CN103114213A - Method for preparing high-purity molybdenum for sapphire growth furnace - Google Patents
Method for preparing high-purity molybdenum for sapphire growth furnace Download PDFInfo
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- CN103114213A CN103114213A CN2012104427543A CN201210442754A CN103114213A CN 103114213 A CN103114213 A CN 103114213A CN 2012104427543 A CN2012104427543 A CN 2012104427543A CN 201210442754 A CN201210442754 A CN 201210442754A CN 103114213 A CN103114213 A CN 103114213A
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Abstract
The invention provides a method for preparing high-purity molybdenum for a sapphire growth furnace so as to meet manufacturing of sapphire production equipment. High-purity molybdenum is prepared by performing electron beam melting, zone melting purification and electromagnetic field purification on the preliminarily purified molybdenum powder, wherein the parameters in the steps are that (1) electron beam melting, namely performing vacuum melting by using electron beams at the temperature of 2600-3000 DEG C and the vacuum degree of 2.5-6mu Pa, and adding carbon for deoxidation; (2) zone melting purification, namely performing zone melting at the temperature of 2900-3100 DEG C by employing electron beam heating; and (3) electromagnetic field purification, namely performing deep purification under the action of the electromagnetic field intensity of 6800-10000A/m. According to pure molybdenum prepared by the process, the molybdenum materials for large high-end sapphire crystal production equipment can be produced, the size can reach 1000*3000mm, and the purity is not less than 99.99 percent; and the impurity comprises the following components in percentage (max.%) by mass: 0.001 percent of Al, 0.001 percent of Ni, 0.001 percent of Si, 0.004 percent of W, 0.001 percent of Ca, 0.001 percent of KA, 0.001 percent of Mg, 0.001 percent of Na and 0.003 percent of O.
Description
Technical field
The invention belongs to the Metal smelting technology, particularly the rare metal purifying technique.
Background technology
For high-end sapphire crystal, its purity requirement reaches 99.99%-99.999%, to improve transmittance.This just requires associated metal heating and vacuum system element, such as the foreign matter content of the materials such as crucible, thermoscreen, heating rod should be low as far as possible, to reduce in crystal growing process the pollution to crystal.The purity of present domestic molybdenum materials main product is 99.95%, can not satisfy high-end sapphire crystal production requirement.
Summary of the invention
The object of the invention is to provide a kind of sapphire growth furnace High-Purity Molybdenum preparation method, to satisfy the manufacturing of sapphire production unit.
Sapphire growth furnace High-Purity Molybdenum preparation method is characterized in that the molybdenum powder of preliminary purification is purified and made through electron beam melting, area smelting refinement, electromagnetic field successively.
And in above-mentioned steps, parameter is chosen as:
(1), electronic beam vacuum smelting: 2600-3000 ℃ of lower vacuum melting, vacuum tightness is 2.5 16 μ Pa with electron beam; And add the carbon deoxidation;
(2), area smelting refinement: the electron beam heating is carried out zone melting at 2900-3100 ℃;
(3), electromagnetic field is purified: the degree of depth is purified under electromagnetic intensity 6800-10000A/m effect.
By the pure molybdenum of technique preparation of the present invention, can produce and satisfy large-scale, high-end sapphire crystal production unit molybdenum plate, its size can reach: 1000 * 3000 millimeters, purity reaches 99.99%min.Foreign matter content is (max.%):
Al：0.001、 Ni：0.001、Si：0.001、W：0.004 、Ca：0.001、 K：0.001、Mg：0.001、Na：0.001、O：0.003。
Embodiment
To begin to prepare molybdenum plate as example from the raw material ammonium molybdate:
Ammonium molybdate → roasting (400-550 ℃) → high-purity hydrogen once reduce (500-700 ℃) → high-purity hydrogen secondary reduction (900-1000 ℃) → batch mixing → screening → isostatic pressing → electron beam melting (2600-3000 ℃, (1300-1450 ℃) → hot rolling (1300-1400 ℃) → thermal treatment (900-1000 ℃) → cold rolling → thermal treatment (800-950 ℃) → moulding → performance test and the check of purifying (6800-10000A/m) → forge of 600-1200KW) → area smelting refinement (2900-3100 ℃) → electromagnetic field.
The core process parameter is selected: 1, electron beam melting: (2600-3000 ℃) vacuum melting refers to remove the process of Gases In Metals impurity under vacuum condition.Be actually and reduce the solubleness of gaseous impurities in metal.According to the Xi Weici law, under constant temperature diatomic gas in metal solubleness and the square root of partial pressure be directly proportional.Therefore improve the vacuum tightness of system, just be equivalent to reduce the dividing potential drop of gas, also can reduce the solubleness of gas in metal, and just can overflow from metal and remove over the portion gas impurity of solubleness.Under high vacuum (2.5 16 μ Pa) condition, moisture is 100 1 200 ℃ of sharply volatilizations, 600-700 ℃ of hydride decompose overflows, basic metal and compound thereof volatilize at 1,100 one 1600 ℃ of temperature, most of iron, nickel, chromium etc. volatilize with the low melting point oxide form, in the time of 2300 ℃, nitrogen volatilization is overflowed, contrast hydrogen, the oxygen that nitrogen is large to the metal affinity, with add the carbon deoxidation (" C]+" O]=CO ↑) and above foreign metal suboxide MeO
NMode remove).2, area smelting refinement: 2900-3100 ℃ zone melting is a kind of method that degree of depth is purified metals, its essence is by the long and narrow material ingot shape of local heating and become a narrow melting zone, and mobile heating makes this narrow melting zone slowly move along the material ingot by certain orientation, utilize impurity in solid phase and liquid phase homostasis concentration difference, in the process that repeatedly melts and solidify, impurity just segregates in solid phase or liquid phase and is removed or redistribute; Resistive heating is generally adopted in the melting zone, induction heating or electron beam heating.3, electromagnetic field is purified: the technology of degree of depth purification refractory metal is used more and more under electromagnetic field (magneticstrength 6800-10000A/m) effect.Electromagnetic field is not limited to the stirring action to molten metal, and main is can make molten metal obtain the even distribution of textural defect and refined grain structure in crystallisation process under electromagnetic field.When the multiphase system crystallization, utilize electromagnetic field that the second-phase orientation is separated out, electromagnetic field plays energy supporting role and stirring action, utilizes the evaporation of impurity and floats second-phase (oxide compound, carbide etc.) and come purified metal.
Claims (3)
1. sapphire growth furnace High-Purity Molybdenum preparation method, is characterized in that the molybdenum powder of preliminary purification is purified and made through electron beam melting, area smelting refinement, electromagnetic field successively.
2. sapphire growth furnace according to claim 1 High-Purity Molybdenum preparation method is characterized in that:
(1), electronic beam vacuum smelting: 2600-3000 ℃ of lower vacuum melting, vacuum tightness is 2.5 16 μ Pa with electron beam; And add the carbon deoxidation;
(2), area smelting refinement: adopt the electron beam heating to carry out zone melting at 2900-3100 ℃;
(3), electromagnetic field is purified: the degree of depth is purified under electromagnetic intensity 6800-10000A/m effect.
3. sapphire growth furnace according to claim 1 and 2 High-Purity Molybdenum preparation method is characterized in that the technique for preparing molybdenum materials with ammonium molybdate is:
Ammonium molybdate → 400-550 ℃ of lower roasting → 500-700 ℃ of lower high-purity hydrogen once reduce → and 900-1000 ℃ lower high-purity hydrogen secondary reduction → batch mixing → screening → isostatic pressing → electron beam melting (2600-3000 ℃, 600-1200KW) → area smelting refinement (2900-3100 ℃) → electromagnetic field purify forging → 1300-1400 ℃ lower hot rolling → 900-1000 ℃ lower thermal treatment → cold rolling → 800-950 ℃ lower thermal treatment → moulding → performance test and check under (6800-10000A/m) → 1300-1450 ℃.
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| CN2012104427543A CN103114213A (en) | 2012-11-08 | 2012-11-08 | Method for preparing high-purity molybdenum for sapphire growth furnace |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441651A (en) * | 2018-03-30 | 2018-08-24 | 厦门虹鹭钨钼工业有限公司 | A kind of preparation method improving molybdenum purity and yield |
| CN109371255A (en) * | 2018-10-30 | 2019-02-22 | 金川集团股份有限公司 | A kind of 6N high-purity cobalt ingot casting method |
| CN112126985A (en) * | 2020-07-10 | 2020-12-25 | 新疆三锐佰德新材料有限公司 | Method and device for physically purifying high-purity aluminum oxide material for sapphire |
Citations (2)
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| CN101148702A (en) * | 2007-10-26 | 2008-03-26 | 上海大学 | Method for smelting and purifying metal in electro-magnetism composite field and device thereof |
| CN102127741A (en) * | 2011-02-11 | 2011-07-20 | 韩伟东 | Method for preparing high-purity molybdenum target for thin film solar cell |
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- 2012-11-08 CN CN2012104427543A patent/CN103114213A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148702A (en) * | 2007-10-26 | 2008-03-26 | 上海大学 | Method for smelting and purifying metal in electro-magnetism composite field and device thereof |
| CN102127741A (en) * | 2011-02-11 | 2011-07-20 | 韩伟东 | Method for preparing high-purity molybdenum target for thin film solar cell |
Non-Patent Citations (1)
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| 李哲等: "高纯钽丝制备工艺探讨", 《稀有金属材料与工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441651A (en) * | 2018-03-30 | 2018-08-24 | 厦门虹鹭钨钼工业有限公司 | A kind of preparation method improving molybdenum purity and yield |
| CN109371255A (en) * | 2018-10-30 | 2019-02-22 | 金川集团股份有限公司 | A kind of 6N high-purity cobalt ingot casting method |
| CN109371255B (en) * | 2018-10-30 | 2020-05-05 | 金川集团股份有限公司 | 6N high-purity cobalt ingot casting method |
| CN112126985A (en) * | 2020-07-10 | 2020-12-25 | 新疆三锐佰德新材料有限公司 | Method and device for physically purifying high-purity aluminum oxide material for sapphire |
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Application publication date: 20130522 |