JPH02263904A - Manufacture of rare earth metal powder - Google Patents
Manufacture of rare earth metal powderInfo
- Publication number
- JPH02263904A JPH02263904A JP8560589A JP8560589A JPH02263904A JP H02263904 A JPH02263904 A JP H02263904A JP 8560589 A JP8560589 A JP 8560589A JP 8560589 A JP8560589 A JP 8560589A JP H02263904 A JPH02263904 A JP H02263904A
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- metal
- earth metal
- alloy
- powder
- 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.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 21
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 21
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 19
- 239000000956 alloy Substances 0.000 claims abstract description 19
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 3
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 239000011261 inert gas Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract description 2
- 230000008016 vaporization Effects 0.000 abstract 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 238000000227 grinding Methods 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical group [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003579 shift reagent Substances 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical group [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 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粉末の製造方法に関する。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for producing rare earth metal powder.
セリウム族、イツトリウム族などの希土類金属は磁性材
料、超電導材料、ＮＭＲシフト試薬などに有用であり、
各方面から注目され需要が急増しているが、酸化され易
く延性があるため、ボールミル等の機械的粉砕によって
は容易に粉末にできないという問題がある。Rare earth metals such as cerium group and yttrium group are useful for magnetic materials, superconducting materials, NMR shift reagents, etc.
Although it is attracting attention from various quarters and its demand is rapidly increasing, it has the problem that it cannot be easily turned into powder by mechanical grinding such as a ball mill because it is easily oxidized and has ductility.
従来行われた方法には、アトマイズ法があるが、これは
高価な装置を必要とするため、コスト高となるので一般
的ではない。Conventional methods include the atomization method, but this is not common because it requires expensive equipment, resulting in high costs.
（課題を解決するための手段］
本発明者らはこの点にかんがみ、低コストで粉末化でき
る方法を課題として鋭意検討を重ねた結果、希土類金属
が比較的他の金属と合金化し易く、この合金は粉砕が容
易であることに着目し、さらに合金組成金属の蒸気圧の
差を利用することによって、課題が解決できることを見
出し、本発明に至ったのである。(Means for Solving the Problems) In view of this, the inventors of the present invention have conducted intensive studies on methods of powdering at low cost, and have found that rare earth metals are relatively easy to alloy with other metals. They focused on the fact that alloys are easy to crush, and discovered that the problem could be solved by utilizing the difference in vapor pressure between alloy composition metals, leading to the present invention.
本発明は、希土類金属Ｒとこれより蒸気圧の高い金属Ｍ
との合金ＲＭを粉砕し、これを真空中で加熱して金ＪＩ
Ｍを蒸発除去することを特徴とする希土類金属粉末の製
造方法を要旨とする。The present invention consists of a rare earth metal R and a metal M having a higher vapor pressure than the rare earth metal R.
The alloy RM is crushed and heated in vacuum to produce gold JI.
The gist of this invention is a method for producing rare earth metal powder, which is characterized by removing M by evaporation.
以下本発明の詳細な説明する。The present invention will be explained in detail below.
本発明では金属Ｍとして少な（とも希土類金属よりも高
い蒸気圧をもつ金属のなかから、合金化できるものを選
定しなければならない。この場合希土類金属や雰囲気ガ
スの種類、真空度等を考慮しなければならないが、好適
な金属としてはＭｇ、ＺｎおよびＣｄがあげられる。し
かしこれらのみに限定されないことはもちろんである。In the present invention, a metal that can be alloyed must be selected as the metal M from a small number of metals (both of which have a vapor pressure higher than that of rare earth metals).In this case, the rare earth metal, the type of atmospheric gas, the degree of vacuum, etc. Suitable metals include Mg, Zn and Cd, but are of course not limited to these.
希土類金属の合金の粉砕は、通常の粉砕手段でもできる
が、酸化を少なくするために不活性雰囲気中で粉砕する
のが望ましい。ジェットミルなどの場合には窒素、アル
ゴンなどの不活性ガス雰囲気下で、ボールミルなどの場
合には、ヘキサンなどの有機溶剤中で粉砕するのがよい
。合金はＩＩＩＩｍ程度以下の粒径に粉砕され、適宜所
望の粒度に篩い分けされる０次に所望の粒度の合金粉末
を加熱炉中で１気圧〜１０”’ｍｍＨｇの真空または不
活性ガス雰囲気中で５００〜１２００℃の温度に加熱す
る。これによって金属Ｍが蒸発し、加熱炉中には高純度
の希土類金属粉末が得られる。この場合の加熱温度によ
っては、金属粉末が凝集することもあるが、再粉砕すれ
ば容易に微粉化される。金属Ｍの蒸発除去に要する時間
を短くするには、高温はど望ましいが、温度が高過ぎる
と、希土類金属粉末が融着し、再粉砕が困難になるので
、温度は、５００〜１２００℃が望ましい。また昇温速
度が速過ぎると金属Ｍを蒸発除去する前に合金粉末が溶
融したり、融着が生じるので適当な昇温速度を選定する
必要がある。これは合金の種類や量および加熱炉の大き
さで選定されるが、通常は６００℃／Ｈｒ以下が好まし
い。Although rare earth metal alloys can be pulverized by conventional pulverization means, it is preferable to pulverize them in an inert atmosphere to reduce oxidation. When using a jet mill, it is preferable to grind under an inert gas atmosphere such as nitrogen or argon, and when using a ball mill, it is preferable to grind in an organic solvent such as hexane. The alloy is pulverized to a particle size of about IIIm or less and sieved to a desired particle size.The alloy powder of the desired particle size is then heated in a heating furnace in a vacuum or inert gas atmosphere of 1 atm to 10'' mmHg. The metal M is heated to a temperature of 500 to 1200°C.This evaporates the metal M, and a highly pure rare earth metal powder is obtained in the heating furnace.Depending on the heating temperature in this case, the metal powder may aggregate. However, it is easily pulverized by re-grinding.A high temperature is preferable to shorten the time required for evaporation removal of metal M, but if the temperature is too high, the rare earth metal powder will fuse and re-grinding will be difficult. Therefore, the temperature is preferably 500 to 1200°C. Also, if the heating rate is too fast, the alloy powder will melt or fusion will occur before the metal M is evaporated and removed, so select an appropriate heating rate. This is selected depending on the type and amount of alloy and the size of the heating furnace, but it is usually preferably 600° C./Hr or less.
以下本発明の具体例を実施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。Specific examples of the present invention will be described below with reference to Examples, but the present invention is not limited thereto.
例中％は重量％を表わす。In the examples, % represents weight %.
実施例１
８０％Ｔｂ−２０％Ｍｇ合金をＡｒ雰囲気のジェットミ
ルで粉砕し、１００メツシユバスの合金粉末を得た。こ
れをＴａルツボに入れ、真空炉中で１．０（１０℃まで
加熱した。合金中のＭｇはルツボの上部に設けたコンデ
ンサ一部に蓄積し、ルツボ内にはＴｂメタル粉末が残っ
た。粉末は一部凝集したので、Ａｒ雰囲気中で粉砕し、
１００メツシユバスのＴｂメタル粉末を得た。Example 1 An 80% Tb-20% Mg alloy was pulverized with a jet mill in an Ar atmosphere to obtain 100 mesh baths of alloy powder. This was placed in a Ta crucible and heated to 1.0° C. (10° C.) in a vacuum furnace. Mg in the alloy was accumulated in a part of the capacitor provided at the top of the crucible, and Tb metal powder remained in the crucible. The powder was partially agglomerated, so it was crushed in an Ar atmosphere.
A 100 mesh bath of Tb metal powder was obtained.
実施例２
７０％Ｄｙ−３０％Ｚｎ合金を、ヘキサン中でボールミ
ルにより粉砕し、４２メツシユバスの合金粉末を得た。Example 2 A 70% Dy-30% Zn alloy was ground in hexane using a ball mill to obtain 42 mesh baths of alloy powder.
これをＭｏルツボに入れ、Ａｒ雰囲気中で８００℃に加
熱した。合金中のＺｎはルツボ上部に設けたコンデンサ
一部に蓄積し、ルツボ内にＤｙメタル粉末を得た。This was placed in a Mo crucible and heated to 800° C. in an Ar atmosphere. Zn in the alloy was accumulated in a part of the capacitor provided above the crucible, and Dy metal powder was obtained in the crucible.
［発明の効果］
本発明によれば希土類金属の粉末が、容易に低コストで
製造できる。[Effects of the Invention] According to the present invention, rare earth metal powder can be easily produced at low cost.
特許出願人 信越化学工業株式会；Patent applicant Shin-Etsu Chemical Co., Ltd.;
Claims (1)
金ＲＭを粉砕し、これを不活性雰囲気または真空中で加
熱して金属Ｍを蒸発除去することを特徴とする希土類金
属粉末の製造方法。 ２、前記金属ＭがＭｇ、ＺｎおよびＣｄから選ばれる請
求項１に記載の希土類金属粉末の製造方法。[Claims] 1. An alloy RM of a rare earth metal R and a metal M having a higher vapor pressure than the rare earth metal R is pulverized, and the alloy RM is heated in an inert atmosphere or vacuum to evaporate and remove the metal M. A method for producing rare earth metal powder. 2. The method for producing rare earth metal powder according to claim 1, wherein the metal M is selected from Mg, Zn, and Cd.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8560589A JPH02263904A (en) | 1989-04-04 | 1989-04-04 | Manufacture of rare earth metal powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8560589A JPH02263904A (en) | 1989-04-04 | 1989-04-04 | Manufacture of rare earth metal powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02263904A true JPH02263904A (en) | 1990-10-26 |
Family
ID=13863459
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8560589A Pending JPH02263904A (en) | 1989-04-04 | 1989-04-04 | Manufacture of rare earth metal powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02263904A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06184601A (en) * | 1992-04-28 | 1994-07-05 | Internatl Business Mach Corp <Ibm> | Method of producing metal powder having additive dispersed uniformly |
-
1989
- 1989-04-04 JP JP8560589A patent/JPH02263904A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06184601A (en) * | 1992-04-28 | 1994-07-05 | Internatl Business Mach Corp <Ibm> | Method of producing metal powder having additive dispersed uniformly |
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