CN104894388A - Method for preparing vanadium target material through electron beam melting - Google Patents
Method for preparing vanadium target material through electron beam melting Download PDFInfo
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- CN104894388A CN104894388A CN201410081151.4A CN201410081151A CN104894388A CN 104894388 A CN104894388 A CN 104894388A CN 201410081151 A CN201410081151 A CN 201410081151A CN 104894388 A CN104894388 A CN 104894388A
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- vanadium
- electron beam
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- beam melting
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- 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
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Abstract
A method for preparing a vanadium target material through electron beam melting, and belongs to the technical filed of preparation of target materials. The method is characterized in that rod-shaped, strip-shaped or irregularly-shaped metal vanadium material scrap or vanadium-aluminum alloy with the vanadium content of 90% is adopted as a raw material and is molten in an magnetic focusing electron beam melting furnace, and undergoes pull-down ingot production under the pressure in the furnace of 1*10>-1>-1*10<-3>Pa, the voltage of an electron gun of 25-30kv and the current of the electron gun of 3-6A to produce a product with the diameter of 100-150mm and the ingot length of 500-1300nm. The purity of the product produced through the method can reach above 99.95%, and can completely meet demands of ion plating on target materials. The method allows vanadium target wastes to be recovered and re-molten, and has the characteristics of low cost, good purification effect and simple process.
Description
Technical field
The present invention relates to the technical field preparing high purity vanadium target by physical metallurgy technology, particularly a kind of electron beam melting technology is by the method for the Impurity removals such as the aluminium in vanadium, iron, belongs to the preparing technical field of target.
Background technology
Vanadium dioxide (VO
2) film is metallographic phase by semi-conductor phase in version transformation temperature is 68 DEG C, along with the transformation of phase, VO
2the electricity of film and the sudden change of optical property generation reversibility, make VO
2film becomes the ideal functionality material manufacturing electricity, optics.Such as can be made into micro-metering bolometer, storer, photoswitch etc.By film doping technology, transformation temperature can be reduced to room temperature, when temperature changes, the transmissivity producing phase transformation coating also changes thereupon, especially for making smart window, has very important meaning for save energy.
The main raw material(s) of this kind of masking technique is exactly vanadium target, and high purity vanadium target will have a wide range of applications.Made target many employings powder metallurgic method of refractory metal, for the method for the lower metal of fusing point also useful vacuum melting, but above technique is more complicated, and target purity is lower in the past.
Summary of the invention
The present invention, in view of the problem existing for prior art, is intended to openly a kind of electron beam melting and removes the method for impurity in vanadium, namely utilize electron beam melting technology, prepare highly purified target vanadium ingot.
Technical solution of the present invention is achieved in that
The method of vanadium target is prepared in electron beam melting, it is characterized in that, connects the irregular vanadium metal rim leftovers such as bar-shaped, strip with argon arc welding, or is placed in the feed bin of electromagnetic focusing electron beam melting furnace as melt electrode with the vananum containing vanadium 90%; By high-power electron beam, melt electrode bombarded, melt, melting, and obtain highly purified vanadium target through the mode of pervaporation under the condition always vacuumized.
In electromagnetic focusing electron beam melting furnace during melting, draw ingot under employing, the pressure in body of heater is 1x10
-1-1x10
-3pa, electron beam gun voltage 2.5-3 ten thousand volts, electric current 3-6 ampere, the vanadium target ingot product diameter made is 100-150mm, the long 500-1300mm of ingot.
Adopt and be interrupted charging, the mode ingot of lower traction continuously, being interrupted feed time is per minute 8-12mm, and lower pulling speed is 5-8mm.
Above-mentioned can adopt repeatedly bombard, melt, melting the mode of the evaporation always vacuumized circulate and repeatedly obtain purer vanadium target.
The product purity that this method is produced can reach more than 99.95%, can meet the demand of ion film plating to target completely.Can also remelting be reclaimed for discarded vanadium target, have that cost is low, refining effect good, the simple feature of technique.Under high vacuum atmosphere, remove the impurity such as aluminium, iron by electron beam melting mode; In high vacuum atmosphere, adopt and be interrupted charging, the mode ingot of lower traction continuously.
The described vanadium ingot aluminum content produced is not more than 0.004%, and it is more than 99.95% that iron-holder is not more than 0.0046%. purity.
Accompanying drawing explanation
The structural representation of Fig. 1 electron beam melting furnace;
1. tungstencathode; 2. negative electrode; 3. bunching electrode; 4. accelerating anode; 5. a magnetic focusing lens; 6. hurdle orifice plate; 7. two magnetic focusing lens; 8. hurdle orifice plate; 9. three magnetic focusing lens; 10. magnetic scanning lens; 11. bodies of heater; 12. electronic beam currents; 13. molten baths; 14. water jacketed copper crucibles (crystallizer); The 15. vanadium ingots solidified; 16. spindle supports; 17. drag spindle blade; 18. vanadium raw materials; 19. feed boxs; 20. feeding devices.
Embodiment
Be further described method of the present invention by embodiment below, will contribute to doing further to understand to the present invention and advantage thereof, protection scope of the present invention is not by the restriction of embodiment, and protection scope of the present invention is decided by claims.
Embodiment 1:
Connect bar-shaped, strip and other irregular vanadium metal rim leftovers with argon arc welding or be placed in feed bin as melt electrode with the vananum containing vanadium 90%; After installing, after being sealed the burner hearth of electromagnetic focusing electronics smelting furnace, startup oil-sealed rotary pump is exhausted and vacuumizes, and then startup lobe pump and diffusion pump are exhausted and vacuumize, and open the molecular pump of gun chamber, and vacuum tightness is at 3x10
-2-1x10
-3pa.
1) close main high pressure, secondary high pressure and filament voltage sky is opened, and presses main high pressure, secondary high pressure and filament control loop, opens the focusing of corresponding rifle, deflection and scanning power supply simultaneously;
2) blower fan of electron beam gun is driven;
3) to filament electrified regulation, electric current is made to be transferred to 30 ~ 40A
4) secondary high pressure is added to 1500V
5) viewing window is opened;
6) start to draw bundle.First fall secondary high pressure, make bombarding current remain on about 0.4A, make main high pressure as much as possible the full file location of first grade, close main high pressure simultaneously, first adjusts the power of electron beam gun to 3kw,
7) electron beam gun power is strengthened.Electron beam gun voltage 2.5-3 ten thousand volts, electric current 3-6 ampere,
8) electron beam gun bombards melt electrode, one end of fusing, temperature is 2500-3000 DEG C, the bottomless water jacketed copper crucible that the liquid raw material of melting drips to diameter 150mm obtains melting, drag spindle blade dragging to draw the vanadium ingot that it solidifies to move down, lower pulling speed is per minute 5-8mm, period feed time be per minute 8-12mm.
The vanadium ingot density made by the method for the present embodiment is 6.11 gram per centimeters, reaches theoretical density.Purity is high, and gaseous impurities is few, matrix crystallization, densification.
Embodiment 2.
For improving purity further, carry out secondary purification to the vanadium ingot through melting once, be about except per minute 5-8mm except input speed reduces, all the other change as following table by the foreign matter content of aluminium and iron after the melting of above-described embodiment 1 processing method: (other impurity is trace)
| After melting once (embodiment 1) | After secondary purification (embodiment 2) | |
| Fe（%） | 0.03 | 0.004 |
| Al（%） | 0.0073 | 0.0042 |
Obtain significantly improve further as shown visible purity.
Claims (4)
1. the method for vanadium target is prepared in electron beam melting, it is characterized in that, connects irregular vanadium metal rim leftover with argon arc welding, or is placed in the feed bin of electromagnetic focusing electron beam melting furnace as melt electrode with the vananum containing vanadium 90%; By high-power electron beam, melt electrode bombarded, melt, melting, and obtain highly purified vanadium target through the mode of pervaporation under the condition always vacuumized.
2. according to the method for claim 1, it is characterized in that, in electromagnetic focusing electron beam melting furnace during melting, draw ingot under employing, the pressure in body of heater is 1x10
-1-1x10
-3pa, electron beam gun voltage 2.5-3 ten thousand volts, electric current 3-6 ampere.
3. according to the method for claim 2, it is characterized in that, adopt and be interrupted charging, the mode ingot of lower traction continuously, being interrupted feed time is per minute 8-12mm, and lower pulling speed is 5-8mm.
4., according to the method for claim 1, it is characterized in that, adopt repeatedly bombard, melt, the mode of evaporation that melting also vacuumizes always circulates and repeatedly obtains purer vanadium target.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410081151.4A CN104894388A (en) | 2014-03-06 | 2014-03-06 | Method for preparing vanadium target material through electron beam melting |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410081151.4A CN104894388A (en) | 2014-03-06 | 2014-03-06 | Method for preparing vanadium target material through electron beam melting |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104894388A true CN104894388A (en) | 2015-09-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410081151.4A Pending CN104894388A (en) | 2014-03-06 | 2014-03-06 | Method for preparing vanadium target material through electron beam melting |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1253865A (en) * | 1998-11-12 | 2000-05-24 | 北京有色金属研究总院 | Method for making molybdenum electrode blank and molybdenum head piece blank by using electron-beam smelting method |
| JP2010156049A (en) * | 2009-12-25 | 2010-07-15 | Nippon Mining & Metals Co Ltd | High purity vanadium, target composed of the same vanadium, the same vanadium thin film, method of producing the same vanadium and method of producing the same vanadium spattering target |
| CN102899510A (en) * | 2012-10-31 | 2013-01-30 | 石政君 | Production method of high-purity metal vanadium |
-
2014
- 2014-03-06 CN CN201410081151.4A patent/CN104894388A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1253865A (en) * | 1998-11-12 | 2000-05-24 | 北京有色金属研究总院 | Method for making molybdenum electrode blank and molybdenum head piece blank by using electron-beam smelting method |
| JP2010156049A (en) * | 2009-12-25 | 2010-07-15 | Nippon Mining & Metals Co Ltd | High purity vanadium, target composed of the same vanadium, the same vanadium thin film, method of producing the same vanadium and method of producing the same vanadium spattering target |
| CN102899510A (en) * | 2012-10-31 | 2013-01-30 | 石政君 | Production method of high-purity metal vanadium |
Non-Patent Citations (5)
| Title |
|---|
| 《化工百科全书》编辑委员会: "《冶金和金属材料《化工百科全书》专业卷》", 31 January 2001, 化学工业出版社 * |
| 彭予民 等: "电子束冷床炉熔炼制备高纯金属钒铸锭", 《宝钢技术》 * |
| 曹凤国等: "《特种加工手册》", 30 November 2010, 北京：机械工业出版社 * |
| 李洪桂: "《稀有金属冶金原理及工艺》", 31 January 1981, 冶金工业出版社 * |
| 马宏声: "《钛及难熔金属真空熔炼》", 31 December 2010, 长沙：中南大学出版社 * |
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Application publication date: 20150909 |