JP6491304B2 - 希土類金属溶製脱ガス方法 - Google Patents
希土類金属溶製脱ガス方法Info
- Publication number
- JP6491304B2 JP6491304B2 JP2017239364A JP2017239364A JP6491304B2 JP 6491304 B2 JP6491304 B2 JP 6491304B2 JP 2017239364 A JP2017239364 A JP 2017239364A JP 2017239364 A JP2017239364 A JP 2017239364A JP 6491304 B2 JP6491304 B2 JP 6491304B2
- Authority
- JP
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- Prior art keywords
- rare earth
- metal
- vacuum
- earth metal
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims description 158
- 150000002910 rare earth metals Chemical class 0.000 title claims description 115
- 238000007872 degassing Methods 0.000 title claims description 34
- 238000002844 melting Methods 0.000 title claims description 33
- 230000008018 melting Effects 0.000 title claims description 33
- 229910052751 metal Inorganic materials 0.000 claims description 152
- 239000002184 metal Substances 0.000 claims description 151
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 96
- 239000007789 gas Substances 0.000 claims description 61
- -1 rare earth hydride Chemical class 0.000 claims description 60
- 229910052786 argon Inorganic materials 0.000 claims description 48
- 230000006698 induction Effects 0.000 claims description 45
- 229910052746 lanthanum Inorganic materials 0.000 claims description 44
- 239000002245 particle Substances 0.000 claims description 42
- 239000007788 liquid Substances 0.000 claims description 39
- 239000011261 inert gas Substances 0.000 claims description 20
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 16
- 229910052721 tungsten Inorganic materials 0.000 claims description 16
- 239000010937 tungsten Substances 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 11
- 229910052689 Holmium Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 229910052727 yttrium Inorganic materials 0.000 claims description 7
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052765 Lutetium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 34
- 238000000034 method Methods 0.000 description 30
- 239000012535 impurity Substances 0.000 description 16
- 230000000694 effects Effects 0.000 description 15
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 13
- 238000009413 insulation Methods 0.000 description 12
- 238000000746 purification Methods 0.000 description 12
- 239000003039 volatile agent Substances 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000007670 refining Methods 0.000 description 7
- 238000011109 contamination Methods 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000007790 solid phase Substances 0.000 description 5
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- LCTWRNOEZKTLGG-UHFFFAOYSA-K holmium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Ho+3] LCTWRNOEZKTLGG-UHFFFAOYSA-K 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- DEXZEPDUSNRVTN-UHFFFAOYSA-K yttrium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Y+3] DEXZEPDUSNRVTN-UHFFFAOYSA-K 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002603 lanthanum Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 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
- C22B59/00—Obtaining rare earth metals
-
- 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
- C22B9/003—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals by induction
-
- 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
- C22B9/04—Refining by applying a vacuum
-
- 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
- C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
Description
Claims (10)
- 精製対象である希土類金属を真空環境下で溶融し、溶融金属液を形成するステップS1と、
0.01〜0.05MPaの真空度で、前記精製対象である希土類金属の重量に対して、0.5〜10%の重量で希土類水素化物を前記溶融金属液と混合し、5〜30min保温し、脱ガスされた溶融金属及びガス状物質を得るステップS2と、
前記ガス状物質と前記脱ガスされた溶融金属とを分離し、且つ前記脱ガスされた溶融金属を不活性ガス中で冷却し、脱ガス希土類金属を得るステップS3と、
を含むことを特徴とする希土類金属溶製脱ガス方法。 - 前記希土類金属は、La、Ce、Pr、Nd、Gd、Tb、Dy、Ho、Er、Lu、Y又はScであることを特徴とする請求項1に記載の脱ガス方法。
- 前記ステップS1は、
前記精製対象である希土類金属を中間周波数誘導炉のるつぼに入れ、且つ前記中間周波数誘導炉の炉内を真空引きし、真空チャンバを形成することと、
前記真空チャンバに前記不活性ガスを導入して前記真空チャンバを洗浄し、前記真空チャンバの真空度が10-2Pa未満になった時に、前記真空チャンバを前記精製対象である希土類金属の融点温度よりも50〜100℃高い温度までに昇温し、前記精製対象である希土類金属を溶融し、且つ5〜15min保温した後に、前記溶融金属液を得ることと、
を含むことを特徴とする請求項1に記載の脱ガス方法。 - 前記るつぼは、タングステン製るつぼであることを特徴とする請求項3に記載の脱ガス方法。
- 10〜30kWの電力で前記真空チャンバを昇温することを特徴とする請求項3に記載の脱ガス方法。
- 前記ステップS2は、
前記中間周波数誘導炉の真空システムの排気バルブを閉じて、且つ前記真空チャンバ内に前記不活性ガスを真空度が0.01〜0.05MPaとなるまでに充填することと、
希土類水素化物粒子を前記溶融金属液に添加し、且つ前記真空チャンバの温度を、溶融金属液の表面が凝固状態になった後に5〜30min保温し続け、脱ガスされた溶融金属及びガス状物質を得ることと、
を含むことを特徴とする請求項3に記載の脱ガス方法。 - 前記希土類水素化物粒子の粒子径は、0.1〜5mmであることを特徴とする請求項6に記載の脱ガス方法。
- 前記ステップS3は、
前記真空システムの排気バルブを開け、前記真空チャンバを真空引きすることと、
前記真空チャンバの真空度が10-2Pa以下に戻った後に、前記真空チャンバを前記精製対象である希土類金属の融点温度よりも50〜300℃高い温度までに昇温し、5〜20min保温することと、
保温終了後に、前記脱ガスされた溶融金属を鋳造し、次いで、前記不活性ガスを利用して保護し、且つ室温までに冷却し、前記脱ガスされた希土類金属を得ることと、
を含むことを特徴とする請求項6に記載の脱ガス方法。 - 前記不活性ガスは、アルゴンガスであることを特徴とする請求項1〜8のいずれか1項に記載の脱ガス方法。
- 前記希土類水素化物及び前記精製対象である希土類金属における希土類元素は同じであることを特徴とする請求項1〜8のいずれか1項に記載の脱ガス方法。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201611175185.5A CN108203766B (zh) | 2016-12-16 | 2016-12-16 | 稀土金属熔炼脱气方法 |
CN201611175185.5 | 2016-12-16 |
Publications (2)
Publication Number | Publication Date |
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JP2018095965A JP2018095965A (ja) | 2018-06-21 |
JP6491304B2 true JP6491304B2 (ja) | 2019-03-27 |
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JP2017239364A Active JP6491304B2 (ja) | 2016-12-16 | 2017-12-14 | 希土類金属溶製脱ガス方法 |
Country Status (3)
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JP (1) | JP6491304B2 (ja) |
CN (1) | CN108203766B (ja) |
MY (1) | MY186742A (ja) |
Families Citing this family (5)
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CN110983076B (zh) * | 2019-12-31 | 2022-02-18 | 包头市中鑫安泰磁业有限公司 | 一种高纯稀土的制备装置及制备方法 |
CN112962072B (zh) * | 2021-02-02 | 2023-07-07 | 长沙淮石新材料科技有限公司 | 一种低氧大尺寸含铝基金属间化合物的合金靶材及其制备方法 |
CN114657420B (zh) * | 2022-04-08 | 2023-10-20 | 包头稀土研究院 | 轻稀土-锌合金及其制备方法和用途及熔炼容器的用途 |
CN114752814B (zh) * | 2022-04-08 | 2023-10-20 | 包头稀土研究院 | 重稀土锌合金及其制造方法和用途以及含钨容器的用途 |
CN115821087B (zh) * | 2022-11-30 | 2024-06-04 | 上海大学 | 一种稀土金属等离子脱氧的方法和低含氧量稀土金属 |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
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JPS619533A (ja) * | 1984-06-22 | 1986-01-17 | Showa Denko Kk | 希土類金属の製造方法 |
RU2102513C1 (ru) * | 1993-03-22 | 1998-01-20 | Виталий Евгеньевич Дьяков | Способ получения металлического скандия |
CN101665909B (zh) * | 2009-10-23 | 2012-08-22 | 宁波江丰电子材料有限公司 | 靶材的制备方法 |
CN102465209B (zh) * | 2010-11-02 | 2014-08-27 | 有研稀土新材料股份有限公司 | 一种高纯金属钕的制备方法及其装置 |
CN102465210A (zh) * | 2010-11-02 | 2012-05-23 | 北京有色金属研究总院 | 一种高纯稀土金属的制备方法及其装置 |
JP6087117B2 (ja) * | 2012-11-28 | 2017-03-01 | Jx金属株式会社 | 高純度ネオジムの製造方法、高純度ネオジム、高純度ネオジムを用いて製造したスパッタリングターゲット、高純度ネオジムを成分とする永久磁石 |
DE102013211946A1 (de) * | 2013-06-24 | 2015-01-08 | Siemens Aktiengesellschaft | Verfahren zur Darstellung eines Seltenerdelementes durch eine Redoxreaktion |
CN103409650B (zh) * | 2013-07-25 | 2014-11-12 | 北京大学 | 氢等离子体电弧熔炼技术制备高纯稀土钆单质 |
CN103589874B (zh) * | 2013-09-27 | 2016-01-27 | 北京大学 | 一种在温差下提纯金属材料的方法 |
KR20150042018A (ko) * | 2013-10-10 | 2015-04-20 | 공주대학교 산학협력단 | 진공용해 프로세스에 의한 희토류금속의 정련방법 및 그 제조장치 |
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MY186742A (en) | 2021-08-16 |
JP2018095965A (ja) | 2018-06-21 |
CN108203766B (zh) | 2019-12-27 |
CN108203766A (zh) | 2018-06-26 |
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