JPH04102303A - Manufacture of rare earth magnet - Google Patents
Manufacture of rare earth magnetInfo
- Publication number
- JPH04102303A JPH04102303A JP2220500A JP22050090A JPH04102303A JP H04102303 A JPH04102303 A JP H04102303A JP 2220500 A JP2220500 A JP 2220500A JP 22050090 A JP22050090 A JP 22050090A JP H04102303 A JPH04102303 A JP H04102303A
- Authority
- JP
- Japan
- Prior art keywords
- tray
- rare earth
- film
- magnet
- furnace
- 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
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 23
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 238000000034 method Methods 0.000 claims abstract description 8
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 3
- 238000005245 sintering Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 7
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 239000012298 atmosphere Substances 0.000 abstract description 2
- 238000005530 etching Methods 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 239000003925 fat Substances 0.000 abstract 1
- 230000004927 fusion Effects 0.000 abstract 1
- 239000003921 oil Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000003466 welding Methods 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- QIVUCLWGARAQIO-OLIXTKCUSA-N (3s)-n-[(3s,5s,6r)-6-methyl-2-oxo-1-(2,2,2-trifluoroethyl)-5-(2,3,6-trifluorophenyl)piperidin-3-yl]-2-oxospiro[1h-pyrrolo[2,3-b]pyridine-3,6'-5,7-dihydrocyclopenta[b]pyridine]-3'-carboxamide Chemical compound C1([C@H]2[C@H](N(C(=O)[C@@H](NC(=O)C=3C=C4C[C@]5(CC4=NC=3)C3=CC=CN=C3NC5=O)C2)CC(F)(F)F)C)=C(F)C=CC(F)=C1F QIVUCLWGARAQIO-OLIXTKCUSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000001552 radio frequency sputter deposition Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、モータ、アクチュエータ、各種電子製品、
コンピュータ周辺機器分野で、幅広く実用に供されてい
る希土類磁石の製法に関するものである。[Detailed Description of the Invention] [Industrial Application Field] This invention is applicable to motors, actuators, various electronic products,
This article relates to a method for manufacturing rare earth magnets that are widely used in the field of computer peripherals.
焼結温度が高い希土類磁石を焼結する場合、従来は高融
点金属のＭｏ板を成形体の下に敷いてきたが（セッター
）、希土類磁石は反応性が高いので、それと溶着し、焼
結収縮の均等性を阻害し、歩留り低下、あるいは製品の
品質に影響していた。When sintering rare earth magnets, which have a high sintering temperature, conventionally a Mo plate of high melting point metal was placed under the compact (setter), but since rare earth magnets have high reactivity, it is welded to it and sintered. This hinders the uniformity of shrinkage, lowering yield and affecting product quality.
これまでセンターとして耐熱性の酸化物、窒化物等積々
の材質が検討されている０例えばセラミックス・アルミ
ナ（Ａ１． ｏｚ）はそれ単独では、高温で寸法、強度
の劣化のないものであるが、希土類は活性度が高く、ア
ルミナの酸素をも還元するため、トレーとして使用した
場合、溶着が発生してしまい使用に耐えない、又、上記
ＭＯ板セッターの場合もＭｏの結晶粒が成長し、素材が
劣化、曲がりや反りが出るという欠点があった。Until now, many materials such as heat-resistant oxides and nitrides have been studied as centers. For example, ceramic alumina (A1. oz) alone does not deteriorate in size or strength at high temperatures. Rare earths have high activity and also reduce oxygen in alumina, so if used as a tray, welding will occur and it will not be usable.Also, in the case of the MO plate setter mentioned above, Mo crystal grains will grow. However, there were drawbacks such as the material deteriorating, bending, and warping.
希土類焼結磁石はＳｍＣｏ系、ＮｄＦｅＢ系磁石ともに
、磁気特性を向上するため一般的に、化学量論的組成よ
りも希土類が多い組成が選択される、特に２〜１７系Ｓ
ｍＣｏ磁石の場合は、いわゆる液相焼結を施すのでトレ
ーとの溶着が生しやすい状態にある。又ＮｄＦｅＢ系リ
ング磁石の場合は、磁場配向方向に平行と直角方向とで
焼結収縮率が約１０％異なるので、その配向方向が径方
向の場合、リングに歪みが大きく生じ、楕円の円筒リン
グになる欠点がある。従って、本発明が解決しようとし
ている課題は、焼結体に直接接触するトレーや歪み規制
の中子が高温焼結時に焼結体と溶着することである。For rare earth sintered magnets, for both SmCo and NdFeB magnets, compositions containing more rare earths than the stoichiometric composition are generally selected to improve magnetic properties, especially 2-17 S.
In the case of mCo magnets, so-called liquid phase sintering is performed, so welding with the tray is likely to occur. In addition, in the case of NdFeB ring magnets, the sintering shrinkage rate differs by about 10% between parallel and perpendicular to the magnetic field orientation direction, so if the orientation direction is radial, the ring will be greatly distorted, resulting in an elliptical cylindrical ring. There are drawbacks to it. Therefore, the problem to be solved by the present invention is that the tray and strain control core, which are in direct contact with the sintered body, are welded to the sintered body during high-temperature sintering.
上記問題点を解決するために、トレーや中子を希土類磁
石原料の主成分と同じ希土類からなる希土類酸化物粉末
、あるいは膜で被覆することによって溶着を防止する手
段を採用した。In order to solve the above-mentioned problems, we adopted a means to prevent welding by coating the tray and core with a rare earth oxide powder or film made of the same rare earth as the main component of the rare earth magnet raw material.
一般的に高エネルギー積を有する希土類磁石の組成は、
化学量論的組成よりも希土類量が多く、そのため焼結、
容体化処理中に粒界に希土類リッチ相が析出する。希土
類リッチ相が磁石の表面に滲み出てきて、それがトレー
や歪み規謂の中子と接触したとき、希土類簡素は非常に
活性なので、他の元素、すなわちトレー元素と反応する
ために、溶着現象が生じる。希土類元素の活性度は高く
、それ単独では、およそ１８００℃の高温でも寸法変化
や、強度の劣化のない安定したアルミナ（Ａ１．０３）
に対しても、アルミナの酸素を還元し、それが原因で溶
着が発生してしまう。このような活性度の高い希土類に
対しては、全く同様の希土類の酸化物であれば、還元が
できず溶着も防止できる。Generally, the composition of rare earth magnets with high energy product is:
The amount of rare earths is higher than the stoichiometric composition, so sintering,
A rare earth rich phase precipitates at the grain boundaries during the compaction treatment. When the rare earth rich phase oozes out to the surface of the magnet and it comes into contact with the tray or the core of the strained specification, the rare earth rich phase is so active that it reacts with other elements, i.e. the tray elements, causing welding. A phenomenon occurs. The activity of rare earth elements is high, and by themselves, they can produce stable alumina (A1.03) without dimensional changes or strength deterioration even at high temperatures of approximately 1800°C.
Also, it reduces oxygen in alumina, which causes welding. For such a highly active rare earth, an oxide of exactly the same rare earth cannot be reduced and welding can be prevented.
（実施例〕
以下、本発明について、実施例に基づき詳細に説明する
。トレーや中子の材質早＜ １２００℃の高温で焼結処
理を行うために、ＭｏやＳＵＳを選ぶ。(Example) The present invention will be described in detail based on Examples below.The material of the tray and the core is selected from Mo and SUS in order to carry out the sintering process at a high temperature of <1200°C.
実施例−１
トレーの表面を希土類の酸化物で被覆する前に、まず、
それらの表面に油脂分を有ｆＲ，ｆＪ剤で洗浄し、流水
で溶剤を除去した０次に下地のトレーの表面にＳｍ膜が
強固に付着し被覆するために、５％希酸で洗い清浄表面
を出すと共に、エツチング効果で表面の微細な凹凸を作
った。これら前処理を施された、約３０ｍｘ３０ｍｍの
トレーを高周波真空溶解炉の坩堝の上部に設置し、坩堝
でＳｍ金属を熔解する。蒸発Ｓｍがトレーに付着するの
で、炉の外部よりトレーを移動させて、均一なＳｍｌｌ
１を形成させた。その後、大気中に取り出してＳｍ１ｌ
Ｊの表面を酸化させた。これを２−１７系のＳｍＣｏ磁
石の焼結トレーとして用いて、繰り返し実験を行った。Example-1 Before coating the surface of the tray with rare earth oxide, first,
The oil and fat content on those surfaces was washed with fR and fJ agents, and the solvent was removed with running water.Next, in order to firmly adhere and coat the Sm film on the surface of the underlying tray, it was washed with 5% dilute acid and cleaned. In addition to exposing the surface, the etching effect created minute irregularities on the surface. A tray of approximately 30 m x 30 mm that has been subjected to these pretreatments is placed above a crucible in a high frequency vacuum melting furnace, and Sm metal is melted in the crucible. Evaporated Sm adheres to the tray, so move the tray from outside the furnace to ensure uniform Smll.
1 was formed. After that, take it out into the atmosphere and
The surface of J was oxidized. Repeated experiments were conducted using this as a sintered tray for 2-17 series SmCo magnets.
２回までは防ぐことができたが３回目で溶着が生し膜が
剥がれる結果になった。Although it was possible to prevent the damage up to two times, the third time resulted in welding and the film peeling off.
実施例−２
実施例１と同様に、Ｓｍ膜を形成させた後、トレーを外
熱式真空加熱炉に入れ、Ｑ、 ｌ Ｌｏｒｒ程度の酸素
中で６００℃に加熱して、強固な酸化膜を形成した。こ
れを同様に２−１７系のＳｍｃｏｉｆｆ石の焼結トレー
として用いて、繰り返し実験を行った。Example 2 In the same manner as in Example 1, after forming the Sm film, the tray was placed in an external heating vacuum heating furnace and heated to 600°C in oxygen of about Q, l Lorr to form a strong oxide film. was formed. This was similarly used as a sintered tray for 2-17 series Smcoiff stone, and repeated experiments were conducted.
８回まで溶着を防ぐことができた。Welding could be prevented up to 8 times.
実施例−３
トレーの表面の油脂分を除去後、ＲＦスパッタ装買のサ
ブストレートにセツティングし、まずトレー表面を逆ス
パツタとして、面を清浄にしてからターゲットのＳｍを
スパッタした。トレー上に強固なＳｍ膜が形成され、そ
れを実施例２と同様にトレーを外熱式真空加熱炉に入れ
、０．１ ｔｏｒｒ程度の酸素中で６００℃に加熱して
強固な酸化膜を形成した。これを同様に２−１７系のＳ
ｍＣｏ磁石の焼結トレーとして用いて、繰り返し実験を
行った。Example 3 After removing oil and fat from the surface of the tray, it was set on a substrate for RF sputtering, and the surface of the tray was first subjected to reverse sputtering to clean the surface and then sputtered with Sm as a target. A strong Sm film was formed on the tray, and as in Example 2, the tray was placed in an external vacuum heating furnace and heated to 600°C in oxygen at about 0.1 torr to form a strong oxide film. Formed. Similarly, 2-17 series S
Repeated experiments were conducted using this as a sintered tray for mCo magnets.
２０回まで剥がれることなく溶着を防ぐことができた。Welding could be prevented without peeling up to 20 times.
実施例−４
１Ｑｗｍφｘｉ（１ｗｔＯ中子の表面を希土類の酸化膜
で被覆する前に、まず、それらの表面の油脂分を有機溶
剤で洗浄し流水で溶剤を除去した。ＲＦスパフタ装置の
サブストレートにセツティングし、まず中子表面を逆ス
パッターして、面を清浄にしてからターゲットのＮｄを
スパンターした。トレー上に強固なＮｄ膜が形成され、
それを実施例２と同様にトレーを外熱式真空加熱炉に入
れ、０．１ｔｏｒｒ程度の酸素中で６００℃に加熱して
、強固な酸化膜を形成した。これをＮｄ系の径方向に磁
場配向したリング磁石の焼結処理時の中子として、繰り
返し実験を行った。これも又２０回まで溶着することな
く、かつリングの歪みを防止することができた。Example-4 Before coating the surface of the 1Qwmφxi (1wtO core with a rare earth oxide film, the oil and fat on the surface was first washed with an organic solvent and the solvent was removed with running water. After setting, the core surface was first reverse sputtered to clean the surface, and then the Nd target was sputtered.A strong Nd film was formed on the tray.
The tray was placed in an external heating vacuum heating furnace in the same manner as in Example 2, and heated to 600° C. in oxygen at approximately 0.1 torr to form a strong oxide film. Repeated experiments were conducted using this as a core during the sintering process of a Nd-based ring magnet with magnetic field orientation in the radial direction. This also allowed us to avoid welding up to 20 times and prevent distortion of the ring.
以上述べたように、本発明の希土類磁石原料の主成分と
同じ希土類からなる希土類酸化物の膜でトレーやリング
磁石の中子を強固に被覆して用いると、従来被覆を施し
てない場合１００％発注していた溶着に対し、表１に示
したように、焼結処理時に磁石とトレーまたは中子との
間の溶着が防止できる効果がある。As mentioned above, when the core of a tray or ring magnet is strongly coated with a rare earth oxide film made of the same rare earth as the main component of the rare earth magnet raw material of the present invention, As shown in Table 1, this method has the effect of preventing welding between the magnet and the tray or core during the sintering process, compared to the welding that had been ordered.
表 １Table 1
Claims (2)
料の主成分と同じ希土類からなる希土類酸化物粉末、あ
るいは膜で被覆されたトレーを敷くことを特徴とする希
土類磁石の製造方法。(1) A method for producing a rare earth magnet, which comprises placing a tray coated with a rare earth oxide powder or film made of the same rare earth as the main component of the raw material under the powder compact in the magnet heat treatment process.
と同じ希土類からなる希土類酸化物の膜を被覆された円
柱または円筒等を、リングの中に入れて焼結体の変形規
制を行うことを特徴とする希土類磁石の製造方法。(2) In the heat treatment process of ring magnets, a cylinder or cylinder coated with a rare earth oxide film made of the same rare earth as the main component of the raw material is placed inside the ring to control the deformation of the sintered body. Features: A manufacturing method for rare earth magnets.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2220500A JPH04102303A (en) | 1990-08-22 | 1990-08-22 | Manufacture of rare earth magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2220500A JPH04102303A (en) | 1990-08-22 | 1990-08-22 | Manufacture of rare earth magnet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04102303A true JPH04102303A (en) | 1992-04-03 |
Family
ID=16752016
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2220500A Pending JPH04102303A (en) | 1990-08-22 | 1990-08-22 | Manufacture of rare earth magnet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04102303A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009130279A (en) * | 2007-11-27 | 2009-06-11 | Ulvac Japan Ltd | Method of manufacturing permanent magnet |
| CN111145973A (en) * | 2018-11-06 | 2020-05-12 | 中国科学院宁波材料技术与工程研究所 | Samarium-cobalt permanent magnet containing grain boundary phase and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6354703A (en) * | 1986-08-25 | 1988-03-09 | Daido Steel Co Ltd | Manufacture of rare earth magnet |
| JPS63118031A (en) * | 1986-11-05 | 1988-05-23 | Hitachi Metals Ltd | Manufacture of permanent magnet alloy |
-
1990
- 1990-08-22 JP JP2220500A patent/JPH04102303A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6354703A (en) * | 1986-08-25 | 1988-03-09 | Daido Steel Co Ltd | Manufacture of rare earth magnet |
| JPS63118031A (en) * | 1986-11-05 | 1988-05-23 | Hitachi Metals Ltd | Manufacture of permanent magnet alloy |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009130279A (en) * | 2007-11-27 | 2009-06-11 | Ulvac Japan Ltd | Method of manufacturing permanent magnet |
| CN111145973A (en) * | 2018-11-06 | 2020-05-12 | 中国科学院宁波材料技术与工程研究所 | Samarium-cobalt permanent magnet containing grain boundary phase and preparation method thereof |
| CN111145973B (en) * | 2018-11-06 | 2021-01-05 | 中国科学院宁波材料技术与工程研究所 | Samarium-cobalt permanent magnet containing grain boundary phase and preparation method thereof |
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