JPH03215634A - Method for lowering oxygen content of rare earth metal - Google Patents
Method for lowering oxygen content of rare earth metalInfo
- Publication number
- JPH03215634A JPH03215634A JP905590A JP905590A JPH03215634A JP H03215634 A JPH03215634 A JP H03215634A JP 905590 A JP905590 A JP 905590A JP 905590 A JP905590 A JP 905590A JP H03215634 A JPH03215634 A JP H03215634A
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- earth metal
- oxygen content
- melting
- oxygen
- 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
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 51
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 36
- 239000001301 oxygen Substances 0.000 title claims abstract description 36
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 35
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims description 8
- 238000002844 melting Methods 0.000 claims abstract description 17
- 230000008018 melting Effects 0.000 claims abstract description 17
- -1 rare earth metal fluoride Chemical class 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 abstract description 5
- 238000005266 casting Methods 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000000155 melt Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910004299 TbF3 Inorganic materials 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- LKNRQYTYDPPUOX-UHFFFAOYSA-K trifluoroterbium Chemical compound F[Tb](F)F LKNRQYTYDPPUOX-UHFFFAOYSA-K 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229940123973 Oxygen scavenger Drugs 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000001146 hypoxic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は希土類金属の精製技術に関し、特には希土類金
属中の酸素含有量を容易に、かつ経済的に低下せしめる
希土類金属の低酸素化方法に関する。[Detailed Description of the Invention] (Industrial Application Field) The present invention relates to rare earth metal refining technology, and in particular to a method for reducing the oxygen content of rare earth metals by easily and economically reducing the oxygen content in rare earth metals. Regarding.
（従来の技術と発明が解決しようとする課題）希土類金
属の用途は永久磁石、光磁気用素材等の新分野に拡大し
つつあるが、希土類金属は非常に活性が高く、空気中の
酸素によって容易に酸化される。希土類金属中の酸素は
各種用途における素材の物性を劣化させる原因となるの
で、この酸素含有量の減少が望まれていた。しかし、酸
素含有量を減少させるためには、原料の精製、取扱、保
管および製造工程において不活性ガス雰囲気中で処理す
るなど細心の注意を払う必要があり、通常の方法では酸
素含有量を１，ＯＯＯｐｐｍ以下に低下させることは困
難であった。酸素含有量をさらに低下させるためには、
例えば、高真空ゾーン精製設備のような高価な設備を必
要とし、経済性に問題が残されていた。(Problems to be solved by conventional technology and inventions) The use of rare earth metals is expanding into new fields such as permanent magnets and magneto-optical materials, but rare earth metals are extremely active and are Easily oxidized. Since oxygen in rare earth metals causes deterioration of the physical properties of materials used in various applications, it has been desired to reduce this oxygen content. However, in order to reduce the oxygen content, it is necessary to take great care such as processing the raw materials in an inert gas atmosphere during the refining, handling, storage, and manufacturing processes. , OOOppm or less was difficult to reduce. To further reduce the oxygen content,
For example, expensive equipment such as high-vacuum zone purification equipment is required, and economic efficiency remains unsolved.
本発明の目的は、希土類金属の酸素含有量を容易にかつ
経済的に低下せしめることができる希土類金属の低酸素
化方法を提供することにある。An object of the present invention is to provide a method for reducing the oxygen content of rare earth metals by easily and economically reducing the oxygen content of rare earth metals.
（課題を解決するための手段）
本発明者等は、かかる課題を解決するために、希土類金
属の低酸素化方法ついて種々検討を重ねてきたが、脱酸
素剤として該希土類金属の弗化物を見出し、その反応条
件を確立して、本発明に到達した。(Means for Solving the Problem) In order to solve the problem, the present inventors have repeatedly investigated various methods for reducing the oxygen content of rare earth metals. The present invention was achieved by discovering this and establishing the reaction conditions.
本発明の要旨は次の通りである。The gist of the invention is as follows.
希土類金属および該希土類金属弗化物からなる混合物を
不活性ガスまたは真空中で加熱溶融することを特徴とす
る希土類金属の低酸素化方法。A method for reducing the oxygen content of rare earth metals, which comprises heating and melting a mixture of a rare earth metal and the rare earth metal fluoride in an inert gas or vacuum.
以下、本発明を詳細に説明する。The present invention will be explained in detail below.
本発明が適用される希土類金属元素には、Ｙを含むＬａ
， Ｃｅ， Ｐｒ， Ｎｄ， Ｐｍ， Ｓｍ， Ｅｕ，
Ｇｄ， Ｔｂ， Ｄｙ， Ｈａ， Ｅｒ， Ｔｍ，Ｙ
ｂおよびＬｕＯ内１種もし《は２種以上の混合物が挙げ
られる。Rare earth metal elements to which the present invention is applied include La containing Y;
, Ce, Pr, Nd, Pm, Sm, Eu,
Gd, Tb, Dy, Ha, Er, Tm, Y
b and LuO may be one type, or << may be a mixture of two or more types.
脱酸素剤となる希土類金属弗化物としては、該希土類金
属の弗化物を使用するのが良く、不純物の混入を避ける
ことができる。例えば、Ｔｂ金属に対してはその弗化物
ＴｂＦ３を使用すれば良い。添加量は希土類金属１００
重量部に対して３０〜２００重量部、好ましくは５０〜
１００重量部の範囲が良い。３０重量部以下では脱酸素
の効果が少な《、２００重量部以上では希土類金属中の
弗素の混入量が増加する上に、１バッチ当たりの希土類
金属の処理量が減少するので経済性が悪くなる。希土類
金属から脱酸素される理由は希土類金属酸化物が弗化物
に溶解するためと考えられる。As the rare earth metal fluoride serving as the oxygen scavenger, it is preferable to use a fluoride of the rare earth metal, and contamination with impurities can be avoided. For example, for Tb metal, its fluoride TbF3 may be used. Addition amount is rare earth metal 100
30 to 200 parts by weight, preferably 50 to 200 parts by weight
A range of 100 parts by weight is preferable. If it is less than 30 parts by weight, the deoxidizing effect will be small. If it is more than 200 parts by weight, the amount of fluorine mixed in the rare earth metal will increase, and the amount of rare earth metal processed per batch will decrease, making it uneconomical. . The reason why rare earth metals are deoxidized is thought to be that rare earth metal oxides dissolve in fluorides.
反応条件としては、原料希土類金属および該希土類金属
弗化物をるつぼに仕込み、原料希土類金？および該希土
類金属弗化物の融点より高い温度一般的には１，０００
〜１，６００℃に加熱溶融する。As for the reaction conditions, the raw material rare earth metal and the rare earth metal fluoride are charged into a crucible, and the raw material rare earth metal fluoride is charged into a crucible. and a temperature higher than the melting point of the rare earth metal fluoride, generally 1,000
Heat and melt at ~1,600°C.
この加熱溶融雰囲気は不活性ガス中または真空中とする
必要があり、これにより希土類金属中の酸素が希土類金
属弗化物中に移行する。不活性ガスとしてはアルゴンが
好適であり、真空は０． ＩＴｏｒｒ以下が好ましい。This heating and melting atmosphere must be in an inert gas or vacuum, so that oxygen in the rare earth metal migrates into the rare earth metal fluoride. Argon is suitable as the inert gas, and the vacuum is 0. ITorr or less is preferable.
加熱溶融時間は希土類金属の融点、酸素含有量、処理量
などを考慮して適宜選択されるが、３〜２０分間で良い
。The heating melting time is appropriately selected in consideration of the melting point of the rare earth metal, oxygen content, processing amount, etc., and may be 3 to 20 minutes.
以上の処理後、溶融物は鋳型に傾注してから冷却するか
、またはそのまま冷却すれば良く、希土類金属と希土類
金属弗化物は溶融後比重差により二層分離しているので
低酸素化された希土類金属と０■を吸蔵した希土類金属
弗化物は容易に分離される。After the above treatment, the molten material can be poured into a mold and then cooled, or it can be cooled as it is, and since the rare earth metal and rare earth metal fluoride are separated into two layers due to the difference in specific gravity after melting, they are low in oxygen. The rare earth metal and the rare earth metal fluoride occluded with 0 are easily separated.
このようにして精製された希土類金属中の酸素含有量は
１ ， ０００ｐｐｍ以下と極めて少な＜．Ｃａ等のア
ルカリ土類金属も０． ０１％以下にまで減少しおり、
本発明が低酸素化精製方法として極めて優れていること
が判かる。The oxygen content in the rare earth metals purified in this way is extremely low, less than 1,000 ppm. Alkaline earth metals such as Ca are also 0. Bookmark decreased to less than 0.01%,
It can be seen that the present invention is extremely excellent as a low oxygen purification method.
また必要に応じて上記の処理を２回以上繰り返すことに
より、さらに酸素含有量を減少させることが出来る。こ
こで回収した弗化物は再弗化処理によって繰り返し使用
が可能であり、更に希土類金属の製造用原料としても使
用可能で経済的に有利である。Furthermore, the oxygen content can be further reduced by repeating the above treatment two or more times as necessary. The fluoride recovered here can be used repeatedly by refluorination treatment, and can also be used as a raw material for producing rare earth metals, which is economically advantageous.
以下、本発明の具体的実施態様を実施例と比較例を挙げ
て説明するが、本発明はこれらに限定されるものではな
い。例中％および部は特に断わらない限り重量に拠る。Hereinafter, specific embodiments of the present invention will be described with reference to Examples and Comparative Examples, but the present invention is not limited thereto. In the examples, percentages and parts are by weight unless otherwise specified.
（実施例１）
酸素含有量２， ０００ｐｐｍのＴｂ金属ＩＫｇに対し
、ＴｂＦ３を第１表に示される４水準の重量を混合し、
夫々タンタル製るつぼに仕込み、高周波誘導溶解炉によ
りＡｒ雰囲気下、１５００℃に加熱溶融し、溶融状態を
ＩＯ分間維持した後、Ｍｏ製鋳型に傾注し放冷した。冷
却後二ＭからなるＴｂ金属と弗化物は容易に分離でき、
各々の回収率は９９％および９８％であった。精製した
Ｔｂ金属中の酸素含有量を第１表に示した。ＴｂＦ．量
が多い程低酸素化効果が向上することが判かる。(Example 1) To Ikg of Tb metal with an oxygen content of 2,000 ppm, TbF3 was mixed at four levels of weight shown in Table 1,
Each was charged into a tantalum crucible, heated and melted at 1500° C. in an Ar atmosphere in a high frequency induction melting furnace, and after maintaining the molten state for 10 minutes, it was poured into a Mo mold and allowed to cool. After cooling, Tb metal consisting of 2M and fluoride can be easily separated,
The respective recoveries were 99% and 98%. Table 1 shows the oxygen content in the purified Tb metal. TbF. It can be seen that the larger the amount, the better the hypoxic effect.
（実施例２）
酸素含有量２， ＯＯＯｐｐｍのＴｂ金属１． ０Ｋｇ
とＴｂＦ３０．６Ｋｇとをタンタル製るつぼに仕込み、
Ａｒ雰囲気下１５００℃に加熱溶融し、この状態を４〜
１２分間維持した後、水冷銅製鋳型に傾注し、Ｔｂ金属
とＴｂＦｓの二層よりなるインゴットを得た。Ｔｂ金属
の酸素含有量は第２表に示した通りで、いずれの場合も
１ ， ０００ｐｐｍ以下に安定して低下しており、ま
た、溶融状態維持時間が長い程、低酸素下効果が大きい
ことが判かる。(Example 2) Oxygen content 2, OOOppm Tb metal 1. 0Kg
and TbF30.6Kg in a tantalum crucible,
Melt by heating at 1500°C in an Ar atmosphere, and maintain this state for 4 to 40 minutes.
After maintaining for 12 minutes, the mixture was poured into a water-cooled copper mold to obtain an ingot consisting of two layers of Tb metal and TbFs. The oxygen content of the Tb metal is shown in Table 2, and in all cases it has stably decreased to 1,000 ppm or less, and the longer the molten state is maintained, the greater the effect of low oxygen conditions. I understand.
（実施例３）
酸素含有量１， ６００ｐｐｍのＧｄ金属１． ０Ｋｇ
とＧｄＦ， ０．６Ｋｇとをモリブデン製るつぼに入れ
、これをＩＯ−３−ＪじＬＬ−
Ｔｏｒｒの真空中において黒鉛ヒーター抵抗溶解炉で１
，４００゜Ｃに加熱溶融し、この状態をｌＯ分間維持し
た後、このまま冷却した。Ｇｄ金属の酸素含有量は５３
０ｐｐｍであった。(Example 3) Gd metal with an oxygen content of 1,600 ppm 1. 0Kg
and GdF, 0.6 kg were placed in a molybdenum crucible and melted in a graphite heater resistance melting furnace in a vacuum of IO-3-JLL- Torr.
, 400°C, maintained this state for 10 minutes, and then cooled as it was. The oxygen content of Gd metal is 53
It was 0 ppm.
（実施例４） 酸素含有量２， ５００ｐｐｍのＤｙ金
属０．５ＫｇとＤｙＦｓ ０．４Ｋｇとをタンタル製ル
ツボに仕込み、高周波誘導溶解炉でアルゴン雰囲気中、
１，５８０℃に加熱溶解し、この状態をｌＯ分間維持し
た後、水冷銅製鋳型に傾注した。Ｄｙ金属中の酸素含有
量は７２０ｐｐｍに低下していた。(Example 4) 0.5 kg of Dy metal with an oxygen content of 2,500 ppm and 0.4 kg of DyFs were placed in a tantalum crucible, and heated in an argon atmosphere in a high frequency induction melting furnace.
After heating and melting at 1,580°C and maintaining this state for 10 minutes, the mixture was poured into a water-cooled copper mold. The oxygen content in the Dy metal had decreased to 720 ppm.
（比較例） 酸素含有量２， ０００ｐｐｍのＴｂ金属
１． ０ＫｇとＣａＦ２０、６Ｋｇとをタンタル製ルツ
ボに仕込み、高周波誘導溶解炉でアルゴン雰囲気中、１
，５００℃に加熱溶融し、この状態をｌＯ分間維持した
後、モリブデン製鋳型に傾注した。Ｔｂ金属中の酸素含
有量は１，５００ｐｐｍに低下しただけであり、Ｃａ金
属も１， ３００ｐｐｍ混入するという不利も生じた。(Comparative example) Tb metal with an oxygen content of 2,000 ppm 1. 0Kg and CaF20, 6Kg were placed in a tantalum crucible, and heated in a high frequency induction melting furnace in an argon atmosphere for 1 hour.
After heating and melting at 500° C. and maintaining this state for 10 minutes, the mixture was poured into a molybdenum mold. The oxygen content in the Tb metal was only reduced to 1,500 ppm, and 1,300 ppm of Ca metal was also mixed in, which was a disadvantage.
（発明の効果）
本発明によれば、希土類金属に該希土類金属弗化物を添
加混合し、加熱溶融するという非常に簡便な方法で希土
類金属中の酸素を効率的に低酸素化することが可能とな
り、酸素含有量１ ， ＯＯＯｐｐｍ以下の低酸素希土
類金属が安価に製造でき、産業上その利用価値は極めて
高い。(Effects of the Invention) According to the present invention, it is possible to efficiently reduce oxygen in rare earth metals by a very simple method of adding and mixing the rare earth metal fluoride to rare earth metals and heating and melting the mixture. Therefore, low-oxygen rare earth metals with an oxygen content of 1,000 ppm or less can be produced at low cost, and their utility value in industry is extremely high.
Claims (1)
不活性ガスまたは真空中で加熱溶融することを特徴とす
る希土類金属の低酸素化方法。A method for reducing the oxygen content of rare earth metals, which comprises heating and melting a mixture of a rare earth metal and the rare earth metal fluoride in an inert gas or vacuum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP905590A JPH03215634A (en) | 1990-01-18 | 1990-01-18 | Method for lowering oxygen content of rare earth metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP905590A JPH03215634A (en) | 1990-01-18 | 1990-01-18 | Method for lowering oxygen content of rare earth metal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03215634A true JPH03215634A (en) | 1991-09-20 |
| JPH0585627B2 JPH0585627B2 (en) | 1993-12-08 |
Family
ID=11709947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP905590A Granted JPH03215634A (en) | 1990-01-18 | 1990-01-18 | Method for lowering oxygen content of rare earth metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03215634A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06100957A (en) * | 1992-09-17 | 1994-04-12 | Shin Etsu Chem Co Ltd | Production of high-purity rare earth metal |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07227814A (en) * | 1994-02-22 | 1995-08-29 | Daiken Trade & Ind Co Ltd | Wooden fiber composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6311628A (en) * | 1986-06-30 | 1988-01-19 | Mitsubishi Chem Ind Ltd | Production of rare earth metal |
| JPS6424015A (en) * | 1987-07-17 | 1989-01-26 | Mitsubishi Chem Ind | Production of low-oxygen rare earth metal halide |
-
1990
- 1990-01-18 JP JP905590A patent/JPH03215634A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6311628A (en) * | 1986-06-30 | 1988-01-19 | Mitsubishi Chem Ind Ltd | Production of rare earth metal |
| JPS6424015A (en) * | 1987-07-17 | 1989-01-26 | Mitsubishi Chem Ind | Production of low-oxygen rare earth metal halide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06100957A (en) * | 1992-09-17 | 1994-04-12 | Shin Etsu Chem Co Ltd | Production of high-purity rare earth metal |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0585627B2 (en) | 1993-12-08 |
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