CN110093515B - Method for preparing low-oxygen high-purity titanium ingot by direct distillation-smelting of salt-sandwiched titanium crystal - Google Patents
Method for preparing low-oxygen high-purity titanium ingot by direct distillation-smelting of salt-sandwiched titanium crystal Download PDFInfo
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- CN110093515B CN110093515B CN201910304141.5A CN201910304141A CN110093515B CN 110093515 B CN110093515 B CN 110093515B CN 201910304141 A CN201910304141 A CN 201910304141A CN 110093515 B CN110093515 B CN 110093515B
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000010936 titanium Substances 0.000 title claims abstract description 97
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 97
- 238000003723 Smelting Methods 0.000 title claims abstract description 34
- 239000013078 crystal Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000001301 oxygen Substances 0.000 title claims abstract description 32
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 32
- 238000004821 distillation Methods 0.000 claims abstract description 40
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 150000003839 salts Chemical class 0.000 claims abstract description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052786 argon Inorganic materials 0.000 claims abstract description 18
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 9
- 238000005266 casting Methods 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000007670 refining Methods 0.000 claims abstract description 5
- 238000003860 storage Methods 0.000 claims abstract description 3
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- 230000006698 induction Effects 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000010894 electron beam technology Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 239000010955 niobium Substances 0.000 claims description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- -1 salt titanium crystals Chemical class 0.000 claims 4
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 238000010891 electric arc Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002985 plastic film Substances 0.000 description 3
- 229920006255 plastic film Polymers 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000008045 alkali metal halides Chemical class 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
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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
- 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
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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
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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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
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- Physics & Mathematics (AREA)
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Abstract
A method for preparing a low-oxygen high-purity titanium ingot by directly distilling and smelting salt-containing titanium crystals, belonging to the field of electrochemical metallurgy. Putting the titanium crystal obtained by molten salt electrolytic refining in a distillation crucible in a distillation-smelting furnace under the protection of inert gas, performing vacuum distillation until the salt inclusion removal rate reaches more than 99%, stopping vacuum distillation, and pouring the titanium crystal obtained by distillation into a smelting crucible in a smelting chamber; heating to 1650-; and taking out the titanium ingot in the ingot casting mold after the temperature of the titanium ingot is reduced to the room temperature, and then carrying out argon protection or vacuum sealing storage to obtain the ultra-low oxygen and ultra-high purity titanium ingot. The invention avoids secondary oxidation of high-purity titanium crystal and loss of powder titanium in wet treatment, greatly improves the purity of the high-purity titanium crystal, reduces oxygen content and improves yield; the process flow is green and clean; the final product is ultra-low oxygen and ultra-high purity titanium ingot, and can meet the titanium requirements of high-end electronic circuits, high-end deep space detection and other high-precision fields.
Description
Technical Field
The invention relates to a method for preparing a low-oxygen high-purity titanium ingot by directly distilling and smelting salt-sandwiched titanium crystals, belongs to the field of electrochemical metallurgy, and particularly can realize the preparation of the low-cost, ultra-low-oxygen and ultra-high-purity titanium ingot.
Background
High purity titanium refers to titanium metal having a titanium content greater than 99.95% or 99.99% (i.e., 3N5 or 4N). The high-purity titanium metal not only has the excellent performance of common titanium metal, but also has excellent elongation percentage (50-60%), area shrinkage percentage (70-80%) and ultralow content of harmful impurity elements which cannot be reached by common titanium. Therefore, high-purity titanium is favored in high-end fields such as high-end microelectronics, advanced aerospace technology, precise very large scale integrated circuits and display screens.
The industrial preparation of high-purity titanium mainly adopts a Kroll method and a molten salt electrolysis method. The former requires high purity of titanium tetrachloride and magnesium as raw materials when preparing high-purity titanium, and simultaneously has high requirement on equipment, so the obtained high-purity titanium has high cost; in addition, the oxygen content of the obtained high-purity titanium product is generally higher than 300ppm, and the development requirement of the current high-new scientific technology is difficult to meet. The fused salt electrolysis method can obtain low-oxygen high-purity titanium crystals with oxygen content lower than 100ppm, and has low cost and great development potential. However, the titanium crystals obtained by electrolysis carry with them a partially molten salt electrolyte, causing problems with salt entrapment.
At present, the salt inclusion for treating the high-purity titanium crystal is mainly treated by a wet method, namely, firstly, the salt inclusion is dissolved and removed by water washing, then, an oxide layer on the surface of the titanium crystal is removed by acid washing, the participative acid is removed by water washing again, and finally, drying and packaging are carried out. This wet treatment process causes wastewater problems, and the alkali metal electrolyte in the wastewater cannot be effectively recovered, which eventually results in electrolyte waste and environmental pollution. Meanwhile, the oxygen content of the product can be increased in the processes of washing and pickling for many times, and the loss of high-purity titanium powder can be caused, so that the yield of the high-purity titanium powder is finally reduced.
Disclosure of Invention
Based on the research background, the invention innovatively provides a method for preparing a low-oxygen high-purity titanium ingot by directly distilling and smelting salt-containing titanium crystals. Compared with the traditional method for treating the titanium crystal with the salt by the wet method, the method disclosed by the invention has the advantages that the titanium crystal with the salt is directly treated by a distillation-smelting method, and the titanium crystal obtained by molten salt electrolysis in the whole process is not contacted with air, so that the oxygen content of the obtained titanium ingot is greatly reduced, and the purity of the titanium ingot is improved; in addition, the whole process does not involve waste water and waste acid, and is environment-friendly; and finally, the halide electrolyte obtained by distillation can be recycled, so that the production cost of the titanium ingot is further reduced, and the ultra-low oxygen and ultra-high purity titanium ingot is finally obtained.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing a low-oxygen high-purity titanium ingot by directly distilling and smelting salt-containing titanium crystals is characterized by comprising the following steps:
the method comprises the following steps: putting the titanium crystal obtained by molten salt electrolytic refining into a distillation crucible in a distillation-smelting furnace under the protection of inert gas;
step two: vacuumizing the distillation chamber to 1-100Pa, and heating the titanium crystal in a distillation crucible to 1000-1600 ℃ by adopting an electric heating mode for vacuum distillation;
step three: stopping vacuum distillation until the salt inclusion removal rate reaches more than 99%, and pouring titanium crystals obtained by distillation into a smelting crucible in a smelting chamber by rotating a distillation crucible in the furnace;
step four: heating the titanium crystal in the melting crucible to 1650-2000 ℃ in an electron beam, electric arc or induction heating mode to be in a molten state;
step five: injecting the titanium crystal in a molten state in the melting crucible into an ingot casting mold in a mode of rotating the melting crucible;
step six: and taking out the titanium ingot in the ingot casting mold after the temperature of the titanium ingot is reduced to the room temperature, and then carrying out argon protection or vacuum sealing storage to obtain the ultra-low oxygen and ultra-high purity titanium ingot.
Further, the inert gas in the first step is argon or helium; the distillation-smelting furnace is integrated, the distillation chamber is arranged right above the smelting chamber, and a condensing chamber is arranged right above the distillation chamber and used for collecting and condensing the obtained salt; the distillation crucible is made of high-melting-point metals such as molybdenum, tantalum, niobium, hafnium, zirconium and the like.
Further, selecting the vacuum degree and the temperature in the second step so as not to evaporate the high-purity titanium crystal to a zero boundary point, and stopping distillation when the salt inclusion rate in the high-purity titanium crystal is removed by more than 99%; the heating mode selected can be resistance heating or induction heating.
Further, the rotation of the distillation crucible in the third step is realized by means of a pulley at the bottom of the distillation crucible and a rotating mechanical structure; and the rotation process is realized under the protection of vacuum or inert gas argon.
Further, the crucible for smelting in the fourth step is a copper crucible, and the crucible is provided with a water-cooling protection device to prevent the crucible from being melted; the heating mode of the high-purity titanium crystal can be electron beam heating, and can also be electric arc or induction heating; when electron beam heating is selected, heating is needed under the condition that the vacuum degree is less than 50Pa, and arc or induction heating is carried out under the protection of argon.
Furthermore, the rotation of the smelting crucible in the fifth step is realized through a pulley at the bottom of the crucible and a rotating mechanical structure; and the rotation process is realized under the protection of vacuum or inert gas argon.
Further, the ingot casting mold in the sixth step is made of copper and is provided with a water cooling device for protecting the mold and rapidly cooling the titanium ingot; the obtained ultra-low oxygen and ultra-high purity titanium ingot is vacuum-packed or argon-protected packed by plastic or metal, so that the titanium ingot is prevented from contacting with air.
Compared with the prior art, the invention has the following beneficial effects:
1) in the whole process, the titanium crystal does not contact with air, so that the oxygen content of the obtained titanium ingot can be greatly reduced, and the purity of the titanium ingot is improved;
2) the method does not involve waste water and waste acid, and is environment-friendly;
3) and the alkali metal halide electrolyte obtained by distillation can be recycled, so that the production cost of the titanium ingot is further reduced.
Drawings
FIG. 1 is a schematic view of a direct distillation-melting apparatus for bracketing titanium crystals in example 1.
1. Vacuum and argon pipelines; 2. a valve for collecting distilled impurities and molten salt; 3. vacuum and argon systems; 4. a condensing chamber; 5. a charging valve; 6. a distillation chamber; 7. a distillation crucible; 8. a smelting heat source; 9. a smelting chamber; 10. smelting a crucible; 11. a casting ingot mould; 12. a dummy bar head; 13. and (4) a bracket.
Detailed Description
The present invention will be described in more detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
And stripping and collecting the titanium crystal obtained by molten salt electrolytic refining from the cathode under the protection of argon gas blowing. Subsequently, the titanium crystal was charged into a tantalum distillation crucible in a distillation-melting furnace, and vacuum distillation was carried out at a vacuum degree of 10Pa and a temperature of 1200 ℃. After 2h of distillation, the distillation was stopped and high purity argon was introduced into the furnace. The titanium crystals in the distillation crucible are then poured into a copper water-cooled melting crucible in the melting chamber by internal mechanical structure. Heating the titanium crystal in the melting crucible to 1800 ℃ by adopting an electron beam heating mode, and preserving the heat for 30 min. And injecting the molten high-purity titanium liquid into the copper water-cooling pouring mold through a mechanical device in the furnace. And finally, when the titanium ingot is cooled to room temperature, collecting the titanium ingot through a dummy ingot head, and sealing and storing the titanium ingot in an aluminum-plastic film to obtain the ultra-low oxygen and ultra-high purity titanium ingot with the oxygen content of less than 50ppm and the purity of more than 6N. FIG. 1 is a schematic view of a direct distillation-melting apparatus for intercalated titanium crystals according to the present example.
Example 2
And collecting the cathode titanium crystals under the protection of helium gas blowing. Subsequently, the titanium crystal was charged into a distillation crucible made of molybdenum in a distillation-melting furnace, and vacuum distillation was carried out at a vacuum degree of 20Pa and a temperature of 1100 ℃. After 3 hours of distillation, the distillation was stopped and high purity argon was introduced into the furnace. The titanium crystals in the distillation crucible are then poured into a copper water-cooled melting crucible in the melting chamber by internal mechanical structure. Heating the titanium crystal in the melting crucible to 1700 ℃ by adopting an electric arc heating mode, and preserving the heat for 1 h. And injecting the molten high-purity titanium liquid into the copper water-cooling pouring mold through a mechanical device in the furnace. And finally, when the titanium ingot is cooled to room temperature, collecting the titanium ingot through a dummy ingot head, and sealing and storing the titanium ingot in a plastic film to obtain the ultra-low oxygen and ultra-high purity titanium ingot with the oxygen content of less than 50ppm and the purity of more than 5N.
Example 3
And stripping and collecting the titanium crystal obtained by molten salt electrolytic refining from the cathode under the protection of argon gas blowing. Subsequently, the titanium crystal was charged into a zirconium distillation crucible in a distillation-melting furnace, and vacuum distillation was carried out at a vacuum degree of 20Pa and a temperature of 1000 ℃. After 5h of distillation, the distillation was stopped and high purity argon was introduced into the furnace. Meanwhile, electrolyte obtained by condensation is collected and returned to the electrolytic furnace for continuous use. Titanium crystals in the distillation crucible are poured into a copper water-cooling smelting crucible in the smelting chamber through an internal mechanical structure. Heating the titanium crystal in the melting crucible to 1700 ℃ by adopting an induction heating mode, and preserving the heat for 2 h. And injecting the molten high-purity titanium liquid into the copper water-cooling pouring mold through a mechanical device in the furnace. And finally, when the titanium ingot is cooled to room temperature, collecting the titanium ingot through a dummy ingot head, and sealing and storing the titanium ingot in a plastic film to obtain the ultra-low oxygen and ultra-high purity titanium ingot with the oxygen content of less than 50ppm and the purity of more than 6N.
It should be noted that, according to the above embodiments of the present invention, those skilled in the art can fully implement the full scope of the present invention as defined by the independent claims and the dependent claims, and implement the processes and methods as the above embodiments; and the invention has not been described in detail so as not to obscure the present invention.
The above description is only a part of the embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (5)
1. A method for preparing a low-oxygen high-purity titanium ingot by directly distilling and smelting salt-containing titanium crystals is characterized by comprising the following steps:
the method comprises the following steps: putting the titanium crystal obtained by molten salt electrolytic refining into a distillation crucible in a distillation-smelting furnace under the protection of inert gas;
step two: vacuumizing the distillation chamber to 1-100Pa, and heating the titanium crystal in a distillation crucible to 1000-1600 ℃ for vacuum distillation;
step three: stopping vacuum distillation until the salt inclusion removal rate reaches more than 99%, and pouring titanium crystals obtained by distillation into a smelting crucible in a smelting chamber by rotating a distillation crucible in the furnace;
step four: heating the titanium crystal in the melting crucible to 1650-2000 ℃ to be in a molten state;
step five: injecting the titanium crystal in a molten state in the melting crucible into an ingot casting mold in a mode of rotating the melting crucible;
step six: after the titanium ingot in the ingot casting mold is cooled to room temperature, taking out the titanium ingot, and then carrying out argon protection or vacuum sealing storage to obtain an ultra-low oxygen and ultra-high purity titanium ingot;
the inert gas in the first step is argon or helium; the distillation-smelting furnace is integrated, the distillation chamber is arranged right above the smelting chamber, and a condensing chamber is arranged right above the distillation chamber and used for collecting and condensing the obtained salt; the distillation crucible is made of high-melting-point metals such as molybdenum, tantalum, niobium, hafnium and zirconium;
selecting the vacuum degree and temperature in the second step so as not to evaporate the high-purity titanium crystal to zero, and stopping distillation when the salt inclusion rate in the high-purity titanium crystal is removed by more than 99%; the heating mode selected is electric heating or resistance heating or induction heating.
2. The method for preparing the low-oxygen high-purity titanium ingot by direct distillation-smelting of the intercalated salt titanium crystals as claimed in claim 1, wherein the rotation of the distillation crucible in the third step is realized by a pulley at the bottom of the distillation crucible and a rotating mechanical structure; and the rotation process is realized under the protection of vacuum or inert gas argon.
3. The method for preparing the low-oxygen high-purity titanium ingot by direct distillation-smelting of the intercalated salt titanium crystals as claimed in claim 1, wherein the smelting crucible in the fourth step is a copper crucible, and the crucible is provided with a water cooling protection device to prevent the crucible from being melted; the heating mode of the high-purity titanium crystal is as follows: electron beam heating, arc heating or induction heating; when electron beam heating is selected, heating is needed under the condition that the vacuum degree is less than 50Pa, and arc or induction heating is carried out under the protection of argon.
4. The method for preparing the low-oxygen high-purity titanium ingot by direct distillation-smelting of the intercalated salt titanium crystals as claimed in claim 1, wherein the rotation of the smelting crucible in the fifth step is realized by a pulley at the bottom of the crucible and a rotating mechanical structure; and the rotation process is realized under the protection of vacuum or inert gas argon.
5. The method for preparing the low-oxygen high-purity titanium ingot by direct distillation-smelting of the intercalated salt titanium crystals as claimed in claim 1, wherein in the sixth step, the ingot casting mold is made of copper and is provided with a water cooling device for protecting the mold and rapidly cooling the titanium ingot; the obtained ultra-low oxygen and ultra-high purity titanium ingot is vacuum-packed or argon-protected packed by plastic or metal, so that the titanium ingot is prevented from contacting with air.
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