CN111235399A - Method for preparing titanium rod, titanium alloy and titanium alloy device - Google Patents

Method for preparing titanium rod, titanium alloy and titanium alloy device Download PDF

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CN111235399A
CN111235399A CN202010172805.XA CN202010172805A CN111235399A CN 111235399 A CN111235399 A CN 111235399A CN 202010172805 A CN202010172805 A CN 202010172805A CN 111235399 A CN111235399 A CN 111235399A
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titanium
cooled copper
copper crucible
induction
water
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CN111235399B (en
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王书杰
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Shaanxi Chuang Neng New Material Technology Co.,Ltd.
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王书杰
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16—Remelting metals
    • C22B9/20—Arc remelting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
    • C22B34/1286—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using hydrogen containing agents, e.g. H2, CaH2, hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1295—Refining, melting, remelting, working up of titanium
    • 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

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  • Chemical & Material Sciences (AREA)
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  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a method for preparing a titanium rod, the titanium rod, a titanium alloy and a titanium alloy device, and relates to the technical field of metal smelting and purification. According to the method, titanium oxide or rutile is put into a molten pool for smelting titanium at a high temperature by using an argon-hydrogen plasma arc, the titanium oxide or rutile is dissolved in a pure titanium melt at a high temperature, then nonmetallic elements such as oxygen are removed by using hydrogen, along with the process of putting reduction smelting, the melt in the molten pool flows into an induction water-cooled copper crucible for directional solidification, and then the directional solidification is carried out again by combining the induction water-cooled copper crucible after zone smelting. The impurity elements are removed by repeatedly carrying out separation and purification through zone melting and directional solidification in an induction water-cooled copper crucible, and the purity of the prepared titanium rod is higher through multiple purifications and finally vacuum dehydrogenation of the titanium rod.

Description

Method for preparing titanium rod, titanium alloy and titanium alloy device
Technical Field
The invention relates to the technical field of metal purification and smelting, in particular to a method for preparing a titanium rod, the titanium rod, a titanium alloy and a titanium alloy device.
Background
The metal titanium and the alloy thereof have the characteristics of low density, high specific strength, corrosion resistance, strong biocompatibility and the like, are widely applied to the industries of aerospace, aviation, navigation, weaponry, petroleum, chemical engineering, metallurgy, medicine and the like, and become indispensable strategic resources in national economy. The reserves of titanium in China account for the first world, but the production capacity is seriously insufficient, especially for pure titanium with higher purity. In high-end structural materials, the oxygen content in the titanium alloy can seriously affect the performance of the titanium alloy, and the demand on the titanium alloy with higher purity is huge.
The traditional method for refining the metallic titanium is a Kroll method, the titanium is reduced from a titanium chloride melt mainly through magnesium or sodium, the method is high in energy consumption and heavy in pollution, and the method needs to be developed towards large-scale, automatic and energy-saving directions at present. More than 20 new refining methods are available, such as TiO2By direct reduction (FFC), by calthermic reduction electrolysis (OS),Metal Hydride Reduction (MHR), Armstrong (ITP). TiO 22Due to TiO in the direct reduction (FFC) method2Non-conducting, large current is needed to ionize oxygen atoms in the initial stage of electrolysis, and how to prevent other impurity atoms from being reduced in the titanium reduction process is a difficult problem, and anode burning loss exists. Compared with the Kroll method, the calthermic reduction electrolysis (OS) method has the advantage of energy conservation, but the separation of the titanium product and the electrolyte is extremely difficult. The metal hydride reduction Method (MHR) is to produce titanium powder by the reduction of metal hydride, and the products are titanium, metal oxide and hydrogen. The Armstrong process (ITP) consists essentially of TiCl4Steam is sprayed into excessive molten metal sodium, the method belongs to the upgrading of the Kroll method, the purity of the obtained titanium is high, the titanium is the highest maturity of a new refining method, and how to further reduce the oxygen content is to be further improved.
The method has the disadvantages of high energy consumption and high pollution; or more impurities; or the separation is difficult, and usually only titanium oxide can be singly refined or titanium salt is prepared first, so the process is complex, and the industrialization of titanium refining and purification and the requirement of cost reduction are not facilitated.
Disclosure of Invention
The invention aims to provide a method for preparing a titanium rod, which has the advantages of simple process, environmental protection and energy saving.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method for preparing a titanium rod, characterized by: the method uses a device for preparing the titanium rod, and comprises the following steps:
firstly, circulating water is introduced into the whole system, and the whole system is vacuumized to 10 DEG-1Pa to 10-3Pa, then placing the top end of a high-purity titanium support rod at a balance interface position in a first induction melting water-cooled copper crucible, connecting the high-purity titanium support rod with a lower pull rod, placing an initial pure titanium material in the electrode melting water-cooled copper crucible, starting an argon-hydrogen plasma torch to work, continuously putting titanium oxide or rutile into the electrode melting water-cooled copper crucible through a feeding pipe after the initial pure titanium material is melted and balanced, wherein the surface layer part of the titanium melt reaches 2400 ℃, and oxygen is generated at high temperatureDissolving titanium or rutile in a pure titanium melt, introducing impurities such as oxygen, iron and the like into the titanium melt in an atomic form, dissolving hydrogen atoms in the atmosphere in a furnace body in a titanium molten pool at high temperature, and removing oxygen elements, nitrogen elements and carbon elements in the melt by the hydrogen elements dissolved in the titanium melt; along with the continuous increase of titanium element in the electrode smelting water-cooled copper crucible during smelting, titanium melt in a titanium molten pool overflows and flows into the first induction smelting water-cooled copper crucible, the first induction smelting water-cooled copper crucible is observed through the first observation tube, when the titanium melt overflowing into the first induction smelting water-cooled copper crucible reaches half of the inner space of the first induction smelting water-cooled copper crucible, the induction coil of the water-cooled copper crucible around the first induction smelting water-cooled copper crucible is started, the inflowing melt is continuously in a molten state under the action of electromagnetic induction, and the titanium melt on the high-purity titanium support rod is welded with the titanium melt;
after a melt hump in the first induction smelting water-cooled copper crucible is flush with the upper edge of the first induction smelting water-cooled copper crucible, the lower pull rod continuously moves downwards, along with the movement of the lower pull rod, titanium melt discharged from the bottom of the first induction smelting water-cooled copper crucible is solidified into a titanium rod, according to the movement distance of the lower pull rod, when the original upper end surface position of the high-purity titanium support rod is positioned at the upper end surface of the second induction smelting water-cooled copper crucible, the movement of the lower pull rod is stopped, meanwhile, the feeding in the feeding pipe is stopped, the second induction coil is started to perform induction heating on the titanium rod until the titanium rod is melted and fused, then the lower pull rod is driven to move, after the upper surface of the fused titanium rod on the lower pull rod is flush with a balance interface in the second induction smelting water-cooled copper crucible, the induction coil of the water-cooled copper crucible outside the second induction smelting water-cooled copper crucible is started, and the first clamping guide wheel is started simultaneously to feed the feeding pipe to enable the first induction smelting water-cooled copper The titanium rod in the second induction coil zone continuously solidifies and enters the second induction coil zone, and is heated by the second induction coil to form stable titanium melt liquid drops, and the titanium melt liquid drops fall into a second induction melting water-cooled copper crucible;
observing the melting condition of the titanium rod and the condition in the second induction melting water-cooled copper crucible through a second observation tube, after the hump of the melt in the second induction melting water-cooled copper crucible is flush with the upper edge of the second induction melting water-cooled copper crucible, continuously moving a lower pull rod downwards, solidifying the titanium melt discharged from the bottom of the second induction melting water-cooled copper crucible into the titanium rod, stopping the movement of the lower pull rod when the original upper end surface position of a high-purity titanium support rod is positioned at the upper end surface of a third induction melting water-cooled copper crucible according to the movement distance of the lower pull rod, and simultaneously stopping the feeding in a feeding tube and stopping the induction heating of a second induction coil and the driving of a first clamping guide wheel; starting a fourth induction coil to perform induction heating on the titanium rod until the titanium rod is melted and fused, then driving a lower pull rod to move, stopping the movement of the lower pull rod after the upper surface of the fused titanium rod on the lower pull rod is level with a balance interface in a third induction smelting water-cooled copper crucible, and starting a water-cooled copper crucible induction coil outside the third induction smelting water-cooled copper crucible; feeding materials into a feeding pipe, simultaneously starting a first clamping guide wheel to enable a titanium rod in a first induction melting water-cooled copper crucible to continuously solidify and enter a second induction coil area, simultaneously starting a second clamping guide wheel to enable a titanium rod in a second induction melting water-cooled copper crucible to continuously solidify and enter a fourth induction coil area, heating the titanium rod discharged from the first induction melting water-cooled copper crucible through a second induction coil to form stable titanium melt liquid drops, enabling the titanium melt liquid drops to fall into the second induction melting water-cooled copper crucible, simultaneously heating the titanium rod discharged from the second induction melting water-cooled copper crucible through the fourth induction coil to form stable titanium melt liquid drops, and enabling the titanium melt liquid drops to fall into a third induction melting water-cooled copper crucible;
observing the melting condition of the titanium rod and the condition in the third induction melting water-cooled copper crucible through a third observation tube, after the hump of the melt in the third induction melting water-cooled copper crucible is flush with the upper edge of the third induction melting water-cooled copper crucible, the lower pull rod starts to move downwards along with the downward movement of the lower pull rod, the titanium melt in the third induction melting water-cooled copper crucible is pulled out in the form of the titanium rod, the aim of removing oxygen and other non-metallic impurities from hydrogen is realized, the processes of fractional solidification and impurity removal in the first induction melting water-cooled copper crucible, the second induction melting water-cooled copper crucible and the third induction melting water-cooled copper crucible are realized, when the impurities in the molten pools in the first induction melting water-cooled copper crucible and the second induction melting water-cooled copper crucible are excessive, the first slag collecting pool and the second slag collecting pool are poured, then the whole process is repeated, and finally the obtained titanium rod is subjected to high-temperature vacuum dehydrogenation, and realizing the preparation of the titanium rod.
The further technical scheme is that the method also comprises the following steps: along with the directional solidification of titanium bars in the first induction melting water-cooled copper crucible and the second induction melting water-cooled copper crucible, impurities in molten pools in the first induction melting water-cooled copper crucible and the second induction melting water-cooled copper crucible are more and more, the heating of the second induction coil and the fourth induction coil is stopped by stopping the feeding of the feeding pipe, the movement of the lower pull rod, the first clamping guide wheel and the second clamping guide wheel, and after no molten drop drops in the areas of the titanium molten pool, the second induction coil and the fourth induction coil, melts containing more impurities in the first induction melting water-cooled copper crucible and the second induction melting water-cooled copper crucible are poured into the first slag collecting pool and the second slag collecting pool through the rotary driving motor; the pouring time is selected mainly according to the condition of titanium oxide or rutile with certain impurity content, and the selection scheme is as follows: when the high-purity titanium support rod moves and is conveyed to a balance interface position in a third induction melting water-cooling copper crucible, the movement distance is L, and the melt is poured; or when the high-purity titanium support rod moves for 2L, 3L.
After the melt is poured, rotating and erecting the first induction melting water-cooled copper crucible and the second induction melting water-cooled copper crucible through a water-cooled copper crucible supporting rod; starting feeding of a feeding pipe, simultaneously starting a second induction coil and a fourth induction coil to heat the residual titanium rods clamped at the lower parts of the first induction smelting water-cooled copper crucible and the second induction smelting water-cooled copper crucible to be melted, continuously feeding titanium oxide or rutile into the electrode smelting water-cooled copper crucible through the feeding pipe again, dissolving hydrogen atoms in the atmosphere in a furnace body in a titanium molten pool at high temperature, continuously increasing titanium elements in the electrode smelting water-cooled copper crucible along with smelting, overflowing titanium melt in the titanium molten pool to flow into the first induction smelting water-cooled copper crucible, observing the first induction smelting water-cooled copper crucible through a first observation pipe, and starting driving of a first clamping guide wheel when the highest point of a hump is level with the upper edge of the first induction smelting water-cooled copper crucible so that the residual titanium rods clamped at the lower part of the first induction smelting water-cooled copper crucible start to move downwards, meanwhile, dripping molten drops to a second induction melting water-cooled copper crucible; when the highest point of the hump is level with the upper edge of the second induction melting water-cooled copper crucible, starting the driving of the second clamping guide wheel to ensure that the residual titanium rod clamped at the lower part of the second induction melting water-cooled copper crucible starts to move downwards, simultaneously dripping molten drops into a third induction melting water-cooled copper crucible, and starting the movement of a lower pull rod to ensure that the whole process is carried out stably;
after the titanium rod is prepared, stopping the argon-hydrogen plasma torch, simultaneously stopping feeding in the feeding pipe, stopping induction heating of the second induction coil, driving of the first clamping guide wheel, induction heating of the fourth induction coil and driving of the second clamping guide wheel, stopping the induction coils of the water-cooled copper crucibles around the first induction smelting water-cooled copper crucible and the second induction smelting water-cooled copper crucible, pouring the melt in the first induction smelting water-cooled copper crucible and the second induction smelting water-cooled copper crucible into the first slag accumulation pool and the second slag accumulation pool again, heating the titanium melt in the water-cooled copper crucible induction coil outside the third induction smelting water-cooled copper crucible by the water-cooled copper crucible induction coil outside the third induction smelting water-cooled copper crucible, preventing the titanium melt from being solidified into the third induction smelting water-cooled copper crucible in the process of pulling down the pull rod, and discharging the titanium melt in the third induction smelting water-cooled copper crucible to form the titanium rod along with the pull down of the pull rod, then the furnace is disassembled and the titanium rod is taken out.
The further technical scheme is that after the outer titanium rod is prepared for the first time, the titanium rod is prepared again, and the method comprises the following steps:
firstly, placing the top end of a high-purity titanium support rod at a balance interface position in a third induction melting water-cooled copper crucible, placing an initial pure titanium material in the electrode melting water-cooled copper crucible, starting an argon-hydrogen plasma torch to work, continuously putting titanium oxide or rutile into the electrode melting water-cooled copper crucible through a feeding pipe after the initial pure titanium material is melted and balanced, wherein the surface layer part of the titanium melt reaches 2400 ℃, the titanium oxide or rutile is dissolved in the pure titanium melt at high temperature, impurities such as oxygen, iron and the like enter the titanium melt in an atomic form, hydrogen atoms in the atmosphere in a furnace body are dissolved in a titanium molten pool at high temperature, and the hydrogen elements dissolved in the titanium melt remove oxygen elements, nitrogen elements and carbon elements in the melt; along with the continuous increase of titanium element in the electrode smelting water-cooled copper crucible during smelting, the titanium melt in the titanium molten pool overflows and flows into the first induction smelting water-cooled copper crucible, a water-cooled copper crucible induction coil around the first induction smelting water-cooled copper crucible is started, the inflowing melt is continuously in a melting state under the action of electromagnetic induction, and the residual titanium rod after the titanium rod is smelted for the first time is welded with the titanium melt in the first induction smelting water-cooled copper crucible;
starting a second induction coil to perform induction heating on the titanium rod until the titanium rod is molten, simultaneously starting a first clamping guide wheel to enable the titanium rod in the first induction melting water-cooled copper crucible to continuously solidify and enter a second induction coil area, heating the titanium rod through the second induction coil to form stable titanium melt liquid drops, and enabling the titanium melt liquid drops to fall into the second induction melting water-cooled copper crucible; simultaneously starting a second clamping guide wheel to enable a titanium rod in the second induction melting water-cooled copper crucible to continuously solidify and enter a fourth induction coil area, heating the titanium rod discharged from the second induction melting water-cooled copper crucible through the fourth induction coil to form stable titanium melt liquid drops, and enabling the titanium melt liquid drops to fall into a third induction melting water-cooled copper crucible;
observing the melting condition of a titanium rod at the lower end of the second induction melting water-cooled copper crucible and the condition in the third induction melting water-cooled copper crucible through a third observation tube, driving a lower pull rod to move downwards after a melt hump in the third induction melting water-cooled copper crucible is flush with the upper edge of the third induction melting water-cooled copper crucible, stopping feeding of a feeding tube and working of an argon plasma torch along with the downward pulling of the lower pull rod before the titanium rod reaches a preset length, and stopping heating of a water-cooled copper crucible induction coil, a first induction coil and a second induction coil around the first induction melting water-cooled copper crucible and the second induction melting water-cooled copper crucible, and rotating a first clamping guide wheel and a second clamping guide wheel;
and keeping the induction coil of the water-cooled copper crucible around the third induction melting water-cooled copper crucible to work until all the titanium melt in the third induction melting water-cooled copper crucible is discharged to form a titanium rod.
The further technical scheme is as follows: the furnace body is filled with argon/hydrogen mixed gas, the pressure of the argon/hydrogen mixed gas is 0.05MPa-5MPa, and the volume proportion of hydrogen is 5% -40%.
The further technical scheme is as follows: the initial position of the top end of the high-purity titanium support rod can prevent the top end of the high-purity titanium support rod from being melted, before pure titanium is melted and separated, the position of a solid-liquid interface is found through test melting of the pure titanium, and the position is the initial position of the top end of the high-purity titanium support rod; the high-purity titanium support rod is made of high-purity titanium through casting or forging, and 30% of smelting interface control error is reserved downwards when the high-purity titanium support rod passes through the initial smelting stages of a first induction smelting water-cooled copper crucible, a second induction smelting water-cooled copper crucible and a third induction smelting water-cooled copper crucible in the initial stage so as to avoid the over-smelting phenomenon.
The further technical scheme is as follows: the inner diameter sizes of the first induction melting water-cooled copper crucible, the second induction melting water-cooled copper crucible and the third induction melting water-cooled copper crucible are sequentially increased by 10-20%.
The further technical scheme is as follows: circulating water is introduced into the lower pull rod for cooling.
The further technical scheme is as follows: and an exhaust system and a pressure balance valve are arranged on the inner wall of the furnace body, and the exhaust system is used for discharging gas containing impurities, water vapor, methane gas, ammonia gas and the like out of the furnace body.
The invention also discloses a titanium rod, which is characterized in that: the method for preparing the titanium rod is used for preparing the titanium rod.
The invention also discloses a titanium alloy material, which is characterized in that: the titanium rod was used for preparation.
The invention also discloses a titanium alloy device, which is characterized in that: the titanium alloy material is used for preparation.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: according to the method, titanium oxide or rutile is put into a molten pool for smelting titanium at a high temperature by using an argon-hydrogen plasma arc, then the titanium oxide or rutile is reduced by using hydrogen, along with the reduction smelting, the melt in the molten pool flows into an induction water-cooled copper crucible for directional solidification, and then the melt is combined with the induction water-cooled copper crucible for directional solidification again after zone smelting. The titanium rod is prepared by repeatedly carrying out separation and purification through zone melting and directional solidification in an induction water-cooled copper crucible, and the prepared titanium rod has higher purity through multiple purifications.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a schematic structural diagram of the device according to the embodiment of the invention after the first smelting;
FIG. 2 is a schematic view of a partial structure of an induction water-cooled copper crucible in the apparatus according to the embodiment of the present invention;
FIG. 3 is a schematic structural diagram of an apparatus according to an embodiment of the present invention in an initial stage of preparing a titanium rod by separation and purification;
FIG. 4 is a schematic structural diagram (deslagging) of the device in the end stage of preparing the titanium rod by separation and purification according to the embodiment of the invention;
FIG. 5 is a schematic view of the structure of a guide wheel of the device according to the embodiment of the invention;
FIG. 6 is a schematic view of the structure of an auxiliary wheel of the device according to the embodiment of the present invention;
wherein: 1: an argon-hydrogen plasma torch; 2: a feed pipe; 3: plasma arc; 4: electrode smelting water-cooled copper crucible; 5: a titanium melt; 6: a first alternating current power supply; 7: a second alternating current power supply; 8: a third alternating current power supply; 9: a first induction melting water-cooled copper crucible; 10: a second induction melting water-cooled copper crucible; 11: a third induction melting water-cooled copper crucible; 12: a first clamping guide wheel; 13: a second clamping guide wheel; 14: a first induction coil; 15: a second induction coil; 16: a first slag accumulation pool; 17: a second slag collecting tank; 18: a high-purity titanium support bar; 19: a lower pull rod; 20: a high frequency direct current power supply; 21: a second sight tube; 22: a third observation tube; 23: a first sight tube; 24: a primary purification rod; 25: a secondary purification rod; 26: purifying the rod for the third time; 27-1: a pressure balancing valve; 27-2: an exhaust system; 28: smelting a hump; 29: titanium melt droplets; 30: a water-cooled copper crucible induction coil; 31: a rotary drive motor; 32: a rotating shaft; 33: a guide wheel driving motor; 34 an auxiliary wheel; 35: and a supporting rod of the water-cooled copper crucible smelting system.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
As shown in fig. 1-6, the embodiment of the invention discloses an apparatus for preparing a titanium rod, comprising a furnace body, wherein an argon/hydrogen mixed gas is filled in the furnace body, an argon-hydrogen plasma torch 1 and a feeding pipe 2 are arranged at the top of the furnace body, a power supply input end of the plasma torch 1 is positioned at the outer side of the furnace body, a high-frequency direct current power supply 20 is used for providing a working power supply for the plasma torch, the lower end of the plasma torch is positioned in the furnace body, an electrode smelting water-cooled copper crucible 4 is arranged in the furnace body below the plasma torch, a plasma arc 3 can be generated between the plasma torch and a raw material in the electrode smelting water-cooled copper crucible 4, and the raw material is smelted through the plasma arc 3 to form a titanium melt; one end of the feeding pipe 2 is positioned at the outer side of the furnace body, and the other end of the feeding pipe is positioned at the upper side of the electrode smelting water-cooled copper crucible 4 and is used for conveying raw materials into the electrode smelting water-cooled copper crucible 4;
a first induction melting water-cooling copper crucible 9 is arranged below a liquid outlet of the electrode melting water-cooling copper crucible 4, and the lower end of the first induction melting water-cooling copper crucible 9 is provided with an opening, so that corresponding materials can enter from the upper end opening of the first induction melting water-cooling copper crucible and then are discharged from the lower end opening of the first induction melting water-cooling copper crucible. A first induction coil is arranged on the outer side of the first induction melting water-cooling copper crucible 9, a first alternating current power supply 6 is used for providing a working power supply for the first induction coil, the lower end of the first induction melting water-cooling copper crucible 9 is provided with two first auxiliary wheels 34, the lower side of the first auxiliary wheels 34 is provided with two first clamping guide wheels 12, the inner distance of the two first auxiliary wheels 34 and the inner distance of the two first clamping guide wheels 12 are matched with the inner diameter of the first induction melting water-cooling copper crucible 10, a second induction coil 14 is arranged at the lower side of the first clamping guide wheel 12, the second induction coil 14 supplies power to the first clamping guide wheel through an independent alternating current power supply, a distance is kept between the upper edge of the second induction coil 14 and the lower edge of the first induction melting water-cooled copper crucible 9, the distance is such that the titanium melt in the first induction melting water-cooled copper crucible 9 solidifies first when it is discharged.
The lower part of the second induction coil 14 is provided with a second induction melting water-cooled copper crucible 11, the distance between the lower end of the second induction coil 14 and the upper end of the second induction melting water-cooled copper crucible 10 is D-2D, D is the inner diameter of the water-cooled copper crucible to be melted, the lower end of the second induction melting water-cooled copper crucible 11 is provided with an opening, the outer side of the second induction melting water-cooled copper crucible 10 is provided with a third induction coil, a second alternating current power supply 7 is used for providing a working power supply for the third induction coil, the lower end of the second induction melting water-cooled copper crucible 10 is provided with two second auxiliary wheels, the lower side of the second auxiliary wheels is provided with two second clamping guide wheels 13, the inner distances of the two second auxiliary wheels and the inner distances of the two second clamping guide wheels 13 are matched with the inner diameter of the second induction melting water-cooled copper crucible 10, a fourth induction coil 15 is arranged on the lower side of the second clamping guide wheel 13, and the fourth induction coil 15 supplies power to the second clamping guide wheel through an independent alternating current power supply; a distance is kept between the upper edge of the fourth induction coil 15 and the lower edge of the second induction melting water-cooled copper crucible 10, and the distance is a distance which enables the titanium melt in the second induction melting water-cooled copper crucible 10 to be solidified first when being discharged.
The water-cooled copper crucible 11 is smelted in the below of fourth induction coil 15 is provided with the third induction, just one section distance has between fourth induction coil 15 and the water-cooled copper crucible 11 is smelted in the third induction, the lower extreme of water-cooled copper crucible 11 is smelted in the third induction has the opening, the outside of water-cooled copper crucible 11 is smelted in the third induction is provided with fifth induction coil, and third alternating current power supply 8 is used for fifth induction coil provides working power supply, and high pure titanium bracing piece 18 is located in the furnace body, and its lower extreme is connected with the upper end of pull rod 19, the lower extreme of pull rod 19 extends to outside the furnace body and be connected with pull rod elevating gear's power take off end, high pure titanium bracing piece 18 is in can enter into under the drive of pull rod in the water-cooled copper crucible 9 is smelted in the first induction. After the first smelting of the titanium rod is finished, a section of the titanium rod is reserved in the first induction smelting water-cooled copper crucible 9, and the lower end of the section of the titanium rod extends to a position between the two first clamping guide wheels 12; similarly, a section of titanium rod is reserved in the second induction melting water-cooled copper crucible 10, and the lower end of the section of titanium rod extends to a position between the two second clamping guide wheels 13; molten titanium does not remain in the third induction melting water-cooled copper crucible 11, and the molten titanium is completely discharged from the bottom of the third induction melting water-cooled copper crucible 11 to form a titanium rod.
The furnace body is provided with a pressure balance valve 27-1 and an exhaust system 27-2, the exhaust system (27-2) is used for discharging reduced gases such as impurity gases, water vapor, methane gas, ammonia gas and the like contained in the furnace body out of the smelting system, and the argon-hydrogen mixed gas is discharged by the argon-hydrogen plasma torch 1, so that the pressure in the system can be ensured to be stable.
As shown in fig. 1, 3 and 4, a first observation tube 23 is arranged at the top of the furnace body, the visual field of the first observation tube 23 covers the upper end opening of the electrode smelting water-cooled copper crucible 4, the lower end opening of the feeding tube 2 and the upper end opening of the first induction smelting water-cooled copper crucible 9, and the material conditions in the electrode smelting water-cooled copper crucible 4 and the first induction smelting water-cooled copper crucible 9 are observed through the first observation tube 23; a second observation tube 21 is arranged on the side wall of the furnace body, the visual field of the second observation tube 21 covers the area of the second induction coil 12 and the upper port of the second induction melting water-cooled copper crucible 10, and the melting condition of a titanium rod in the second induction coil 12 and the condition of materials in the second induction melting water-cooled copper crucible 10 are observed through the second observation tube 21; and a third observation tube 22 is arranged on the side wall of the furnace body, and the visual field of the second observation tube 22 covers the fourth induction coil 15 area and the upper port of the third induction melting water-cooling copper crucible 11.
Further, as shown in FIG. 2, a water-cooled copper crucible support rod 35 is arranged on the side wall of the furnace body corresponding to the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10, the inner side end part of the water-cooled copper crucible supporting rod 35 is fixed with a rotary driving motor 31, the power output ends of the two rotary driving motors 31 are respectively and fixedly connected with the protective covers at the outer sides of the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10, the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10 can be horizontally rotated by 90 degrees by the action of the rotary driving motor 31, the guide wheel driving motor 33 is fixed on the outer sides of the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10, the guide wheel driving motor 33 is used for driving the guide wheel on the lower side of the corresponding induction melting water-cooled copper crucible to act.
Further, as shown in fig. 1 to 3, a first slag collecting tank 16 is disposed on a side wall of the furnace body corresponding to the first induction melting water-cooled copper crucible 9, and a second slag collecting tank 17 is disposed on a side wall of the furnace body corresponding to the second induction melting water-cooled copper crucible 10, when the first induction melting water-cooled copper crucible 9 or the second induction melting water-cooled copper crucible 10 rotates under the action of the rotary driving motor 31, the impurity-rich titanium melt in the first induction melting water-cooled copper crucible 9 flows into the first slag collecting tank 16, and the impurity-rich titanium melt in the second induction melting water-cooled copper crucible 10 flows into the second slag collecting tank 17.
The invention also discloses a method for preparing the titanium rod, which comprises the following steps:
firstly, circulating water is introduced into the whole system, and the whole system is vacuumized to 10 DEG-1Pa to 10-3Pa, then placing the top end of a high-purity titanium support rod 18 at a balanced interface position in a first induction melting water-cooled copper crucible 9, connecting the high-purity titanium support rod 18 with a lower pull rod 19, placing an initial pure titanium material in an electrode melting water-cooled copper crucible 4, starting an argon-hydrogen plasma torch 1 to work, continuously putting titanium oxide or rutile into the electrode melting water-cooled copper crucible 4 through a feeding pipe 2 after the initial pure titanium material is melted and balanced, wherein the temperature of the surface layer part of the titanium melt reaches 2400 ℃, the titanium oxide or rutile is dissolved in the pure titanium melt at high temperature, impurities such as oxygen and iron enter the titanium melt in an atomic form, hydrogen atoms in the atmosphere in a furnace body are dissolved in a titanium molten pool 5 at high temperature, and the hydrogen elements dissolved in the titanium melt remove oxygen elements, nitrogen elements and carbon elements in the melt; along with the continuous increase of titanium element in the electrode smelting water-cooled copper crucible 4 during smelting, titanium melt in the titanium molten pool 5 overflows and flows into the first induction smelting water-cooled copper crucible 9, the first induction smelting water-cooled copper crucible 9 is observed through the first observation tube 23, when the titanium melt overflowing into the first induction smelting water-cooled copper crucible 9 reaches half of the inner space thereof, a water-cooled copper crucible induction coil around the first induction smelting water-cooled copper crucible 9 is started, the inflowing melt continues to be in a molten state under the action of electromagnetic induction, and the titanium melt on the high-purity titanium support rod 18 is welded with the titanium melt;
after the hump of the melt in the first induction melting water-cooled copper crucible 9 is level with the upper edge of the first induction melting water-cooled copper crucible 9, the lower pull rod 19 continuously moves downwards, along with the movement of the lower pull rod 19, the titanium melt discharged from the bottom of the first induction melting water-cooled copper crucible 9 is solidified into a titanium rod, according to the movement distance of the lower pull rod 19, when the original upper end surface position of the high-purity titanium support rod 18 is positioned at the upper end surface of the second induction melting water-cooled copper crucible 10, the movement of the lower pull rod 19 is stopped, the feeding in the feeding pipe 2 is stopped at the same time, the second induction coil 14 is started to perform induction heating on the titanium rod until the titanium rod is melted and fused, then the lower pull rod 19 is driven to move, after the upper surface of the fused titanium rod on the lower pull rod 19 is level with the balance interface in the second induction melting water-cooled copper crucible 9, the lower pull rod is stopped to move, the water-cooled copper induction coil outside the second induction melting water, then feeding materials into the feeding pipe 2, starting the first clamping guide wheel 12 at the same time to enable the titanium rod in the first induction melting water-cooled copper crucible 9 to continuously solidify and enter the area of the second induction coil 14, heating the titanium rod through the second induction coil 14 to form stable titanium melt liquid drops 29, and enabling the titanium melt liquid drops 29 to drop into the second induction melting water-cooled copper crucible 10;
observing the melting condition of the titanium rod and the condition in the second induction melting water-cooled copper crucible 10 through a second observation tube 21, after the hump of the melt in the second induction melting water-cooled copper crucible 10 is flush with the upper edge of the second induction melting water-cooled copper crucible 10, continuously moving a lower pull rod 19 downwards, solidifying the titanium melt discharged from the bottom of the second induction melting water-cooled copper crucible 10 into the titanium rod, and stopping the movement of the lower pull rod 19 when the original upper end surface position of a high-purity titanium support rod 18 is positioned at the upper end surface of a third induction melting water-cooled copper crucible 11 according to the movement distance of the lower pull rod 19, and simultaneously stopping the feeding in the feeding tube 2 and stopping the induction heating of a second induction coil 14 and the driving of a first clamping guide wheel 12; starting a fourth induction coil 15 to perform induction heating on the titanium rod until the titanium rod is melted and fused, then driving a lower pull rod 19 to move, stopping the movement of the lower pull rod after the upper surface of the fused titanium rod on the lower pull rod 19 is level with a balance interface in a third induction smelting water-cooled copper crucible 11, and starting a water-cooled copper crucible induction coil outside the third induction smelting water-cooled copper crucible 11; then feeding materials into the feeding pipe 2, simultaneously starting the first clamping guide wheel 12 to enable the titanium rod in the first induction melting water-cooled copper crucible 9 to enter a region of the second induction coil 14 while solidifying continuously, simultaneously starting the second clamping guide wheel 13 to enable the titanium rod in the second induction melting water-cooled copper crucible 10 to enter a region of the fourth induction coil 15 while solidifying continuously, heating the titanium rod discharged from the first induction melting water-cooled copper crucible 9 through the second induction coil 14 to form stable titanium melt liquid drops 29, enabling the titanium melt liquid drops 29 to fall into the second induction melting water-cooled copper crucible 10, simultaneously heating the titanium rod discharged from the second induction melting water-cooled copper crucible 10 through the fourth induction coil 15 to form stable titanium melt liquid drops 29, and enabling the titanium melt liquid drops 29 to fall into the third induction melting water-cooled copper crucible 11;
observing the melting condition of the titanium rod and the condition in the third induction melting water-cooled copper crucible 11 through a third observation tube 22, after the hump of the melt in the third induction melting water-cooled copper crucible 11 is flush with the upper edge of the third induction melting water-cooled copper crucible 11, the lower pull rod 19 starts to move downwards, along with the downward movement of the lower pull rod 19, the titanium melt in the third induction melting water-cooled copper crucible 11 is pulled out in the form of the titanium rod, so that the oxygen and other non-metal impurities are removed from hydrogen, and the impurities are removed through fractional solidification in the first induction melting water-cooled copper crucible 9, the second induction melting water-cooled copper crucible 10 and the third induction melting water-cooled copper crucible 11, when the impurities in the molten pools in the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10 are excessive, the impurities are poured into the first slag collecting pool 16 and the second slag collecting pool 17, and then the whole process is repeated, and finally, the obtained titanium rod is subjected to high-temperature vacuum dehydrogenation to realize the preparation of the titanium rod.
Further, the method comprises the following steps: along with the directional solidification of titanium rods in the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10, impurities in a molten pool in the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10 are more and more, the heating of the second induction coil 14 and the fourth induction coil 15 is stopped by stopping the feeding of the feeding pipe 2, the movement of the pull rod 19, the first clamping guide wheel 12 and the second clamping guide wheel 13, and after no molten drop drops in the areas of the titanium molten pool 5, the second induction coil 14 and the fourth induction coil 15, melts containing more impurities in the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10 are poured into the first slag collecting pool 16 and the second slag collecting pool 17 through the rotary driving motor 31; the pouring time is selected mainly according to the condition of titanium oxide or rutile with certain impurity content, and the selection scheme is as follows: when the high-purity titanium support rod 18 moves and is conveyed to the position of a balance interface in the third induction melting water-cooled copper crucible 11, the movement distance is L, and the melt is poured; or the melt is poured when the high-purity titanium support rod 18 moves for 2L, 3L.
After the melt is poured, the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10 are rotated and erected through the water-cooled copper crucible support rod 35; starting the feeding of the feeding pipe 2, simultaneously starting the second induction coil 14 and the fourth induction coil 15 to heat the residual titanium rods clamped at the lower parts of the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10 to be melted, continuously feeding titanium oxide or rutile into the electrode melting water-cooled copper crucible 4 through the feeding pipe 2 again, dissolving hydrogen atoms in the atmosphere in the furnace body in the titanium molten pool 5 at high temperature, continuously increasing titanium elements in the electrode melting water-cooled copper crucible 4 along with the melting, enabling titanium melt in the titanium molten pool 5 to overflow and flow into the first induction melting water-cooled copper crucible 9, observing the first induction melting water-cooled copper crucible 9 through the first observation pipe 23, starting the driving of the first clamping guide wheel 12 when the highest point of the hump is level with the upper edge of the first induction melting water-cooled copper crucible 9, and enabling the residual titanium rods clamped at the lower part of the first induction melting water-cooled copper crucible 9 to start to move downwards, meanwhile, dripping molten drops to a second induction melting water-cooled copper crucible 10; when the highest point of the hump is level with the upper edge of the second induction melting water-cooled copper crucible 10, starting the driving of the second clamping guide wheel 13, so that the residual titanium rod clamped at the lower part of the second induction melting water-cooled copper crucible 10 starts to move downwards, meanwhile, dripping molten drops into the third induction melting water-cooled copper crucible 10, and starting the movement of the lower pull rod 19, so that the whole process is carried out stably;
after the titanium rod is prepared, stopping the argon-hydrogen plasma torch 1, simultaneously stopping feeding in the feeding pipe 2, stopping induction heating of the second induction coil 14, driving of the first clamping guide wheel 12, induction heating of the fourth induction coil 14 and driving of the second clamping guide wheel 13, stopping the water-cooled copper crucible induction coils around the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10, pouring the melts in the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10 into the first slag collecting pool 16 and the second slag collecting pool 17 again, heating the titanium melt in the water-cooled copper crucible induction coil outside the third induction melting water-cooled copper crucible 11 to prevent the titanium melt from being solidified into the third induction melting water-cooled copper crucible 11 in the process of pulling down the pull rod, and discharging the titanium melt in the third induction melting water-cooled copper crucible 11 to form the titanium rod along with the pulling down of the pull rod, then the furnace is disassembled and the titanium rod is taken out.
After the outer titanium rod is prepared for the first time, the titanium rod is prepared again, and the method comprises the following steps:
firstly, the top end of a high-purity titanium support rod 18 is placed at a balanced interface position in a third induction melting water-cooled copper crucible 11, an initial pure titanium material is placed in an electrode melting water-cooled copper crucible 4, an argon-hydrogen plasma torch 1 is started to work, after the initial pure titanium material is melted and balanced, titanium oxide or rutile is continuously put into the electrode melting water-cooled copper crucible 4 through a feeding pipe 2, the temperature of the surface layer part of the titanium melt reaches 2400 ℃, the titanium oxide or the rutile is dissolved in the pure titanium melt at high temperature, impurities such as oxygen, iron and the like enter the titanium melt in an atomic form, hydrogen atoms in the atmosphere in a furnace body are dissolved in a titanium molten pool 5 at high temperature, and the hydrogen elements dissolved in the titanium melt remove oxygen elements, nitrogen elements and carbon elements in the melt; along with the continuous increase of titanium element in the electrode smelting water-cooled copper crucible 4 during smelting, the titanium melt in the titanium molten pool 5 overflows and flows into the first induction smelting water-cooled copper crucible 9, the water-cooled copper crucible induction coil around the first induction smelting water-cooled copper crucible 9 is started, the inflowing melt is continuously in a molten state under the action of electromagnetic induction, and the residual titanium rods after the titanium rods are smelted for the first time are welded with the titanium melt in the first induction smelting water-cooled copper crucible 9;
the second induction coil 14 is started to perform induction heating on the titanium rod until the titanium rod is molten, meanwhile, the first clamping guide wheel 12 is started to enable the titanium rod in the first induction melting water-cooled copper crucible 9 to continuously solidify and enter the area of the second induction coil 14, the titanium rod is heated by the second induction coil 14 to form stable titanium melt liquid drops 29, and the titanium melt liquid drops 29 drop into the second induction melting water-cooled copper crucible 10; simultaneously starting a second clamping guide wheel 13 to enable the titanium rod in the second induction melting water-cooled copper crucible 10 to continuously solidify and enter the region of a fourth induction coil 15, heating the titanium rod discharged from the second induction melting water-cooled copper crucible 10 through the fourth induction coil 14 to form stable titanium melt liquid drops 29, and dropping the titanium melt liquid drops 29 into a third induction melting water-cooled copper crucible 11;
observing the melting condition of a titanium rod at the lower end of the second induction melting water-cooled copper crucible 10 and the condition in the third induction melting water-cooled copper crucible 11 through a third observation tube 22, driving a lower pull rod 19 to move downwards after a melt hump in the third induction melting water-cooled copper crucible 11 is flush with the upper edge of the third induction melting water-cooled copper crucible 11, stopping feeding of a feeding tube, stopping the work of an argon plasma torch and stopping the heating of water-cooled copper crucible induction coils, a first induction coil 14 and a second induction coil 15 around the first induction melting water-cooled copper crucible 9 and the second induction melting water-cooled copper crucible 10 and the rotation of a first clamping guide wheel and a second clamping guide wheel along with the downward pulling of the lower pull rod before the titanium rod reaches a preset length;
and keeping the water-cooled copper crucible induction coil around the third induction melting water-cooled copper crucible 11 to work until all the titanium melt in the third induction melting water-cooled copper crucible 11 is discharged to form a titanium rod.
Further, the furnace body is filled with argon/hydrogen mixed gas, the pressure of the argon/hydrogen mixed gas is 0.05MPa-5MPa, the volume proportion of hydrogen is 5% -40%, and the initial position of the top end of the high-purity titanium support rod (18) can be prevented from being melted off; the high-purity titanium support rod 18 is made of high-purity titanium through casting or forging, and 30% of smelting interface control error is reserved downwards when the high-purity titanium support rod passes through the initial smelting stages of the first induction smelting water-cooled copper crucible 9, the second induction smelting water-cooled copper crucible 10 and the third induction smelting water-cooled copper crucible 11 in the initial stage so as to avoid the over-smelting phenomenon.
The inside diameter size of the first induction melting water-cooled copper crucible 9, the second induction melting water-cooled copper crucible 10 and the third induction melting water-cooled copper crucible 11 is sequentially increased by 10% -20%, so that the titanium rod can conveniently enter the second induction melting water-cooled copper crucible 10 from the first induction melting water-cooled copper crucible 9, and enter the third induction melting water-cooled copper crucible 11 from the second induction melting water-cooled copper crucible 10. Circulating water is introduced into the lower pull rod 19 for cooling, so that the temperature of the lower pull rod is prevented from being too high.
Furthermore, the titanium alloy can be prepared by the prepared titanium rod, and then related devices can be prepared by the prepared titanium alloy, and the manufacturing device and the method thereof are not repeated herein.
According to the device and the method, titanium oxide or rutile is put into a molten pool for smelting titanium at high temperature by using an argon-hydrogen plasma arc, the titanium oxide or rutile is dissolved in a pure titanium melt at high temperature, then nonmetallic elements such as oxygen are removed by using hydrogen, along with the process of putting reduction smelting, the melt in the molten pool flows into an induction water-cooled copper crucible for directional solidification, and then the directional solidification is carried out again by combining the induction water-cooled copper crucible after zone smelting. The titanium rod is prepared by repeatedly carrying out separation and purification through zone melting and directional solidification in an induction water-cooled copper crucible, and the device and the method have the advantages that the purity of the prepared titanium rod is high through repeated purification and finally vacuum dehydrogenation of the titanium rod.

Claims (10)

1. A method for preparing a titanium rod, characterized by: the method uses a device for preparing the titanium rod, and comprises the following steps:
firstly, circulating water is introduced into the whole system, and the whole system is vacuumized to 10 DEG-1Pa to 10-3Pa, then placing the top end of a high-purity titanium support rod (18) at the position of a balance interface in a first induction melting water-cooled copper crucible (9), connecting the high-purity titanium support rod (18) with a lower pull rod (19), placing an initial pure titanium material in an electrode melting water-cooled copper crucible (4), starting an argon-hydrogen plasma torch (1) to work, continuously putting titanium oxide or rutile into the electrode melting water-cooled copper crucible (4) through a feeding pipe (2) after the initial pure titanium material is melted and balanced, wherein the surface layer part of the titanium melt reaches 2400 ℃, and titanium oxide or rutile is at high temperatureRutile is dissolved in a pure titanium melt, impurities such as oxygen, iron and the like enter the titanium melt in an atomic form, hydrogen atoms in the atmosphere in a furnace body are dissolved in a titanium molten pool (5) at high temperature, and oxygen elements, nitrogen elements and carbon elements in the melt are removed by the hydrogen elements dissolved in the titanium melt; along with the continuous increase of titanium element in the electrode smelting water-cooled copper crucible (4) during smelting, titanium melt in the titanium molten pool (5) overflows and flows into the first induction smelting water-cooled copper crucible (9), the first induction smelting water-cooled copper crucible (9) is observed through the first observation tube (23), when the titanium melt overflowing into the first induction smelting water-cooled copper crucible (9) reaches half of the inner space of the first induction smelting water-cooled copper crucible, a water-cooled copper crucible induction coil around the first induction smelting water-cooled copper crucible (9) is started, the inflowing melt is continuously in a melting state under the action of electromagnetic induction, and the titanium melt on the high-purity titanium support rod (18) is welded with the titanium melt;
after a hump of melt in the first induction melting water-cooled copper crucible (9) is level with the upper edge of the first induction melting water-cooled copper crucible (9), the lower pull rod (19) continuously moves downwards, along with the movement of the lower pull rod (19), titanium melt discharged from the bottom of the first induction melting water-cooled copper crucible (9) is solidified into a titanium rod, when the original upper end surface position of the high-purity titanium support rod (18) is positioned at the upper end surface of the second induction melting water-cooled copper crucible (10) according to the movement distance of the lower pull rod (19), the movement of the lower pull rod (19) is stopped, simultaneously the feeding in the feeding pipe (2) is stopped, the second induction coil (14) is started to inductively heat the titanium rod until the titanium rod is melted and fused, then the lower pull rod (19) is driven to move, after the upper surface of the fused titanium rod on the lower pull rod (19) is level with a balance interface in the second induction melting water-cooled copper crucible (9), stopping the movement of the lower pull rod, starting a water-cooled copper crucible induction coil on the outer side of the second induction melting water-cooled copper crucible (10), then feeding materials into the feeding pipe (2), simultaneously starting the first clamping guide wheel (12) to enable a titanium rod in the first induction melting water-cooled copper crucible (9) to enter a second induction coil (14) area while continuously solidifying, heating the titanium rod through the second induction coil (14) to form stable titanium melt liquid drops (29), and enabling the titanium melt liquid drops (29) to drop into the second induction melting water-cooled copper crucible (10);
observing the melting condition of the titanium rod and the condition in the second induction melting water-cooled copper crucible (10) through a second observation pipe (21), after the hump of the melt in the second induction melting water-cooled copper crucible (10) is flush with the upper edge of the second induction melting water-cooled copper crucible (10), continuously moving a lower pull rod (19) downwards, solidifying the titanium melt discharged from the bottom of the second induction melting water-cooled copper crucible (10) into the titanium rod, and stopping the movement of the lower pull rod (19) according to the movement distance of the lower pull rod (19) when the original upper end surface position of a high-purity titanium support rod (18) is positioned at the upper end surface of a third induction melting water-cooled copper crucible (11), and simultaneously stopping the feeding in a feeding pipe (2) and stopping the induction heating of a second induction coil (14) and the driving of a first clamping guide wheel (12); starting a fourth induction coil (15) to perform induction heating on the titanium rod until the titanium rod is melted and fused, then driving a lower pull rod (19) to move, stopping the lower pull rod to move after the upper surface of the fused titanium rod on the lower pull rod (19) is level with a balance interface in a third induction smelting water-cooled copper crucible (11), and starting a water-cooled copper crucible induction coil on the outer side of the third induction smelting water-cooled copper crucible (11); then feeding materials into the feeding pipe (2) and simultaneously starting the first clamping guide wheel (12) to ensure that the titanium rod in the first induction melting water-cooled copper crucible (9) continuously solidifies and enters the area of the second induction coil (14), and simultaneously starting a second clamping guide wheel (13) to enable the titanium rod in the second induction melting water-cooled copper crucible (10) to continuously solidify and enter the region of a fourth induction coil (15), the titanium rod discharged from the first induction melting water-cooled copper crucible (9) is heated by a second induction coil (14) to form a stable titanium melt liquid drop (29), the titanium melt liquid drop (29) drops into a second induction melting water-cooled copper crucible (10), meanwhile, a titanium rod discharged from the second induction melting water-cooled copper crucible (10) is heated through a fourth induction coil (15) to form a stable titanium melt liquid drop (29), and the titanium melt liquid drop (29) drops into a third induction melting water-cooled copper crucible (11);
observing the melting condition of the titanium rod and the condition in the third induction melting water-cooled copper crucible (11) through a third observation tube (22), after the hump of the melt in the third induction melting water-cooled copper crucible (11) is flush with the upper edge of the third induction melting water-cooled copper crucible (11), the lower pull rod (19) starts to move downwards, along with the downward movement of the lower pull rod (19), the titanium melt in the third induction melting water-cooled copper crucible (11) is pulled out in the form of the titanium rod, thereby realizing the step solidification impurity removal process of removing oxygen and other non-metallic impurities from hydrogen to the first induction melting water-cooled copper crucible (9), the second induction melting water-cooled copper crucible (10) and the third induction melting water-cooled copper crucible (11), when the impurities in the molten pools in the first induction melting water-cooled copper crucible (9) and the second induction melting water-cooled copper crucible (10) are excessive, pouring the impurities into the first slag accumulation pool (16) and the second slag accumulation pool (17), and then repeating the whole process, and finally removing hydrogen from the obtained titanium rod at high temperature in vacuum to realize the preparation of the titanium rod.
2. A method of producing a titanium rod according to claim 1, characterized in that said method further comprises the steps of:
along with the directional solidification of the titanium bars in the first induction melting water-cooled copper crucible (9) and the second induction melting water-cooled copper crucible (10), the impurities in the molten pool in the first induction melting water-cooled copper crucible (9) and the second induction melting water-cooled copper crucible (10) are more and more, the heating of the second induction coil (14) and the fourth induction coil (15) is stopped by stopping the feeding of the feeding pipe (2), the movement of the lower pull rod (19), the first clamping guide wheel (12) and the second clamping guide wheel (13), after no molten drop drips in the areas of the titanium molten pool (5), the second induction coil (14) and the fourth induction coil (15), the method comprises the following steps of pouring melts containing more impurities in a first induction melting water-cooled copper crucible (9) and a second induction melting water-cooled copper crucible (10) into a first slag collecting pool (16) and a second slag collecting pool (17) through a rotary driving motor (31); the pouring time is selected mainly according to the condition of titanium oxide or rutile with certain impurity content, and the selection scheme is as follows: when the high-purity titanium support rod (18) moves and is conveyed to a balance interface position in the third induction melting water-cooled copper crucible (11), the movement distance is L, and the melt is poured; or when the high-purity titanium support rod (18) moves for 2L, 3L.
After the melt is poured, the first induction melting water-cooled copper crucible (9) and the second induction melting water-cooled copper crucible (10) are rotated and erected through a water-cooled copper crucible supporting rod (35); starting the feeding of the feeding pipe (2), simultaneously starting the second induction coil (14) and the fourth induction coil (15) to heat the residual titanium rods clamped at the lower parts of the first induction melting water-cooled copper crucible (9) and the second induction melting water-cooled copper crucible (10) to start melting, continuously feeding titanium oxide or rutile into the electrode melting water-cooled copper crucible (4) through the feeding pipe (2), dissolving hydrogen atoms in the atmosphere in the furnace body into a titanium molten pool (5) at high temperature, continuously increasing titanium elements in the electrode melting water-cooled copper crucible (4) along with the melting, overflowing titanium melt in the titanium molten pool (5) into the first induction melting water-cooled copper crucible (9), observing the first induction melting water-cooled copper crucible (9) through a first observation pipe (23), and when the highest point of a hump is flush with the upper edge of the first induction melting water-cooled copper crucible (9), starting the driving of a first clamping guide wheel (12) to enable the residual titanium rods clamped at the lower part of the first induction melting water-cooled copper crucible (9) to start to move downwards, and simultaneously dripping molten drops to a second induction melting water-cooled copper crucible (10); when the highest point of the hump is level with the upper edge of the second induction melting water-cooled copper crucible (10), starting the driving of the second clamping guide wheel (13), so that the residual titanium rod clamped at the lower part of the second induction melting water-cooled copper crucible (10) starts to move downwards, meanwhile, dripping molten drops into the third induction melting water-cooled copper crucible (10), and starting the movement of a lower pull rod (19), so that the whole process is carried out stably;
after the titanium rod is prepared, stopping the argon-hydrogen plasma torch (1), simultaneously stopping feeding in the feeding pipe (2), stopping induction heating of the second induction coil (14), driving of the first clamping guide wheel (12), induction heating of the fourth induction coil (15) and driving of the second clamping guide wheel (13), stopping the water-cooled copper crucible induction coils around the first induction smelting water-cooled copper crucible (9) and the second induction smelting water-cooled copper crucible (10) from pouring the melt in the first induction smelting water-cooled copper crucible (9) and the second induction smelting water-cooled copper crucible (10) into the first slag collecting pool (16) and the second slag collecting pool (17), heating the titanium melt in the water-cooled copper crucible induction coils outside the third induction smelting water-cooled copper crucible (11) to prevent the titanium melt from being solidified into the third induction smelting water-cooled copper crucible (11) in the process of pulling down the pull rod, along with the downward pulling of the lower pull rod, the titanium melt in the third induction melting water-cooled copper crucible (11) is completely discharged to form a titanium rod, and then the furnace is disassembled to take out the titanium rod.
3. The method for preparing a titanium rod according to claim 1, wherein the step of preparing the titanium rod again after the first preparation of the titanium rod comprises the steps of:
firstly, the top end of a high-purity titanium support rod (18) is placed at a balanced interface position in a third induction melting water-cooled copper crucible (11), an initial pure titanium material is placed in an electrode melting water-cooled copper crucible (4), an argon-hydrogen plasma torch (1) is started to work, after the initial pure titanium material is melted and balanced, titanium oxide or rutile is continuously put into the electrode melting water-cooled copper crucible (4) through a feeding pipe (2), the temperature of the surface layer part of the titanium melt reaches 2400 ℃, the titanium oxide or the rutile is dissolved in the pure titanium melt at high temperature, impurities such as oxygen and iron enter the titanium melt in an atomic form, hydrogen atoms in the atmosphere in a furnace body are dissolved in a titanium molten pool (5) at high temperature, and the hydrogen elements dissolved in the titanium melt remove oxygen elements, nitrogen elements and carbon elements in the melt; along with the continuous increase of titanium element in the electrode smelting water-cooled copper crucible (4) during smelting, titanium melt in the titanium molten pool (5) overflows and flows into the first induction smelting water-cooled copper crucible (9), a water-cooled copper crucible induction coil around the first induction smelting water-cooled copper crucible (9) is started, the inflowing melt is continuously in a melting state under the action of electromagnetic induction, and the residual titanium rod after the titanium rod is smelted for the first time is welded with the titanium melt in the first induction smelting water-cooled copper crucible (9);
starting a second induction coil (14) to perform induction heating on the titanium rod until the titanium rod is molten, simultaneously starting a first clamping guide wheel (12) to enable the titanium rod in the first induction melting water-cooled copper crucible (9) to continuously solidify and enter a second induction coil (14) area, heating the titanium rod through the second induction coil (14) to form stable titanium melt liquid drops (29), and enabling the titanium melt liquid drops (29) to drop into a second induction melting water-cooled copper crucible (10); simultaneously starting a second clamping guide wheel (13) to enable a titanium rod in the second induction melting water-cooled copper crucible (10) to continuously solidify and enter a fourth induction coil (15) area, heating the titanium rod discharged from the second induction melting water-cooled copper crucible (10) through a fourth induction coil (14) to form stable titanium melt liquid drops (29), and dropping the titanium melt liquid drops (29) into a third induction melting water-cooled copper crucible (11);
observing the melting condition of a titanium rod at the lower end of the second induction melting water-cooled copper crucible (10) and the condition in the third induction melting water-cooled copper crucible (11) through a third observation tube (22), driving a lower pull rod (19) to move downwards after a melt hump in the third induction melting water-cooled copper crucible (11) is flush with the upper edge of the third induction melting water-cooled copper crucible (11), stopping feeding of a feeding tube and the work of an argon plasma torch and stopping the heating of water-cooled copper crucible induction coils, a first induction coil (14) and a second induction melting water-cooled copper crucible induction coil (15) around the first induction melting water-cooled copper crucible (9) and the second induction melting water-cooled copper crucible (10) and the rotation of a first clamping guide wheel and a second clamping guide wheel along with the downward pulling of the lower pull rod;
and keeping the induction coil of the water-cooled copper crucible around the third induction melting water-cooled copper crucible (11) to work until all the titanium melt in the third induction melting water-cooled copper crucible (11) is discharged to form a titanium rod.
4. The method of producing a titanium rod according to claim 1, wherein: the furnace body is filled with argon/hydrogen mixed gas, the pressure of the argon/hydrogen mixed gas is 0.05MPa-5MPa, and the volume proportion of hydrogen is 5% -40%.
5. The method of producing a titanium rod according to claim 1, wherein: the initial position of the top end of the high-purity titanium support rod (18) can be prevented from being melted, before pure titanium is melted and separated, the position of a solid-liquid interface is found through test melting of pure titanium, and the position is the initial position of the top end of the high-purity titanium support rod (18); the high-purity titanium support rod (18) is made of high-purity titanium through casting or forging, and when the high-purity titanium support rod passes through the initial smelting stages of the first induction smelting water-cooled copper crucible (9), the second induction smelting water-cooled copper crucible (10) and the third induction smelting water-cooled copper crucible (11) in the initial stage, 30% of smelting interface control errors are reserved downwards so as to avoid the over-smelting phenomenon.
6. The method of producing a titanium rod according to claim 1, wherein: the inner diameter sizes of the first induction melting water-cooled copper crucible (9), the second induction melting water-cooled copper crucible (10) and the third induction melting water-cooled copper crucible (11) are sequentially increased by 10-20%.
7. The method of producing a titanium rod according to claim 1, wherein: circulating water is introduced into the lower pull rod (19) for cooling, an exhaust system (27-2) and a pressure balance valve are arranged on the inner wall of the furnace body, and the exhaust system (27-2) is used for exhausting gas containing impurities, water vapor, methane gas, ammonia gas and the like out of the furnace body.
8. A titanium rod, characterized in that: prepared using the method of any one of claims 1 to 7.
9. A titanium alloy material is characterized in that: the titanium rod prepared according to claim 8.
10. A titanium alloy device, characterized by: the titanium alloy material prepared according to claim 9.
CN202010172805.XA 2020-03-13 2020-03-13 Method for preparing titanium rod, titanium alloy and titanium alloy device Active CN111235399B (en)

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CN111334674A (en) * 2020-03-13 2020-06-26 王书杰 Device for preparing titanium rod, titanium alloy and titanium alloy device
CN113210576A (en) * 2021-05-17 2021-08-06 上海大学 Method and device for producing metal thin strip

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CN113210576A (en) * 2021-05-17 2021-08-06 上海大学 Method and device for producing metal thin strip

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