JPH06100957A - Production of high-purity rare earth metal - Google Patents
Production of high-purity rare earth metalInfo
- Publication number
- JPH06100957A JPH06100957A JP27377692A JP27377692A JPH06100957A JP H06100957 A JPH06100957 A JP H06100957A JP 27377692 A JP27377692 A JP 27377692A JP 27377692 A JP27377692 A JP 27377692A JP H06100957 A JPH06100957 A JP H06100957A
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- earth metal
- oxygen
- fluorine
- weight
- 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.)
- Granted
Links
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- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、電子材料、磁石材料等
として有用な高純度希土類金属の製造法に関するもので
ある。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a high-purity rare earth metal useful as an electronic material, a magnet material and the like.
【０００２】[0002]
【従来の技術】希土類金属は非常に活性の強い金属であ
り、酸素、フッ素、タンタル（るつぼ材質）等の不純物
の少ないものを製造するためには、原料の精製、製造工
程および取扱、保管時には細心の注意を払う必要があ
り、ゾーンメルト、固相電解、蒸留精製、昇華精製等の
方法があるが、何れもコストがかかり、また長時間を要
した。2. Description of the Related Art A rare earth metal is a metal having a very high activity, and in order to produce a substance with a small amount of impurities such as oxygen, fluorine, tantalum (crucible material), it is necessary to purify the raw material, process the production, handle and store it. Although it is necessary to pay close attention and there are methods such as zone melting, solid-phase electrolysis, distillation purification, and sublimation purification, all of them are costly and require a long time.
【０００３】[0003]
【発明が解決しようとする課題】本発明はかかる欠点を
解消した高純度希土類金属の製造法を提供しようとする
ものである。DISCLOSURE OF THE INVENTION The present invention is intended to provide a method for producing a high-purity rare earth metal which solves the above drawbacks.
【０００４】[0004]
【課題を解決するための手段】本発明者等は、上記課題
を解決するために脱酸素剤を種々検討した結果、希土類
弗化物の添加が極めて有効であることを見出し、本発明
を完成したもので、その要旨は、希土類金属と当該希土
類弗化物とを不活性ガスまたは眞空中で加熱溶解して酸
素を除去し、次いで、希土類金属を10-4Torr以上の高眞
空中で再溶解して脱フッ素することを特徴とする高純度
希土類金属の製造法にある。As a result of various investigations on the oxygen scavenger in order to solve the above problems, the present inventors have found that the addition of rare earth fluorides is extremely effective, and completed the present invention. The outline is that the rare earth metal and the rare earth fluoride are heated and dissolved in an inert gas or air to remove oxygen, and then the rare earth metal is redissolved in a high air temperature of 10 -4 Torr or more. It is a method for producing a high-purity rare earth metal, which is characterized by defluorinating by means of defluorination.
【０００５】以下、本発明を詳細に説明する。本発明は
希土類金属中の不純物レベルが10-1〜10-2重量％の市販
品を10-2〜10-3重量％まで約1/10に精製しようとするも
ので、希土類金属としてはＹを含む La,Ce,Pr,Nd,Pm,S
m,Eu,Gd,Tb,Dy,Ho,Er,Tm,YbおよびLuに適用することが
できる。原料となる市販希土類金属中の不純物として
は、酸素、フッ素、カルシウム等があるが、中でも酸
素、フッ素はレベルが高く、また市販品製造時に使用さ
れるるつぼ材質としてのタンタルは0.1 〜１重量％のレ
ベルで混入しているので用途によっては更に精製した高
純度品が要望されている。The present invention will be described in detail below. The present invention is intended to purify a commercial product having an impurity level of 10 -1 to 10 -2 wt% in a rare earth metal to about 10 -10 to 2 -10 -3 wt%. Including La, Ce, Pr, Nd, Pm, S
It can be applied to m, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu. Impurities in commercially available rare earth metals as raw materials include oxygen, fluorine, calcium, etc. Among them, oxygen and fluorine have a high level, and tantalum as a crucible material used in the production of commercial products is 0.1 to 1% by weight. Since it is mixed in at the level of, the highly purified product is required depending on the application.
【０００６】本発明は、希土類金属中の酸素を低減する
ため、当該希土類弗化物を添加して共融する方法であ
り、酸素の減少は希土類酸化物が希土類弗化物中に溶解
するためと推測される。また、Caの減少はCaと添加した
弗化物とが次式のように反応して弗化Caになるためと考
えられる。 Ca ＋ ＲＦ2 ─→ CaＦ2 ＋ Ｒ （Ｒは希土類元素） 添加する希土類弗化物の量は当該希土類金属に対して重
量％で10％以上、好ましくは30％以上である。10％未満
では脱酸素効果が少ない。溶解はアルゴン等の不活性ガ
ス雰囲気下または10-2Torr程度の眞空下に行ない、溶解
時間は数分〜30分が良い。次いで冷却すれば、弗化物は
金属との比重差でるつぼ上層で固化しているので容易に
分離できる。The present invention is a method of eutecticizing by adding the rare earth fluoride in order to reduce oxygen in the rare earth metal, and it is speculated that the decrease in oxygen is due to dissolution of the rare earth oxide in the rare earth fluoride. To be done. It is considered that the decrease in Ca is due to the reaction of Ca with the added fluoride as shown in the following formula to form Ca fluoride. Ca + RF 2- > CaF 2 + R (R is a rare earth element) The amount of the rare earth fluoride added is 10% or more, preferably 30% or more by weight% with respect to the rare earth metal. If it is less than 10%, the deoxidizing effect is small. Dissolution is carried out under an atmosphere of an inert gas such as argon or under a vacuum of about 10 -2 Torr, and the dissolution time is preferably several minutes to 30 minutes. Then, if cooled, the fluoride is solidified in the upper layer of the crucible due to the difference in specific gravity from the metal, so that the fluoride can be easily separated.
【０００７】次いで脱酸素した希土類金属を10-4Torr以
上の高眞空下に再溶解し、10分〜60分かけて脱フッ素す
る。フッ素の減少は希土類金属中の弗化物の蒸気圧が希
土類金属よりも若干高いことによるものと推定される。Then, the deoxygenated rare earth metal is redissolved in a high atmosphere of 10 -4 Torr or more and defluorinated for 10 to 60 minutes. It is presumed that the decrease of fluorine is due to the vapor pressure of fluoride in the rare earth metal being slightly higher than that of the rare earth metal.
【０００８】[0008]
【実施例】以下、本発明の実施態様を実施例を挙げて具
体的に説明するが、本発明はこれらに限定されるもので
はない。 （実施例１）酸素0.20重量％、フッ素0.10重量％、Ta
（タンタル）0.01重量％含有Tb（テルビウム）メタル１
KgにTbＦ3 0.6Kg を添加し、Taるつぼ中アルゴンガス雰
囲気下、高周波溶解炉で 1,500℃に加熱溶解した後、水
冷Cu鋳型に傾注し、Tbメタルを得た。次いでTbメタルを
水冷Cuハース中10-5の眞空下に電子ビーム溶解炉で再溶
解して脱フッ素した。Tbメタル中の酸素は0.03重量％、
フッ素は0.02重量％まで低下し、、タンタルは0.05重量
％であった。EXAMPLES The embodiments of the present invention will be specifically described below with reference to examples, but the present invention is not limited thereto. (Example 1) 0.20 wt% oxygen, 0.10 wt% fluorine, Ta
(Tantalum) 0.01 wt% Tb (terbium) metal 1
0.6 kg of TbF 3 was added to Kg, and the mixture was heated and melted at 1,500 ° C. in a high frequency melting furnace in a Ta crucible in an argon gas atmosphere, and then poured into a water-cooled Cu mold to obtain a Tb metal. Then, the Tb metal was remelted in a water-cooled Cu hearth under a vacuum of 10 −5 in an electron beam melting furnace for defluorination. Oxygen in Tb metal is 0.03% by weight,
Fluorine was reduced to 0.02% by weight and tantalum was 0.05% by weight.
【０００９】（実施例２）酸素0.16重量％、フッ素0.08
重量％、Ta 0.01 重量％含有Gd（ガドリニウム）メタル
１Kgを使用した以外は実施例１と同様に処理した結果、
Gdメタル中の酸素は0.03重量％、フッ素は0.01重量％ま
で低下し、タンタルは0.03重量％であった。(Example 2) Oxygen 0.16% by weight, fluorine 0.08
As a result of the same treatment as in Example 1 except that 1 kg of Gd (gadolinium) metal containing 1% by weight of Ta and 0.01% by weight of Ta was used,
Oxygen in the Gd metal was reduced to 0.03% by weight, fluorine was reduced to 0.01% by weight, and tantalum was 0.03% by weight.
【００１０】（実施例３）市販のTb、Gdメタルを実施例
１と同条件で処理した結果を表１に示す。Example 3 Table 1 shows the results obtained by treating commercially available Tb and Gd metals under the same conditions as in Example 1.
【表１】 酸 素 フッ素 タンタル（各重量％） Tb市販品 0.16 0.06 0.30 Tb処理品 0.03 0.02 0.05 Gd市販品 0.36 0.08 0.10 Gd処理品 0.03 0.01 0.03 [Table 1] Oxygen Fluorine Tantalum (each weight%) Tb commercial product 0.16 0.06 0.30 Tb treated product 0.03 0.02 0.05 Gd commercial product 0.36 0.08 0.10 Gd treated product 0.03 0.01 0.03
【００１１】（比較例）酸素0.15重量％、フッ素0.06重
量％、Ta 0.01 重量％含有Tbメタル１KgをTaるつぼ中で
Arガス雰囲気下に溶解し、Tbインゴットを得た。Tbメタ
ル中の酸素は0.16重量％、フッ素は0.06重量％、Taは0.
30重量％であった。(Comparative Example) 1 kg of Tb metal containing 0.15% by weight of oxygen, 0.06% by weight of fluorine and 0.01% by weight of Ta in a Ta crucible.
It was melted in an Ar gas atmosphere to obtain a Tb ingot. Oxygen in Tb metal is 0.16% by weight, fluorine is 0.06% by weight, Ta is 0.
It was 30% by weight.
【００１２】[0012]
【発明の効果】本発明によれば極めて簡単な操作で脱酸
素、脱フッ素が可能となり、高純度希土類金属が得ら
れ、産業上その利用価値は極めて高い。EFFECTS OF THE INVENTION According to the present invention, deoxygenation and defluorination can be performed by an extremely simple operation, a high-purity rare earth metal can be obtained, and its industrial utility value is extremely high.
Claims (1)
ガスまたは眞空中で加熱溶解して酸素を除去し、次い
で、希土類金属を10-4Torr以上の高眞空中で再溶解して
脱フッ素することを特徴とする高純度希土類金属の製造
法。1. A rare earth metal and the rare earth fluoride are heated and dissolved in an inert gas or a vacuum to remove oxygen, and then the rare earth metal is redissolved and removed in a high vacuum of 10 -4 Torr or more. A method for producing a high-purity rare earth metal, which is characterized by fluorine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4273776A JP2702649B2 (en) | 1992-09-17 | 1992-09-17 | Manufacturing method of high purity rare earth metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4273776A JP2702649B2 (en) | 1992-09-17 | 1992-09-17 | Manufacturing method of high purity rare earth metal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06100957A true JPH06100957A (en) | 1994-04-12 |
| JP2702649B2 JP2702649B2 (en) | 1998-01-21 |
Family
ID=17532419
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4273776A Expired - Fee Related JP2702649B2 (en) | 1992-09-17 | 1992-09-17 | Manufacturing method of high purity rare earth metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2702649B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7674427B2 (en) * | 2005-06-29 | 2010-03-09 | Shin-Etsu Chemical Co., Ltd. | Rare earth metal member and making method |
| JP2014105359A (en) * | 2012-11-28 | 2014-06-09 | Jx Nippon Mining & Metals Corp | Method for producing high purity neodymium, high purity neodymium, sputtering target produced by using high purity neodymium, permanent magnet including high purity neodymium as component |
| CN105331815A (en) * | 2015-10-15 | 2016-02-17 | 乐山盛和稀土股份有限公司 | Leaching technology of fluorine carbonate rare earth ore |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6424015A (en) * | 1987-07-17 | 1989-01-26 | Mitsubishi Chem Ind | Production of low-oxygen rare earth metal halide |
| JPH01116038A (en) * | 1987-10-30 | 1989-05-09 | Nippon Mining Co Ltd | Manufacture of high purity rare earth metal |
| JPH03170627A (en) * | 1989-11-28 | 1991-07-24 | Shin Etsu Chem Co Ltd | Method for deoxidizing from rare earth metal |
| JPH03215634A (en) * | 1990-01-18 | 1991-09-20 | Shin Etsu Chem Co Ltd | Method for lowering oxygen content of rare earth metal |
-
1992
- 1992-09-17 JP JP4273776A patent/JP2702649B2/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6424015A (en) * | 1987-07-17 | 1989-01-26 | Mitsubishi Chem Ind | Production of low-oxygen rare earth metal halide |
| JPH01116038A (en) * | 1987-10-30 | 1989-05-09 | Nippon Mining Co Ltd | Manufacture of high purity rare earth metal |
| JPH03170627A (en) * | 1989-11-28 | 1991-07-24 | Shin Etsu Chem Co Ltd | Method for deoxidizing from rare earth metal |
| JPH03215634A (en) * | 1990-01-18 | 1991-09-20 | Shin Etsu Chem Co Ltd | Method for lowering oxygen content of rare earth metal |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7674427B2 (en) * | 2005-06-29 | 2010-03-09 | Shin-Etsu Chemical Co., Ltd. | Rare earth metal member and making method |
| TWI408256B (en) * | 2005-06-29 | 2013-09-11 | Shinetsu Chemical Co | Rare earth metal member and manufacturing method thereof |
| JP2014105359A (en) * | 2012-11-28 | 2014-06-09 | Jx Nippon Mining & Metals Corp | Method for producing high purity neodymium, high purity neodymium, sputtering target produced by using high purity neodymium, permanent magnet including high purity neodymium as component |
| CN105331815A (en) * | 2015-10-15 | 2016-02-17 | 乐山盛和稀土股份有限公司 | Leaching technology of fluorine carbonate rare earth ore |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2702649B2 (en) | 1998-01-21 |
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