and then a KF interface is mounted on top of the stainless steel bellows 114. .
  • the energy beam emitting head 11 can be shaken within a certain angular range.
  • a heat insulating baffle made of a high-melting ceramic material having a hole in the center is provided on the upper end surface of the cold heading 52 52
  • the diameter of the center hole should be significantly larger than the diameter of the energy beam.
  • the purpose of the heat shield baffle 52 is to prevent the energy beam from bombarding the side wall of the cold head 5 and reduce the loss of radiant heat.
  • the vacuum-filling argon system 15 is installed outside the vacuum chamber 1, and the vacuum-filling argon system 15 is supplied to the vacuum chamber 1 Fill with argon.
  • the cooling system 17 is used to cool the cold head 5 .
  • the control cabinet 19 is connected to the vacuum chamber 1 , high frequency or intermediate frequency induction power supply 9 , vacuum - argon charging system 15 , cooling system 17 and control them.
  • the casting mold 21 is installed obliquely below the cold head 5.
  • the invention provides a method for melting and casting refractory metals and alloys thereof combined with cold head induction melting technology and energy beam technology, which requires the use of the first embodiment of the above apparatus, comprising the following steps:
  • Step 1 Smelting: During the smelting process, the induction power source 9 is controlled to cause the induction coil 7 to generate an electromagnetic field B
  • the energy beam generator 13 is controlled such that the energy beam emitting head 11 emits an energy beam N, and the energy beam N causes the local charge in the cold head 5 to reach a high temperature and melt to form a local molten pool, and the electromagnetic field B
  • the furnace material is integrally heated to expand the local molten pool and obtain electromagnetic stirring until all the metal charge forms a uniform molten pool;
  • Step 2 Tumble casting: After the smelting is finished, the energy beam generator 13 is controlled so that the energy beam emitting head 11 stops emitting the energy beam. N, control the inductive power supply 9 so that the induction coil 7 continues to work to maintain the electromagnetic field B, the electromagnetic field B continues to heat the molten pool, while removing the heat shield baffle 52, tilting the cold head 5, the refractory metal melt 100 Cast into the casting mold 21.
  • the present invention proposes a second embodiment of an apparatus for melting and casting a refractory metal and an alloy thereof, comprising the same vacuum chamber 1 as the apparatus described in the first embodiment, truss 3, induction Circle 7 , high frequency or intermediate frequency induction power supply 9 , energy beam emitting head 11 , energy beam generator 13 , vacuum - argon filling system 15 , cooling system 17 , control cabinet 19 .
  • the difference is that it includes a cold head 31, a casting mold 33, a plug 35 and a pull rod 37.
  • the cold head 31 is installed in the vacuum chamber 1.
  • the induction coil 7 is circumferentially disposed outside the cold head 31.
  • the cold head 31 includes a bottom plate 312 having a bottom casting opening 314 in the center thereof.
  • the casting mold 33 is installed in the vacuum chamber 1 directly below the cold head 31, and the casting mold 33
  • the opening has an opening 332 at the bottom.
  • the dam 35 is attached to the top end of the tie rod 37, and the pull rod 37 is inserted into the opening 332 of the casting mold 33. Medium.
  • the present invention proposes another method of melting and casting refractory metals and alloys thereof in combination with cold head induction melting technology and energy beam technology, and requires the use of the second embodiment of the above apparatus, including the following steps:
  • Step 1 Smelting: During the smelting process, the induction power source 9 is controlled to cause the induction coil 7 to generate an electromagnetic field B
  • the energy beam generator 13 is controlled such that the energy beam emitting head 11 emits an energy beam N, and the energy beam N causes the local charge in the cold head 5 to reach a high temperature and melt to form a local molten pool, and the electromagnetic field B
  • the furnace material is integrally heated to expand the local molten pool and obtain electromagnetic stirring until all the metal charge forms a uniform molten pool;
  • Step 2 Bottom casting: After the smelting is finished, the induction power source 9 and the energy beam generator 13 are controlled to make the induction coil 7 The electromagnetic field B continues to be generated and the energy beam emitting head 11 continues to emit the energy beam N while opening the bottom casting port 54 at the bottom of the cold heading 5, so that the melt is injected into the casting mold through the bottom casting port 54. Medium.
  • a feeder 41 is added at the top of the vacuum chamber 1 at the feeder 41.
  • the refractory metal charge to be smelted is loaded into the medium 100.
  • a casting chamber 51 is added below the vacuum chamber 1 to place the casting mold 33 in the casting chamber 51.
  • a first valve 53 is installed in the middle, and a second valve 55 is opened on the side wall of the casting chamber 51.
  • the casting chamber 51 and the vacuum chamber 1 are blocked by the first valve 53 to open the second valve 55
  • the casting material in the mold 33 is taken out, and then the casting chamber 51 is placed back under the vacuum chamber 1, and the casting chamber 51 is evacuated and filled with argon gas to open the first valve 53.
  • the feeder 41 Add a specified amount of material to be smelted to ⁇ 31, and then start the melting and casting of the second furnace material. In this way, it is also possible to carry out more melting and casting of the heat.
  • a continuous feeding-drawing device can be added to the equipment of Figure 2 (as shown in Figure 8). With this device, the raw materials can be continuously added and processed by the ingot technique.
  • the directional solidification device can be obtained by modifying the continuous feeding-drawing device (as shown in Figure 9). It can make the smelted material form oriented crystal structure or single crystal during solidification, or purify the material.
  • the above equipment can also be equipped with some operating mechanisms, such as feeding mechanism, stirring mechanism, turning mechanism, casting mechanism, temperature measurement - Temperature control system, argon purification system, etc.
  • the core of the invention is the fusion of refractory metals and alloys in combination with vacuum cold head induction melting techniques and vacuum energy beam cold head melting techniques.
  • the main body of the apparatus of the present invention is a vacuum cold head induction melting furnace, and an energy beam emitting head is added. And energy beam generator 13 .
  • Energy beam technology is characterized by high temperatures, which can achieve temperatures of 5,000 ° C or even tens of thousands of degrees, so using this technology can smelt a variety of refractory metals, including a melting point of 3400 °C tungsten.
  • the smelting process is generated by the induction power source 9 through the induction coil 7 and the energy beam B and the energy beam emitting head 11 Completion:
  • the electromagnetic field B heats the whole charge, and the energy beam N causes the local charge to reach high temperature and melt.
  • the heating and stirring of the electromagnetic field B gradually enlarges the melting zone, and finally the furnace is completely melted. Due to electromagnetic fields
  • the agitation of B the composition of the melt 100 is uniform (see Figure 4).
  • the induction heating system can be activated first (induction coil 7 and a high frequency or intermediate frequency induction power supply 9 ), the charge is preheated as a whole, and then the energy beam device (the energy beam emitting head 11 and the energy beam generator 13) is activated to form a local molten pool in the charge.
  • the above induction coil 7 and the energy beam emitting head 11 These two heat sources can also be activated at the same time, ending at the same time; or alternate work; or sometimes work together, sometimes work alone.
  • the casting mold may use a water-cooled metal mold, preferably a water-cooled copper mold, or a non-metal mold prepared from a material such as zirconia, boron nitride, or magnesium oxide.
  • the principle of selecting a non-metallic material to prepare a mold is: The melting point of the material should be significantly higher than the metal or alloy being smelted.
  • Silicon carbide and graphite can also be used in casting molds for refractory metals and alloys. However, these materials cause carbonization of metals. Therefore, when they are used to make molds, the inner surface of the mold is preferably zirconia, boron nitride, or oxidized. Coating of materials such as magnesium. The selection principle of the coating material is the same as that of the non-metal mold material.
  • the shape of the bottom portion of the mold cavity can be designed to have a beveled shape.
  • a non-metallic mold When casting materials are required to be slowly cooled, a non-metallic mold should be used and an insulation layer or a heater should be placed at the bottom, around or on the surface of the mold.
  • the medium frequency power supply has a power of 250kw and a frequency of 15kHz.
  • an energy beam emitting head 11 and an energy beam generator 13 as auxiliary heat sources 13 An arc beam is used - the tungsten electrode is mounted above the cold head 5, and the power of the DC power supply to the electrode is 100 kw.
  • the equipment After the equipment is started, vacuum is applied. After the vacuum reaches 5 ⁇ 10 -3 Pa, the high-purity argon of 0.05 MPa is charged, and then the induction power supply 9 is started to heat the charge 100 to 1200 °C. Heating is continued until a molten pool having a temperature exceeding 3600 ° C is formed in the charge 100.
  • the power delivered by the induction power source 9 to the induction coil 7 is increased, and the cold head 5 is shaken, the energy beam emitting head 11 is shaken, the range of the molten pool is gradually increased, and finally the entire charge 100 is melted.
  • the medium frequency power supply has a power of 250kw and a frequency of 15kHz.
  • an energy beam emitting head 11 and an energy beam generator 13 as auxiliary heat sources 13 An arc beam is used - the tungsten electrode is mounted above the cold head 5, and the power of the DC power supply to the electrode is 100 kw.
  • the equipment After the equipment is started, vacuum is applied. After the vacuum reaches 5 ⁇ 10 -3 Pa, the high-purity argon of 0.05 MPa is charged, and then the induction power supply 9 is started to heat the charge 100 to 1200 °C. Heating is continued until a molten pool having a temperature exceeding 3600 ° C is formed in the charge 100.
  • the power delivered by the induction power source 9 to the induction coil 7 is increased, and the cold head 5 is shaken, the energy beam emitting head 11 is shaken, the range of the molten pool is gradually increased, and finally the entire charge 100 is melted.
  • both the arc N and the electromagnetic field B continue to operate while the cold head is turned on.
  • the bottom bottom casting port 314 allows the melt 100 to be injected into the water-cooled copper casting mold 33 through the bottom casting port 314.

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Abstract

一种结合冷坩埚（5）感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，包括以下步骤：1）熔炼，感应线圏产生电磁场（B），能量束发射头（11）发出能量束（N），能量束N使冷坩埚（5）中的局部炉料达到高温并熔化形成局部熔池，电磁场（B）整体加热炉料，使局部熔池扩大并获得电磁搅拌，直至全部金属炉料形成成分均匀的整体熔池；2）倾转铸造，在熔炼结束后，停止发射能量束（N），感应线圏继续工作维持电磁场（B），电磁场（B）继续加热熔池，同时移开隔热挡板，倾转冷坩埚（11），将难熔金属浇注到铸造模具（21）之中。对于难熔金属和合金，该方法能够制备出成分准确、均匀以及致密的材料。

Description

一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法 技术领域
本发明涉及一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法。
背景技术
难熔金属 ( 见下表 ) 一般指熔点在 1800 ～ 3400℃ 的金属，如钨、铼、钽、钼、铌、铪、钒、铬、锆等金属，有时，将熔点为 1660℃ 的钛也归入此类。
金属 钨 W 铼 Re 钽 Ta 钼 Mo 铌 Nb 铪 Hf 钒 V 铬 Cr 锆 Zr 钛 Ti
熔点（℃） 3410 3180 2996 2610 2468 2227 1902 1857 1852 1660
上述金属和以它们为基础的合金（即难熔金属及其合金）在工程、军事和高科技领域有重要用途。
例如，金属钨用于电光源和电子管元件，冶金、焊接的电极，以及硬质合金和表面硬化层；钨铜和钨银合金用作电接触点材料；钨与镍、铁、铜等元素组成的高比重合金则用于制造航空和航天器的陀螺仪转子、导向装置和减震装置，机械制造的压铸模、刀夹、镗杆和自动手表重锤，以及武器用的穿甲弹弹芯和防辐射的防护屏。
金属钼用于制作电子器材和电极，也用于制造合金钢和航空、航天用的耐高温超合金；钼合金则用于原子能、航空和航天技术等领域。
金属钽主要用于电容器、电子管和高温合金，以及化工、原子能工业中的抗腐蚀器材，钽钨合金和钽钨铪合金用于化学工业的耐腐蚀材料，航天工业的高温结构材料，以及火箭喷嘴和航天器零件。
铌和铌合金用作宇宙飞船的耐高温结构材料、原子反应堆的结构材料和化学工业中的耐酸器材，铌还用于制作高强度低合金钢和耐高温的超合金，铌同钛、锡、锆、铝、锗的合金则是超导体。
锆和锆合金用作核反应堆的堆芯结构材料， 贮氢材料 和耐腐蚀材料，以及防弹合金钢。
铪用于核反应堆中的控制棒、 X 射线管的阴极材料及硬质合金的添加剂。铬用于制造不锈钢、高温合金、电热合金、合金结构钢和钢的表面改性层，高硬度的铬钴合金用于制作切削工具。
钒主要用于制造不锈钢、结构钢、弹簧钢、工具钢、装甲钢和钢轨，还用于制造高温合金，钒 镓 合金则是重要的超导材料。
钛和钛合金具有比重小，比强度高，抗腐蚀性能优异等特性，是用量最大的难熔金属和合金，用于制作飞机、火箭、导弹 、船舶、汽车和火车车厢的结构材料，以及化工器材和海水淡化装置。此外，钛还是一种重要的贮氢材料。
这些材料在经济和国防方面有重要的用途，但是制造这些材料的技术相当复杂。首先，只有采用特别的加热技术才能达到使这些材料熔化的温度；第二，在这样高的温度下必须有防止金属与气氛、坩埚、模具等环境条件发生强烈反应的特别技术手段。
目前，制备难熔金属和合金的技术有三类：
第一类是高温真空烧结技术，其工艺流程包括：将金属制成粒度合适的粉末，将粉末的混合物压制成型，在等静压设备中增大坯料的致密度，在低于材料熔点的温度和真空的条件下将坯料烧结或热压成致密度比较高的材料。在需要板、棒、带、丝等产品的情况下，还需要通过热加工、冷加工改变材料的形状并进一步提高材料的致密性。这种技术的缺点是材料中有孔隙，致密性不理想，气体的含量比较高，而且工艺流程比较长。
第二类是真空能量束冷坩埚熔炼技术，这儿所指的能量束包括电弧束、等离子束、电子束和激光束等。其中，真空电弧熔炼技术，即真空非自耗电弧熔炼技术的应用比较普遍。这类技术通过采用上述各种能量束获得特别高的温度。由于陶瓷材料在这么高的温度下会同金属熔体产生强烈反应，所以这些技术都使用水冷铜坩埚。要说明的是，这儿所说的冷坩埚是一种不分瓣的水冷坩埚。这种技术的 一个 缺点在于能量束集中，炉料在其聚焦位置熔化，但是当能量束转移到其它位置熔化炉料时，在强烈水冷的条件下，刚才熔化的炉料立即就凝固了。因此，用能量束技术熔炼难熔金属，特别是难熔金属的合金时，难以得到成分准确、均匀、组织一致、材质致密的产品。 这种技术的另一个缺点在于在进行铸造时要停止能量束发射，这导致金属液的温度降低，影响铸件的质量 。
第三类是真空冷坩埚感应熔炼技术（以下简称为冷坩埚感应熔炼技术），这是当代最先进的熔炼技术之一。
如图 1 所示，现有的真空冷坩埚感应熔炼设备由冷坩埚 11 '、感应圈 12 '、真空室 13 '、高频或中频的感应电源 14 '、真空 - 充氩系统 15 '、控制柜 16 '和冷却系统 17 '组成。
炉料（图未示）置于冷坩埚 11 '中，由感应电源 14 '送达感应圈 12 '的高频或中频电流所产生的电磁场穿过坩埚壁加热炉料产生熔炼作用。冷坩埚 11 '一般用紫铜制作，电磁场能穿过金属坩埚壁的原因在于它有若干平行于坩埚轴的缝隙。为了使冷坩埚 11 '在熔炼温度下不熔化，坩埚壁通水冷却。在每一坩埚瓣中通有冷却水。
在上述真空冷坩埚感应熔炼设备中，作为加热源的电磁场对炉料的作用范围是整体的，而且能产生强烈的搅拌作用。所以炉料得到了整体熔化、整体悬浮、整体搅拌。这个条件是获得成分准确、均匀、材质致密的产品所必须的。
但是，在坩埚水冷的条件下，炉料的温度很难达到 2000 ℃以上的高温。
本发明要解决的技术问题在于：克服用真空非自耗电弧熔炼等能量束熔炼技术在熔炼难熔金属和合金时物料呈局部熔化，成分的均匀性难以得到保证的缺点，提出一种在熔炼过程使难熔金属和合金整体熔化，成品具有良好的成分均匀性的新技术。利用这种新技术还可以对难熔金属和合金进行各种铸造操作。
为了解决上述技术问题，本发明提出以下技术方案：一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，需要应用一种设备，该设备包括一真空室、一坩埚架、一冷坩埚、一感应圈、一高频或中频的感应电源、一能量束发射头、一能量束发生器、一铸造模具；
该真空室是一个内部中空的封闭容器；
该坩埚架安装在该真空室内；
该冷坩埚安装在该真空室内，该冷坩埚安装在该坩埚架上，该冷坩埚用致密的紫铜制成，该冷坩埚由若干的坩埚瓣组成，坩埚瓣之间的间隙平行于冷坩埚的轴线；
该感应圈安装在该真空室的内部，该感应圈环绕地安装在该冷坩埚的外部；
该高频或中频的感应电源安装在该真空室的外部，该高频或中频的感应电源连接该感应圈并给该感应圈提供电能；
该能量束发射头安装在该真空室内部顶端，位于该冷坩埚的上方，从该能量束发射头发射出的能量束到达该冷坩埚；
该能量束发生器安装在该真空室的外部，该能量束发生器连接该能量束发射头，该能量束发生器能够产生能量束并传输到该能量束发射头；
该铸造模具安装在该冷坩埚的斜下方；
该能量束发生器是非自耗电弧发生装置，上述能量束发射头发射出的能量束是电弧束；或者该能量束发生器是等离子束发射装置，上述能量束发射头发射出的能量束是等离子束；或者该能量束发生器是电子束发射装置，上述能量束发射头发射出的能量束是电子束；或者该能量束发生器是激光发射装置，上述能量束发射头发射出的能量束是激光束；
在该真空室的顶部安装一 KF 接口，然后安装一不锈钢波纹管，然后在该不锈钢波纹管的顶部再安装一 KF 接口，通过这种 KF 接口，能量束发射头真空密封地安装在真空室顶部，而且可以在一定的角度范围内摆动，发射头的摆动能够在一定程度上使能量束形成的局部熔池扩大；
在冷坩埚的上端面装设一片中心有孔的高熔点陶瓷材料制成的隔热挡板，其中心孔的直径大于能量束的直径，在熔炼过程中，隔热挡板能防止能量束轰击到冷坩埚的侧壁，并减少熔池的辐射热损失，加快炉料熔化过程；
该方法包括以下步骤：
步骤 1 ：熔炼：在熔炼过程中，控制感应电源而使该感应圈产生电磁场 B ，控制能量束发生器而使该能量束发射头发出能量束 N ，能量束 N 使冷坩埚中的局部炉料达到高温并熔化形成局部熔池，电磁场 B 整体加热炉料，使局部熔池扩大并获得电磁搅拌，直至全部金属炉料形成成分均匀的整体熔池；
步骤 2 ：倾转铸造：在熔炼结束后，控制能量束发生器而使该能量束发射头停止发射能量束 N ，控制感应电源而使感应圈继续工作维持电磁场 B ，电磁场 B 继续加热熔池，同时移开隔热挡板，倾转冷坩埚，将难熔金属熔体浇注到铸造模具之中。
上述技术方案的进一步限定在于，该熔炼和铸造难熔金属及其合金的设备还包括一真空 - 充氩系统、一冷却系统、一控制柜，该真空 - 充氩系统安装在该真空室的外部，该真空 - 充氩系统给该真空室充入氩气；该冷却系统用来对冷坩埚进行冷却；该控制柜连接该真空室、高频或中频的感应电源、真空 - 充氩系统、冷却系统，并对它们进行控制。
上述技术方案的进一步限定在于，该铸造模具是水冷的紫铜模具，或者是用氧化锆、氮化硼、或氧化镁材料制备的非金属模具。
上述技术方案的进一步限定在于，该铸造模具是用碳化硅和石墨制成的，该铸造模具的内表面有氧化锆、氮化硼、或氧化镁材料的涂层。
为了解决上述技术问题，本发明提出以下技术方案：一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，其应用一种设备，该设备包括一真空室、一坩埚架、一冷坩埚、一感应圈、一高频或中频的感应电源、一能量束发射头、一能量束发生器、一铸造模具、一坩埚塞和一拉杆；
该真空室是一个内部中空的封闭容器；
该坩埚架安装在该真空室内；
该冷坩埚安装在该真空室内，该冷坩埚安装在该坩埚架上，该冷坩埚用致密的紫铜制成，该冷坩埚由若干的坩埚瓣组成，坩埚瓣之间的间隙平行于冷坩埚的轴线；
该冷坩埚包括有一底板，该底板的中心开设有一底铸口；
该感应圈安装在该真空室的内部，该感应圈环绕地安装在该冷坩埚的外部；
该高频或中频的感应电源安装在该真空室的外部，该高频或中频的感应电源连接该感应圈并给该感应圈提供电能；
该能量束发射头安装在该真空室内部顶端，位于该冷坩埚的上方，从该能量束发射头发射出能量束到达该冷坩埚；
该能量束发生器安装在该真空室的外部，该能量束发生器连接该能量束发射头，该能量束发生器能够产生能量束并传输到该能量束发射头；
该铸造模具安装在该真空室内位于该冷坩埚的正下方，该铸造模具的底部开设有一开口；
该坩埚塞连接在该拉杆的顶端，该拉杆插设于该铸造模具的开口中；
该能量束发生器是非自耗电弧发生装置，上述能量束发射头发射出的能量束是电弧束；或者该能量束发生器是等离子束发射装置，上述能量束发射头发射出的能量束是等离子束；或者该能量束发生器是电子束发射装置，上述能量束发射头发射出的能量束是电子束；或者该能量束发生器是激光发射装置，上述能量束发射头发射出的能量束是激光束；
在该真空室的顶部安装一 KF 接口，然后安装一不锈钢波纹管，然后在该不锈钢波纹管的顶部再安装一 KF 接口，通过这种 KF 接口，能量束发射头真空密封地安装在真空室顶部，而且可以在一定的角度范围内摆动，发射头的摆动能够在一定程度上使能量束形成的局部熔池扩大；
在冷坩埚的上端面装设一片中心有孔的高熔点陶瓷材料制成的隔热挡板，其中心孔的直径大于能量束的直径，在熔炼过程中，隔热挡板能防止能量束轰击到冷坩埚的侧壁，并减少熔池的辐射热损失，加快炉料熔化过程；
该方法包括以下步骤：
步骤 1 ：熔炼：在熔炼过程中，控制感应电源而使该感应圈产生电磁场 B ，控制能量束发生器而使该能量束发射头发出能量束 N ，能量束 N 使冷坩埚中的局部炉料达到高温并熔化形成局部熔池，电磁场 B 整体加热炉料，使局部熔池扩大并获得电磁搅拌，直至全部金属炉料形成成分均匀的整体熔池；
步骤 2 ：底铸：在熔炼结束后，控制感应电源和能量束发生器，而使感应圈继续产生电磁场 B 且能量束发射头继续发出能量束 N ，同时打开冷坩埚底部的底铸口，使熔体通过底铸口注入铸造模具中。
上述技术方案的进一步限定在于，该熔炼和铸造难熔金属及其合金的设备还包括一真空 - 充氩系统、一冷却系统、一控制柜，该真空 - 充氩系统安装在该真空室的外部，该真空 - 充氩系统给该真空室充入氩气；该冷却系统用来对冷坩埚进行冷却；该控制柜连接该真空室、高频或中频的感应电源、真空 - 充氩系统、冷却系统，并对它们进行控制。
上述技术方案的进一步限定在于，该铸造模具是水冷的紫铜模具，或者是用氧化锆、氮化硼、或氧化镁材料制备的非金属模具。
上述技术方案的进一步限定在于，该铸造模具是用碳化硅和石墨制成的，该铸造模具的内表面有氧化锆、氮化硼、或氧化镁材料的涂层。
上述技术方案的进一步限定在于，在真空室的顶部增设一个加料器，在真空室的下方增设一个铸造室，将铸造模具置于铸造室中，在真空室和铸造室之间安装一个第一阀门，铸造室的侧壁上安装一个第二阀门。
本发明的有益效果包括以下几点：
1 、对于难熔金属及其合金的而言，本发明克服了在能量束熔炼技术中炉料只能形成局部熔池，难以得到搅拌的缺点，使炉料能得到整体熔化和充分地电磁搅拌，所以产品的成分准确、均匀。这个优点对于制备难熔金属的合金特别重要。
2 、在能量束熔炼技术中，难熔金属及其合金难以整体熔化对于铸造过程造成了重要的困难，即便有较大的熔池，由于在铸造过程要终止能量束发射，这会导致熔体的温度降低，所以成材率低，铸件质量差。本发明在熔炼过程形成了整体的熔池，在铸造过程电磁场和能量束可以共同继续加热，至少电磁场可以继续加热，使金属液在铸造过程维持着较高的温度。所以在本发明中，铸造过程具有很高的成材率，而且铸件的组织一致，材质致密。
3 、本发明的技术在铸造过程还可以采用离心铸造、压力铸造、真空吸铸等其它特种铸造方式，进一步提高铸件的质量。
4 、在本发明中，可以通过采用连续拉锭技术而获得很高的生产效率，还可以通过采用定向凝固技术，制备出难熔金属及其合金的定向结晶材料甚至单晶，或者对难熔金属及其合金进行提纯。
5 、能量束熔炼设备的规格一般都比较小，而本发明的设备可以达到几十公斤 / 炉至几百公斤 / 炉的规模。所以，利用本发明的技术可以大幅度的提高生产效率，可以生产大尺寸的难熔金属和合金产品。
图 1 是现有的真空冷坩埚感应设备的基本结构示意图。
图 2 是本发明带有能量束辅助热源的冷坩埚真空感应熔炼设备的示意图。
图 3 表示一种使发射头可晃动的真空密封装置--波纹管 -KF 接口装置。
图 4 表示采用本发明设备熔炼金属或合金时炉料的状态。
图 5 是在本发明的设备中进行倾转铸造的示意图。
图 6 是在本发明的设备中进行底铸铸造的示意图。
图 7 增设了加料器和底铸室的设备的示意图。
图 8 是在本发明的设备中进行连续加料和连续拉锭的示意图。
图 9 是在本发明的设备中进行定向凝固的示意图。
请参阅图 2 至图 5 ，为了在熔炼后倾转铸造，本发明提出一种熔炼和铸造难熔金属及其合金的设备的第一实施例，其包括一真空室 1 、一坩埚架 3 、一冷坩埚 5 、一感应圈 7 、一高频或中频的感应电源 9 、一能量束发射头 11 、一能量束发生器 13 、一真空 - 充氩系统 15 、一冷却系统 17 、一控制柜 19 、一铸造模具 21 。
该真空室 1 是一个内部中空的封闭容器。
该坩埚架 3 安装在该真空室 1 内。
该冷坩埚 5 安装在该真空室 1 内，该冷坩埚 5 安装在该坩埚架 3 上。
该冷坩埚 5 使用致密的紫铜制成，该冷坩埚 5 由若干的坩埚瓣（图未示）组成，坩埚瓣之间的间隙平行于冷坩埚 5 的轴线。每一坩埚瓣中都通入冷却水进行充分冷却。
该感应圈 7 安装在该真空室 1 的内部，该感应圈 7 环绕地安装在该冷坩埚 5 的外部。
该高频或中频的感应电源 9 安装在该真空室 1 的外部，该高频或中频的感应电源 9 连接该感应圈 7 并给该感应圈 7 提供电能。
该能量束发射头 11 安装在该真空室 1 内部顶端，位于该冷坩埚 5 的上方，从该能量束发射头 11 发射出能量束 N 到达该冷坩埚 5 ，并对位于冷坩埚 5 中的难熔金属炉料进行加热。
上述能量束发射头 11 发射出的能量束 N ，可以是电弧束、等离子束熔炼技术、电子束熔炼技术或激光束。
该能量束发生器 13 安装在该真空室 1 的外部。该能量束发生器 13 连接该能量束发射头 11 。该能量束发生器 13 能够产生能量束并传输到该能量束发射头 11 。
该能量束发生器 13 可以是非自耗电弧发生装置，或者是等离子束发射装置，或者是电子束发射装置，或者是激光发射装置。
请参阅图 3 ，该能量束发射头 11 与真空室 1 的顶部采用真空密封结合，在该真空室 1 的顶部安装一 KF 接口 112 ，然后安装一不锈钢波纹管 114 ，然后在该不锈钢波纹管 114 的顶部再安装一 KF 接口 112 。这样的结构下，该能量束发射头 11 可以在一定的角度范围内晃动。
在冷坩埚 5 的上端面装设一片中心有孔的高熔点陶瓷材料制成的隔热挡板 52 ，其中心孔的直径应该明显大于能量束的直径，使用隔热挡板 52 的目的是防止能量束轰击到冷坩埚 5 的侧壁，并减少辐射热的损失。
该真空 - 充氩系统 15 安装在该真空室 1 的外部，该真空 - 充氩系统 15 给该真空室 1 充入氩气。
该冷却系统 17 用来对冷坩埚 5 进行冷却。
该控制柜 19 连接该真空室 1 、高频或中频的感应电源 9 、真空 - 充氩系统 15 、冷却系统 17 ，并对它们进行控制。
请参阅图 5 ，该铸造模具 21 安装在该冷坩埚 5 的斜下方。
本发明提出一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，需要使用上述设备第一实施例，包括以下步骤：
步骤 1 ：熔炼：在熔炼过程中，控制感应电源 9 而使该感应圈 7 产生电磁场 B ，控制能量束发生器 13 而使该能量束发射头 11 发出能量束 N ，能量束 N 使冷坩埚 5 中的局部炉料达到高温并熔化形成局部熔池，电磁场 B 整体加热炉料，使局部熔池扩大并获得电磁搅拌，直至全部金属炉料形成成分均匀的整体熔池；
步骤 2 ：倾转铸造：在熔炼结束后，控制能量束发生器 13 而使该能量束发射头 11 停止发射能量束 N ，控制感应电源 9 而使感应圈 7 继续工作维持电磁场 B ，电磁场 B 继续加热熔池，同时移开隔热挡板 52 ，倾转冷坩埚 5 ，将难熔金属熔体 100 浇注到铸造模具 21 之中。
请参阅图 6 ，为了在熔炼后底铸，本发明提出一种熔炼和铸造难熔金属及其合金的设备第二实施例，包括与第一实施例所述的设备相同的真空室 1 、坩埚架 3 、感应圈 7 、高频或中频的感应电源 9 、能量束发射头 11 、能量束发生器 13 、真空 - 充氩系统 15 、冷却系统 17 、控制柜 19 。
不同之处是包括有一冷坩埚 31 、一铸造模具 33 、一坩埚塞 35 和一拉杆 37 。
该冷坩埚 31 安装在该真空室 1 内。该感应圈 7 环绕地设在该冷坩埚 31 的外部。
该冷坩埚 31 包括有一底板 312 ，该底板 312 的中心开设有一底铸口 314 。
该铸造模具 33 安装在该真空室 1 内位于该冷坩埚 31 的正下方，该铸造模具 33 的底部开设有一开口 332 。
该坩埚塞 35 连接在该拉杆 37 的顶端，该拉杆 37 插设于该铸造模具 33 的开口 332 中。
本发明提出另一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，需要使用上述设备第二实施例 ，包括以下步骤：
步骤 1 ：熔炼：在熔炼过程中，控制感应电源 9 而使该感应圈 7 产生电磁场 B ，控制能量束发生器 13 而使该能量束发射头 11 发出能量束 N ，能量束 N 使冷坩埚 5 中的局部炉料达到高温并熔化形成局部熔池，电磁场 B 整体加热炉料，使局部熔池扩大并获得电磁搅拌，直至全部金属炉料形成成分均匀的整体熔池；
步骤 2 ：底铸：在熔炼结束后，控制感应电源 9 和能量束发生器 13 ，而使感应圈 7 继续产生电磁场 B 且能量束发射头 11 继续发出能量束 N ，同时打开冷坩埚 5 底部的底铸口 54 ，使熔体通过底铸口 54 注入铸造模具 33 中。
为了在不打开真空室 1 的条件下进行多炉次的熔炼和铸造，可以对设备的第二实施例进一步做结构上的改变，如图 7 所示，在真空室 1 的顶部增设一个加料器 41 ，在加料器 41 中装入待熔炼的难熔金属炉料 100 。在真空室 1 的下方增设一个铸造室 51 ，将铸造模具 33 置于铸造室 51 中。在真空室 1 和铸造室 51 中安装一个第一阀门 53 ，铸造室 51 的侧壁上开设一个第二阀门 55 。
在完成一次铸造操作后，通过第一阀门 53 隔断铸造室 51 和真空室 1 ，打开第二阀门 55 ，取出模具 33 中的铸造材料，然后将铸造室 51 装回真空室 1 的下面，再对铸造室 51 抽真空和充入氩气后打开第一阀门 53 。与此同时，通过加料器 41 向坩埚 31 中加入指定数量的待熔炼的材料，这时就可以开始第二炉材料的熔炼和铸造。按照这种方式，还可以进行更多炉次的熔炼和铸造。
为了提高生产效率，可以在图 2 的设备的基础上增设一连续加料 - 拉锭装置 ( 如图 8 所示 ) ，利用该装置，可以连续加入原料并进行拉锭技术处理。
在续加料 - 拉锭装置的基础上进行改装，可以得到定向凝固装置 ( 如图 9 所示 ) ，它可以使熔炼后的材料在凝固过程形成定向结晶组织或单晶，或者对材料产生提纯作用。
上述设备还可以装备一些操作机构，例如加料机构、搅拌机构、翻锭机构、铸造机构、测温 - 控温系统、氩气净化系统等。
本发明的核心是结合真空冷坩埚感应熔炼技术和真空能量束冷坩埚熔炼技术来熔炼难熔金属和合金。本发明设备的主体是真空冷坩埚感应熔炼炉，并增加了能量束发射头 11 和能量束发生器 13 。能量束技术的特点是温度高，它们能够实现 5000 ℃甚至数万度的高温，所以用这类技术可以熔炼各种难熔金属，包括熔点为 3400 ℃的钨。
熔炼过程由感应电源 9 通过感应圈 7 产生的电磁场 B 和能量束发射头 11 发出的能量束 N 共同完成：电磁场 B 使炉料整体受热，能量束 N 则使局部炉料达到高温和熔化，电磁场 B 的加热和搅拌作用使熔化区逐渐扩大，最后使炉料全部熔化。由于有电磁场 B 的搅拌作用，熔体 100 的成分是均匀的 ( 参看图 4) 。在一般的情况下，可以先启动感应加热系统（感应圈 7 和一高频或中频的感应电源 9 ），使炉料得到整体预热，然后再启动能量束装置（能量束发射头 11 和能量束发生器 13 ），在炉料中形成局部熔池。但是，上述感应圈 7 和能量束发射头 11 ，这两种热源也可以同时启动，同时结束；或者是交替工作；或者是有时共同工作，有时单独工作。
铸造过程不能使用铸铁、铸钢等无水冷的金属模具，也不能使用用氧化铝、氧化硅等材料制备的陶瓷模具。该铸造模具可以使用水冷的金属模具，最好是水冷的紫铜模具，也可以使用用氧化锆、氮化硼、或氧化镁等材料制备的非金属模具，选择非金属材料制备模具的原则是，材料的熔点应该明显高于被熔炼的金属或合金。
碳化硅和石墨也可以用于难熔金属和合金的铸造模具，但是，这些材料会引起金属碳化，所以，用它们制造模具时，模具的内表面最好有氧化锆、氮化硼、或氧化镁等材料的涂层。涂层材料的选择原则与非金属模具材料的选择原则相同。
为了防止高温金属液对模具底面强烈冲刷损坏模具，可以将模具内腔底部的形状设计成带有斜面的形状。
当要求铸造材料缓慢冷却时，应该使用非金属模具，并且在模具的底部、四周或表面设置保温层，或安装加热器。
制备实施例一：金属钽的熔炼以及倾转铸造
将 5kg 金属钽放入图 2 、图 3 和图 4 所示的冷坩埚真空感应熔炼炉的冷坩埚 5 中，中频电源的功率为 250kw ，频率为 15kHz 。在该熔炼炉中，作为辅助热源的能量束发射头 11 和能量束发生器 13 采用了电弧束--钨电极装在冷坩埚 5 的上方，供应电极的直流电源的功率为 100kw 。
设备启动后先抽真空，真空度达到 5 × 10-3Pa 后充入 0.05MPa 的高纯氩，然后启动感应电源 9 ，将炉料 100 加热到 1200 ℃。继续加热直到在炉料 100 中形成温度超过 3600 ℃的熔池。增大感应电源 9 向感应圈 7 输送的功率，并摇动冷坩埚 5 ，晃动能量束发射头 11 ，使熔池的范围逐步增大，最后使全部炉料 100 熔化。
请参阅图 5 ，在熔炼结束时，停止电弧发射，但是电磁场仍然继续工作，同时倾转冷坩埚 5 ，将熔体 100 浇注到水冷的紫铜的铸造模具 21 之中。
制备实施例二：金属钽的熔炼以及底铸
将 5kg 金属钽放入图 2 、图 3 和图 4 所示的冷坩埚真空感应熔炼炉的冷坩埚 5 中，中频电源的功率为 250kw ，频率为 15kHz 。在该熔炼炉中，作为辅助热源的能量束发射头 11 和能量束发生器 13 采用了电弧束--钨电极装在冷坩埚 5 的上方，供应电极的直流电源的功率为 100kw 。
设备启动后先抽真空，真空度达到 5 × 10-3Pa 后充入 0.05MPa 的高纯氩，然后启动感应电源 9 ，将炉料 100 加热到 1200 ℃。继续加热直到在炉料 100 中形成温度超过 3600 ℃的熔池。增大感应电源 9 向感应圈 7 输送的功率，并摇动冷坩埚 5 ，晃动能量束发射头 11 ，使熔池的范围逐步增大，最后使全部炉料 100 熔化。
请参阅图 6 ，在熔炼结束时，电弧 N 和电磁场 B 均继续工作，同时打开冷坩埚 31 底部的底铸口 314 ，使熔体 100 通过底铸口 314 注入水冷的紫铜的铸造模具 33 中。

Claims (9)

  1. 一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，需要应用一种设备，该设备包括一真空室、一坩埚架、一冷坩埚、一感应圈、一高频或中频的感应电源、一能量束发射头、一能量束发生器、一铸造模具；
    该真空室是一个内部中空的封闭容器；
    该坩埚架安装在该真空室内；
    该冷坩埚安装在该真空室内，该冷坩埚安装在该坩埚架上，该冷坩埚用致密的紫铜制成，该冷坩埚由若干的坩埚瓣组成，坩埚瓣之间的间隙平行于冷坩埚的轴线；
    该感应圈安装在该真空室的内部，该感应圈环绕地安装在该冷坩埚的外部；
    该高频或中频的感应电源安装在该真空室的外部，该高频或中频的感应电源连接该感应圈并给该感应圈提供电能；
    该能量束发射头安装在该真空室内部顶端，位于该冷坩埚的上方，从该能量束发射头发射出的能量束到达该冷坩埚；
    该能量束发生器安装在该真空室的外部，该能量束发生器连接该能量束发射头，该能量束发生器能够产生能量束并传输到该能量束发射头；
    该铸造模具安装在该冷坩埚的斜下方；
    该能量束发生器是非自耗电弧发生装置，上述能量束发射头发射出的能量束是电弧束；或者该能量束发生器是等离子束发射装置，上述能量束发射头发射出的能量束是等离子束；或者该能量束发生器是电子束发射装置，上述能量束发射头发射出的能量束是电子束；或者该能量束发生器是激光发射装置，上述能量束发射头发射出的能量束是激光束；
    在该真空室的顶部安装一 KF 接口，然后安装一不锈钢波纹管，然后在该不锈钢波纹管的顶部再安装一 KF 接口，通过这种 KF 接口，能量束发射头真空密封地安装在真空室顶部，而且可以在一定的角度范围内摆动，发射头的摆动能够在一定程度上使能量束形成的局部熔池扩大；
    在冷坩埚的上端面装设一片中心有孔的高熔点陶瓷材料制成的隔热挡板，其中心孔的直径大于能量束的直径，在熔炼过程中，隔热挡板能防止能量束轰击到冷坩埚的侧壁，并减少熔池的辐射热损失，加快炉料熔化过程；
    其特征在于，该方法包括以下步骤：
    步骤 1 ：熔炼：在熔炼过程中，控制感应电源而使该感应圈产生电磁场 B ，控制能量束发生器而使该能量束发射头发出能量束 N ，能量束 N 使冷坩埚中的局部炉料达到高温并熔化形成局部熔池，电磁场 B 整体加热炉料，使局部熔池扩大并获得电磁搅拌，直至全部金属炉料形成成分均匀的整体熔池；
    步骤 2 ：倾转铸造：在熔炼结束后，控制能量束发生器而使该能量束发射头停止发射能量束 N ，控制感应电源而使感应圈继续工作维持电磁场 B ，电磁场 B 继续加热熔池，同时移开隔热挡板，倾转冷坩埚，将难熔金属熔体浇注到铸造模具之中。
  2. 根据权利要求 1 所述的一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，其特征在于，该熔炼和铸造难熔金属及其合金的设备还包括一真空 - 充氩系统、一冷却系统、一控制柜，该真空 - 充氩系统安装在该真空室的外部，该真空 - 充氩系统给该真空室充入氩气；该冷却系统用来对冷坩埚进行冷却；该控制柜连接该真空室、高频或中频的感应电源、真空 - 充氩系统、冷却系统，并对它们进行控制。
  3. 根据权利要求 1 所述的一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，其特征在于，该铸造模具是水冷的紫铜模具，或者是用氧化锆、氮化硼、或氧化镁材料制备的非金属模具。
  4. 根据权利要求 1 所述的一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，其特征在于，该铸造模具是用碳化硅和石墨制成的，该铸造模具的内表面有氧化锆、氮化硼、或氧化镁材料的涂层。
  5. 一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，其应用一种设备，该设备包括一真空室、一坩埚架、一冷坩埚、一感应圈、一高频或中频的感应电源、一能量束发射头、一能量束发生器、一铸造模具、一坩埚塞和一拉杆；
    该真空室是一个内部中空的封闭容器；
    该坩埚架安装在该真空室内；
    该冷坩埚安装在该真空室内，该冷坩埚安装在该坩埚架上，该冷坩埚用致密的紫铜制成，该冷坩埚由若干的坩埚瓣组成，坩埚瓣之间的间隙平行于冷坩埚的轴线；
    该冷坩埚包括有一底板，该底板的中心开设有一底铸口；
    该感应圈安装在该真空室的内部，该感应圈环绕地安装在该冷坩埚的外部；
    该高频或中频的感应电源安装在该真空室的外部，该高频或中频的感应电源连接该感应圈并给该感应圈提供电能；
    该能量束发射头安装在该真空室内部顶端，位于该冷坩埚的上方，从该能量束发射头发射出能量束到达该冷坩埚；
    该能量束发生器安装在该真空室的外部，该能量束发生器连接该能量束发射头，该能量束发生器能够产生能量束并传输到该能量束发射头；
    该铸造模具安装在该真空室内位于该冷坩埚的正下方，该铸造模具的底部开设有一开口；
    该坩埚塞连接在该拉杆的顶端，该拉杆插设于该铸造模具的开口中；
    该能量束发生器是非自耗电弧发生装置，上述能量束发射头发射出的能量束是电弧束；或者该能量束发生器是等离子束发射装置，上述能量束发射头发射出的能量束是等离子束；或者该能量束发生器是电子束发射装置，上述能量束发射头发射出的能量束是电子束；或者该能量束发生器是激光发射装置，上述能量束发射头发射出的能量束是激光束；
    在该真空室的顶部安装一 KF 接口，然后安装一不锈钢波纹管，然后在该不锈钢波纹管的顶部再安装一 KF 接口，通过这种 KF 接口，能量束发射头真空密封地安装在真空室顶部，而且可以在一定的角度范围内摆动，发射头的摆动能够在一定程度上使能量束形成的局部熔池扩大；
    在冷坩埚的上端面装设一片中心有孔的高熔点陶瓷材料制成的隔热挡板，其中心孔的直径大于能量束的直径，在熔炼过程中，隔热挡板能防止能量束轰击到冷坩埚的侧壁，并减少熔池的辐射热损失，加快炉料熔化过程；
    其特征在于，该方法包括以下步骤：
    步骤 1 ：熔炼：在熔炼过程中，控制感应电源而使该感应圈产生电磁场 B ，控制能量束发生器而使该能量束发射头发出能量束 N ，能量束 N 使冷坩埚中的局部炉料达到高温并熔化形成局部熔池，电磁场 B 整体加热炉料，使局部熔池扩大并获得电磁搅拌，直至全部金属炉料形成成分均匀的整体熔池；
    步骤 2 ：底铸：在熔炼结束后，控制感应电源和能量束发生器，而使感应圈继续产生电磁场 B 且能量束发射头继续发出能量束 N ，同时打开冷坩埚底部的底铸口，使熔体通过底铸口注入铸造模具中。
  6. 根据权利要求 5 所述的一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，其特征在于，该熔炼和铸造难熔金属及其合金的设备还包括一真空 - 充氩系统、一冷却系统、一控制柜，该真空 - 充氩系统安装在该真空室的外部，该真空 - 充氩系统给该真空室充入氩气；该冷却系统用来对冷坩埚进行冷却；该控制柜连接该真空室、高频或中频的感应电源、真空 - 充氩系统、冷却系统，并对它们进行控制。
  7. 根据权利要求 5 所述的一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，其特征在于，该铸造模具是水冷的紫铜模具，或者是用氧化锆、氮化硼、或氧化镁材料制备的非金属模具。
  8. 根据权利要求 5 所述的一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，其特征在于，该铸造模具是用碳化硅和石墨制成的，该铸造模具的内表面有氧化锆、氮化硼、或氧化镁材料的涂层。
  9. 根据权利要求 5 所述的一种结合冷坩埚感应熔炼技术与能量束技术的熔炼和铸造难熔金属及其合金的方法，其特征在于，在真空室的顶部增设一个加料器，在真空室的下方增设一个铸造室，将铸造模具置于铸造室中，在真空室和铸造室之间安装一个第一阀门，铸造室的侧壁上安装一个第二阀门。
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CN116103522A (zh) * 2022-08-03 2023-05-12 中国兵器科学研究院宁波分院 一种钛、锆及其合金球形粉末高频感应熔炼铸造方法
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CN115466863A (zh) * 2022-10-21 2022-12-13 哈尔滨工业大学 一种含lpso结构镁合金真空熔炼浇铸一体化装置及制备方法
CN116607028B (zh) * 2023-07-11 2023-09-29 北京中辰至刚科技有限公司 难熔高熵合金的熔炼方法
CN116607028A (zh) * 2023-07-11 2023-08-18 北京中辰至刚科技有限公司 难熔高熵合金的熔炼方法
CN117721334A (zh) * 2024-02-18 2024-03-19 北京理工大学 一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金的制备方法
CN117721334B (zh) * 2024-02-18 2024-04-30 北京理工大学 一种具有均匀等轴细晶组织的TiZrNb系难熔多主元合金的制备方法

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