CN110093515A - A method of the brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot - Google Patents
A method of the brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot Download PDFInfo
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- CN110093515A CN110093515A CN201910304141.5A CN201910304141A CN110093515A CN 110093515 A CN110093515 A CN 110093515A CN 201910304141 A CN201910304141 A CN 201910304141A CN 110093515 A CN110093515 A CN 110093515A
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- titanium
- distillation
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- 239000010936 titanium Substances 0.000 title claims abstract description 112
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 111
- 238000002844 melting Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 40
- 150000003839 salts Chemical class 0.000 title claims abstract description 31
- 206010021143 Hypoxia Diseases 0.000 title claims abstract description 13
- 208000018875 hypoxemia Diseases 0.000 title claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000013078 crystal Substances 0.000 claims abstract description 35
- 230000008018 melting Effects 0.000 claims abstract description 31
- 239000001301 oxygen Substances 0.000 claims abstract description 21
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 21
- 229910052786 argon Inorganic materials 0.000 claims abstract description 20
- 238000004821 distillation Methods 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 19
- 238000003723 Smelting Methods 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- 238000007670 refining Methods 0.000 claims abstract description 5
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 5
- 238000007789 sealing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 238000010891 electric arc Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 238000010894 electron beam technology Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 229920003023 plastic Polymers 0.000 claims description 4
- 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 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
- 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
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 229910052571 earthenware Inorganic materials 0.000 claims 1
- 238000005485 electric heating Methods 0.000 claims 1
- 238000009461 vacuum packaging Methods 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 10
- 238000004140 cleaning Methods 0.000 abstract description 2
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 238000005868 electrolysis reaction Methods 0.000 description 6
- PTVDYARBVCBHSL-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu] PTVDYARBVCBHSL-UHFFFAOYSA-N 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000010025 steaming Methods 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 239000012535 impurity Substances 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
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 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
Classifications
-
- 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
-
- 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
-
- 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
Abstract
A method of the brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot, belongs to electrochemistry field of metallurgy.Stop vacuum distillation for being atmospherically distilled to when folder salt removal rate reaches 99% or more in distillation crucible that titanium crystal obtained by fused-salt electrolytic refining is placed under inert gas protection in distillation-smelting furnace, distillation gained titanium crystal is poured into the indoor melting kettle of melting；It is heated to 1650-2000 DEG C, will be injected in ingot mold in such a way that the titanium crystal of molten condition is by rotation melting kettle in melting kettle；It is taken out after titanium ingot in ingot mold is cooled to room temperature, is then saved in argon gas protection or vacuum sealing, obtain Ultra Low-oxygen, ultra-pure titanium ingot.The invention avoids the losses of the secondary oxidation of titanium crystal high-purity in wet-treating and powder titanium, greatly improve the purity of high-purity titanium crystal, reduce oxygen content, improve recovery rate；Process flow green, cleaning；Final products therefrom is Ultra Low-oxygen, ultra-pure titanium ingot, can meet the titanium demand in the high-precision pointed collar domain such as high-end electronic circuit and tip deep space exploration.
Description
Technical field
The present invention relates to the methods that a kind of brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot, belong to electrochemistry
Field of metallurgy is specific that low cost, the preparation of Ultra Low-oxygen, ultra-pure titanium ingot can be achieved.
Background technique
High purity titanium refers to that Ti content is higher than the titanium of 99.95% or 99.99% (i.e. 3N5 or 4N).High-purity titanium is not
Only possess excellent performance possessed by common titanium, meanwhile, excellent elongation percentage (50-60%), the contraction percentage of area (70-
80%) and the objectionable impurities elements of super low loading are that common titanium can not be reached.Therefore, high purity titanium is in high-end microelectronics, point
Hold space technology, accurate super large-scale integration and display screen etc. high-end fields by favor.
The preparation of industrialization of high purity titanium is mainly based on Kroll method and fused salt electrolysis process.The former wants when preparing high purity titanium
Raw material titanium tetrachloride and magnesium is asked to have higher purity, while it is to the more demanding of equipment, therefore gained high purity titanium is at high cost
It is high；In addition, the high-purity titanium products oxygen content of gained is generally higher than 300ppm, it is difficult to which the development for meeting current high-and-new science and technology is wanted
It asks.Fused salt electrolysis process can obtain hypoxemia, the high-purity titanium crystal that oxygen content is lower than 100ppm, and its is low in cost, great development
Potentiality.However, electrolysis gained titanium crystal can carry part molten salt electrolyte, folder salt problem is caused.
Currently, the folder salt for handling high-purity titanium crystal mainly takes wet-treating, i.e., salt is pressed from both sides using washing dissolution removal first,
Titanium crystalline substance surface oxide layer is then removed using pickling, acid is participated in using washing removal again, finally drying encapsulation.At this wet process
Reason process will cause wastewater problem, and the alkali metal electrolysis matter in the waste water can not be recycled effectively, ultimately cause the wave of electrolyte
Take and the pollution of environment.Meanwhile repeatedly washing, acid cleaning process not only will increase product oxygen content, while will cause high purity titanium
The loss of powder finally reduces its recovery rate.
Summary of the invention
Based on the studies above background, present invention novelty proposes that a kind of brilliant directly distillation-melting of folder salt titanium prepares hypoxemia
The method of high purity titanium ingot.Relative to the method for conventional wet processing folder salt titanium crystal, the present invention is directlyed adopt salt titanium crystal is pressed from both sides
The processing of distillation-melting method, in whole process titanium crystal obtained by molten-salt electrolysis will not ingress of air, therefore can greatly reduce
The oxygen content of gained titanium ingot, improves its purity；In addition, will not relate to waste water, spent acid in whole flow process, it is environmental-friendly；Finally, steaming
Evaporating gained halide electrolyte can reuse, to further decrease titanium ingot production cost, finally obtain Ultra Low-oxygen, superelevation
Pure titanium ingot.
To achieve the above object, the present invention the following technical schemes are provided: a kind of brilliant direct distillation-melting of folder salt titanium prepare it is low
The method of oxygen high purity titanium ingot, it is characterised in that the following steps are included:
Step 1: titanium crystal obtained by fused-salt electrolytic refining is placed in the steaming in distillation-smelting furnace under inert gas protection
It evaporates in crucible；
Step 2: being evacuated to 1-100Pa for distillery, and titanium crystal is then being distilled crucible using electrically heated mode
Inside it is heated to 1000-1600 DEG C of vacuum distillation；
Step 3: it is atmospherically distilled to when folder salt removal rate reaches 99% or more and stops vacuum distillation, and by turning in furnace
Dynamic distillation crucible pours into distillation gained titanium crystal in the indoor melting kettle of melting；
Step 4: the titanium crystal in melting kettle is heated to 1650- by the way of electron beam, electric arc or induction heating
2000 DEG C, be in molten condition；
Step 5: ingot mould will be injected in such a way that the titanium crystal of molten condition is by rotation melting kettle in melting kettle
In tool；
Step 6: taking out after titanium ingot in ingot mold is cooled to room temperature, then saves in argon gas protection or vacuum sealing,
Obtain Ultra Low-oxygen, ultra-pure titanium ingot.
Further, inert gas is argon gas or helium in the step 1；Distillation-smelting furnace is integrated, distillery
It is placed in the surface of working chamber, furthermore the upper part setting condensation chamber of distillery presss from both sides salt for collecting condensation gained；Distill crucible
It is process for high melting point metal molybdenum, tantalum, niobium, hafnium, zirconium etc..
Further, the selection of the step 2 vacuum degree and temperature works as height not make high purity titanium crystalline substance be evaporated to 1 boundary's point
Folder salt rate in pure titanium crystal stops distillation when removing 99% or more；Selected heating method can may be sense for resistance heating
It should heat.
Further, the rotation that crucible is distilled in the step 3 is mechanical by the pulley of distillation crucible bottom and rotation
Structure is realized；And rotation process is realized under the protection of vacuum or inert gas argon gas.
Further, melting kettle is copper crucible in the step 4, and the crucible has water-cooled protecting device, to prevent
Crucible is melted；The heating method of high purity titanium crystalline substance can heat for electron beam, be also possible to electric arc or induction heating；Select electronics
It needs to be heated in the case where vacuum degree is less than 50Pa when Shu Jiare, electric arc or induction heating then add under protection of argon gas
Heat.
Further, the rotation of melting kettle passes through crucible bottom in the step 5 pulley and rotation mechanical structure
It realizes；And rotation process is realized under the protection of vacuum or inert gas argon gas.
Further, ingot mold is copper in the step 6, and has water cooling plant, for protecting mold, and is made
Titanium ingot is quickly cooled down；Gained Ultra Low-oxygen, ultra-pure titanium ingot is using plastics or metal vacuum is packed or argon gas protective packaging, thus
Avoid contact of the titanium ingot with air.
Compared with the existing technology, beneficial effects of the present invention are as follows:
1), in whole process titanium crystal will not ingress of air, therefore can greatly reduce gained titanium ingot oxygen content, improve
Its purity；
2) waste water, spent acid, be will not relate to, it is environmental-friendly；
3), distillation gained alkali halide electrolyte can reuse, and be produced into further decrease titanium ingot
This.
Detailed description of the invention
Fig. 1 is the brilliant directly distillation-smelting apparatus schematic diagram of the folder salt titanium of embodiment 1.
1, vacuum and argon gas pipeline；2, it distills impurity and fused salt collects valve；3, vacuum and argon system；4, condensation chamber；
5, feed valve；6, distillery；7, crucible is distilled；8, melting heat source；9, working chamber；10, melting kettle；11, ingot mold；
12, dummy bar head；13, bracket.
Specific embodiment
The present invention will be described in more detail below by specific embodiment, but protection scope of the present invention is not limited
In these embodiments.
Embodiment 1
Under argon gas blowing protection, titanium crystal obtained by fused-salt electrolytic refining is removed into collection from cathode.Then, by the titanium
Crystal is added in the tantalum system distillation crucible in distillation-smelting furnace, and vacuum steaming is carried out at vacuum degree 10Pa, 1200 DEG C of temperature
It evaporates.Stop distilling after distillation 2h, high-purity argon gas is passed through into furnace.The titanium in crucible then will be distilled by internal mechanical structure
Crystal pours into the indoor copper water cooling melting kettle of melting.Using electron beam heating method by the titanium crystal in melting kettle
1800 DEG C are heated to, and keeps the temperature 30min.Molten high purity titanium liquid is injected into copper water cooling by mechanical device in furnace and pours mold
It is interior.Finally, titanium ingot is collected by dummy bar head, and is sealed in aluminum plastic film, oxygen is obtained and contains when titanium ingot is cooled to room temperature
Amount is lower than 50ppm, and purity is higher than Ultra Low-oxygen, the ultra-pure titanium ingot of 6N.Fig. 1 is that this example presss from both sides the brilliant directly distillation of salt titanium-melting dress
Set schematic diagram.
Embodiment 2
Under helium blowing protection, cathode titanium crystal is collected.Then, which is added in distillation-smelting furnace
Molybdenum system is distilled in crucible, and is evaporated in vacuo at vacuum degree 20Pa, 1100 DEG C of temperature.Stop distilling after distillation 3h, to
High-purity argon gas is passed through in furnace.The titanium crystal distilled in crucible is then poured by the indoor copper of melting by internal mechanical structure
In water cooling melting kettle.The titanium crystal in melting kettle is heated to 1700 DEG C using electric arc heated mode, and keeps the temperature 1h.It will melt
High purity titanium liquid injects copper water cooling by mechanical device in furnace and pours in mold.Finally, passing through when titanium ingot is cooled to room temperature
Dummy bar head collects titanium ingot, and is sealed in plastic foil, obtains oxygen content lower than 50ppm, Ultra Low-oxygen of the purity higher than 5N,
Ultra-pure titanium ingot.
Embodiment 3
Under argon gas blowing protection, titanium crystal obtained by fused-salt electrolytic refining is removed into collection from cathode.Then, by the titanium
Crystal is added in the zirconium system distillation crucible in distillation-smelting furnace, and vacuum steaming is carried out at vacuum degree 20Pa, 1000 DEG C of temperature
It evaporates.Stop distilling after distillation 5h, high-purity argon gas is passed through into furnace.Meanwhile condensation gained electrolyte being collected, and return to electrolysis
It is continued to use in furnace.The titanium crystal distilled in crucible is poured into the indoor copper water cooling melting of melting by internal mechanical structure
In crucible.The titanium crystal in melting kettle is heated to 1700 DEG C using induction heating mode, and keeps the temperature 2h.By molten high purity titanium liquid
Body injects copper water cooling by mechanical device in furnace and pours in mold.Finally, when titanium ingot is cooled to room temperature, it will by dummy bar head
Titanium ingot is collected, and is sealed in plastic foil, obtains oxygen content lower than 50ppm, purity is higher than Ultra Low-oxygen, the ultra-pure titanium of 6N
Ingot.
It should be noted that those skilled in the art are that this hair may be implemented completely according to the various embodiments described above of the present invention
Bright independent claims and the full scope of appurtenance, realize process and the same the various embodiments described above of method；And the present invention is not
It elaborates and partly belongs to techniques well known.
The above, part specific embodiment only of the present invention, but scope of protection of the present invention is not limited thereto, appoints
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, should all cover by what those skilled in the art
Within protection scope of the present invention.
Claims (7)
1. a kind of method that the brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot, it is characterised in that the following steps are included:
Step 1: titanium crystal obtained by fused-salt electrolytic refining is placed in the distillation earthenware in distillation-smelting furnace under inert gas protection
In crucible；
Step 2: being evacuated to 1-100Pa for distillery, and titanium crystal is then heated to 1000-1600 DEG C in distillation crucible
Vacuum distillation；
Step 3: it is atmospherically distilled to when folder salt removal rate reaches 99% or more and stops vacuum distillation, and steamed in furnace by rotation
Crucible is evaporated, distillation gained titanium crystal is poured into the indoor melting kettle of melting；
Step 4: being heated to 1650-2000 DEG C for the titanium crystal in melting kettle, is in molten condition；
Step 5: ingot mold will be injected in such a way that the titanium crystal of molten condition is by rotation melting kettle in melting kettle
In；
Step 6: taking out after titanium ingot in ingot mold is cooled to room temperature, then saves, obtains in argon gas protection or vacuum sealing
Ultra Low-oxygen, ultra-pure titanium ingot.
2. the method that a kind of brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot, feature exist as described in claim 1
Inert gas is argon gas or helium in the step 1；Distillation-smelting furnace is integrated, distillery be placed in working chamber just on
Side, furthermore the upper part setting condensation chamber of distillery presss from both sides salt for collecting condensation gained；Distillation crucible be high melting point metal molybdenum,
Tantalum, niobium, hafnium, zirconium are process.
3. the method that a kind of brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot, feature exist as described in claim 1
In the selection of the step 2 vacuum degree and temperature not make high purity titanium crystalline substance be evaporated to 1 boundary's point, when the folder salt in high-purity titanium crystal
Stop distillation when 99% or more rate removal；Selected heating method is electric heating or resistance heating or induction heating.
4. the method that a kind of brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot, feature exist as described in claim 1
The rotation that crucible is distilled in the step 3 is realized by the pulley and rotation mechanical structure of distillation crucible bottom；And it rotates
Process is realized under the protection of vacuum or inert gas argon gas.
5. the method that a kind of brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot, feature exist as described in claim 1
Melting kettle is copper crucible in the step 4, and the crucible has water-cooled protecting device, is melted to prevent crucible；It is high-purity
The heating method of titanium crystalline substance are as follows: the mode of electron beam heating, electric arc heated or induction heating；It selects to need when electron beam heating true
Reciprocal of duty cycle is heated in the case where being less than 50Pa, and electric arc or induction heating then heat under protection of argon gas.
6. the method that a kind of brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot, feature exist as described in claim 1
The rotation of melting kettle is realized by the pulley and rotation mechanical structure of crucible bottom in the step 5；And rotation process
It is realized under the protection of vacuum or inert gas argon gas.
7. the method that a kind of brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot, feature exist as described in claim 1
Ingot mold is copper in the step 6, and has water cooling plant, for protecting mold, and is quickly cooled down titanium ingot；Institute
Ultra Low-oxygen, ultra-pure titanium ingot are obtained using plastics or metal vacuum packaging or argon gas protective packaging, to avoid titanium ingot and air
Contact.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910304141.5A CN110093515B (en) | 2019-04-16 | 2019-04-16 | Method for preparing low-oxygen high-purity titanium ingot by direct distillation-smelting of salt-sandwiched titanium crystal |
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| CN201910304141.5A CN110093515B (en) | 2019-04-16 | 2019-04-16 | Method for preparing low-oxygen high-purity titanium ingot by direct distillation-smelting of salt-sandwiched titanium crystal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112891973A (en) * | 2021-01-15 | 2021-06-04 | 中国科学院上海应用物理研究所 | Method for reducing oxygen content in halide molten salt |
| CN114853101A (en) * | 2022-05-18 | 2022-08-05 | 菏泽万清源环保科技有限公司 | Low-temperature evaporation treatment device and method for industrial waste liquid |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1571866A (en) * | 2001-10-17 | 2005-01-26 | 日本轻金属株式会社 | Method and apparatus for smelting titanium metal |
| CN102032783A (en) * | 2011-01-14 | 2011-04-27 | 李碚 | Cold crucible induction melting equipment for melting titanium or titanium alloy and melting and ingot pulling method |
| CN104195355A (en) * | 2014-08-13 | 2014-12-10 | 湖南稀土金属材料研究院 | Zirconium and method for preparing zirconium |
| CN106947874A (en) * | 2017-04-18 | 2017-07-14 | 北京科技大学 | A kind of method that two-step method prepares high purity titanium |
| CN107760877A (en) * | 2016-08-18 | 2018-03-06 | 宁波创润新材料有限公司 | The method of smelting of ingot casting |
| CN107805828A (en) * | 2017-10-23 | 2018-03-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Press from both sides the post-processing approach of salt titanium valve crude product |
| CN109266863A (en) * | 2018-11-27 | 2019-01-25 | 宝鸡市华烨钛镍金属有限公司 | A kind of high purity titanium ingot method of purification |
| CN109439902A (en) * | 2018-12-21 | 2019-03-08 | 有研工程技术研究院有限公司 | A kind of method that calcium original position distillation-deoxidation prepares high purity titanium |
-
2019
- 2019-04-16 CN CN201910304141.5A patent/CN110093515B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1571866A (en) * | 2001-10-17 | 2005-01-26 | 日本轻金属株式会社 | Method and apparatus for smelting titanium metal |
| CN102032783A (en) * | 2011-01-14 | 2011-04-27 | 李碚 | Cold crucible induction melting equipment for melting titanium or titanium alloy and melting and ingot pulling method |
| CN104195355A (en) * | 2014-08-13 | 2014-12-10 | 湖南稀土金属材料研究院 | Zirconium and method for preparing zirconium |
| CN107760877A (en) * | 2016-08-18 | 2018-03-06 | 宁波创润新材料有限公司 | The method of smelting of ingot casting |
| CN106947874A (en) * | 2017-04-18 | 2017-07-14 | 北京科技大学 | A kind of method that two-step method prepares high purity titanium |
| CN107805828A (en) * | 2017-10-23 | 2018-03-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Press from both sides the post-processing approach of salt titanium valve crude product |
| CN109266863A (en) * | 2018-11-27 | 2019-01-25 | 宝鸡市华烨钛镍金属有限公司 | A kind of high purity titanium ingot method of purification |
| CN109439902A (en) * | 2018-12-21 | 2019-03-08 | 有研工程技术研究院有限公司 | A kind of method that calcium original position distillation-deoxidation prepares high purity titanium |
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| CN112891973A (en) * | 2021-01-15 | 2021-06-04 | 中国科学院上海应用物理研究所 | Method for reducing oxygen content in halide molten salt |
| CN114853101A (en) * | 2022-05-18 | 2022-08-05 | 菏泽万清源环保科技有限公司 | Low-temperature evaporation treatment device and method for industrial waste liquid |
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