JPH0611006B2 - Rare earth permanent magnet manufacturing method - Google Patents
Rare earth permanent magnet manufacturing methodInfo
- Publication number
- JPH0611006B2 JPH0611006B2 JP59073997A JP7399784A JPH0611006B2 JP H0611006 B2 JPH0611006 B2 JP H0611006B2 JP 59073997 A JP59073997 A JP 59073997A JP 7399784 A JP7399784 A JP 7399784A JP H0611006 B2 JPH0611006 B2 JP H0611006B2
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- permanent magnet
- earth permanent
- oxide film
- heat treatment
- 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.)
- Expired - Lifetime
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims description 17
- 150000002910 rare earth metals Chemical class 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title claims 4
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000000956 alloy Substances 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 description 10
- 238000001704 evaporation Methods 0.000 description 10
- 238000011282 treatment Methods 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 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
- H01F1/0551—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0552—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Powder Metallurgy (AREA)
- Hard Magnetic Materials (AREA)
Description
【発明の詳細な説明】 〔技術分野〕 本発明は、希土類永久磁石の熱処理において、あらかじ
め厚さ５００〜３０００Åの酸化膜を付与した後に処理
を行なうことにより、より高性能な永久磁石を得る製造
方法に係わる。Description: TECHNICAL FIELD The present invention relates to a heat treatment of a rare earth permanent magnet, which is produced by applying an oxide film having a thickness of 500 to 3000 Å in advance and then performing the treatment to obtain a higher performance permanent magnet. Involved in the method.
希土類永久磁石は、現在最も高いエネルギー積を有して
いることから、機器の小型化，省エネルギー化への貢献
度は極めて大きい。このため、各種機器への用途開発，
実用化研究は急速に高まり、その応用範囲は一気に拡大
してきた。本永久磁石は、通常、１２００〜３００℃程
度の溶体化処理，時効処理等の熱処理を必要とする。こ
れは、製造方法が、粉末焼結法あるいは樹脂ポンド法に
かかわらず必要な工程である。ところが一般に、希土類
金属は非常に蒸発しやすい。そのため高温での熱処理に
おいては、希土類金属の選択的な蒸発がはげしく、蒸発
による組成変動のため、高性能化を阻害する一因となっ
ていた。Since rare earth permanent magnets currently have the highest energy product, their contribution to miniaturization of equipment and energy saving is extremely large. Therefore, application development for various equipment,
Practical application research has grown rapidly, and its range of applications has expanded rapidly. This permanent magnet usually requires heat treatment such as solution treatment and aging treatment at about 1200 to 300 ° C. This is a necessary process regardless of the powder sintering method or the resin pond method. However, rare earth metals are generally very likely to evaporate. Therefore, in the heat treatment at a high temperature, selective evaporation of the rare earth metal is violent, and the composition variation due to evaporation is one of the factors that hinder the performance improvement.
本発明の目的は、前記した高温熱処理時の希土類金属の
蒸発の影響を緩和し、より高性能な永久磁石を得ること
にある。An object of the present invention is to alleviate the influence of evaporation of rare earth metal during the above-mentioned high temperature heat treatment and to obtain a permanent magnet with higher performance.
希土類磁石の蒸発過程は、以下のように説明できる。希
土類磁石を高温で熱処理すると、希土類元素（以下Ｒ元
素と称する。）はその蒸気圧が高いため、他の磁石成分
（遷移金属元素または、Ｓｉ，Ｂ，Ｃ等の非金属元素）
に比して、優先的に蒸発して行く。このとき、第１図
に示すようにまず表面部より、Ｒ元素の蒸発が生じ、そ
の部分はＲ元素がなくなるため、組成変動が生じること
となる。しかしさらに、Ｒ元素が蒸発するには、Ｒ元素
の存在しない部分（第１図の斜線部分）を通り抜ける
必要が生じる。この部分をＲ元素が通り抜けることは非
常に困難なため、Ｒ元素は第１図に示した粒界を通じ
て蒸発を起こすようになる。しかしこの現象も、拡散過
程であるため、表面部からの蒸発に比すれば、困難な過
程である。本発明は、こういった現象を利用して、熱処
理前に厚さ５００〜３０００Åの酸化膜を付与し、その
酸化膜により蒸発現象を妨げようとするものである。す
なわち、希土類磁石を高温熱処理する前に、予備処理と
して２００〜４００℃程度で１分〜１時間以内の処理を
行ない、厚さ５００〜３０００Å程度の酸化膜を付与す
る。酸化膜はこの程度の厚さでは、完全な希土類酸化物
色を示さず、緩衝色となり、磁気性能への影響も無視し
うる。この後、本来の熱処理工程へ移る。酸化膜付与に
より、Ｒ元素の蒸発は、酸化膜を介して起こらねばなら
ず、蒸発過程は著しく妨げられる。このため高性能化阻
害原因となっていた。Ｒ元素蒸発による組成変動が妨げ
られ、高性能磁石が得られるのである。The evaporation process of the rare earth magnet can be explained as follows. When the rare earth magnet is heat-treated at a high temperature, the rare earth element (hereinafter referred to as the R element) has a high vapor pressure, and therefore other magnet components (transition metal element or non-metal element such as Si, B, C).
Compared to, it preferentially evaporates. At this time, as shown in FIG. 1, first, the R element evaporates from the surface portion, and the R element disappears in that portion, so that the composition changes. However, further, in order for the R element to evaporate, it is necessary to pass through a portion where the R element does not exist (hatched portion in FIG. 1). Since it is very difficult for the R element to pass through this portion, the R element will be vaporized through the grain boundaries shown in FIG. However, since this phenomenon is also a diffusion process, it is a difficult process as compared with evaporation from the surface portion. The present invention utilizes such a phenomenon to provide an oxide film having a thickness of 500 to 3000 Å before the heat treatment, and the oxide film prevents the evaporation phenomenon. That is, before the high temperature heat treatment of the rare earth magnet, a pretreatment is performed at 200 to 400 ° C. for 1 minute to 1 hour to provide an oxide film having a thickness of 500 to 3000 Å. At such a thickness, the oxide film does not show a perfect rare earth oxide color and becomes a buffer color, and its influence on the magnetic performance can be neglected. After this, the process goes to the original heat treatment step. By applying the oxide film, the evaporation of the R element must occur through the oxide film, and the evaporation process is significantly hindered. For this reason, it has been a cause of impeding performance. The composition variation due to the evaporation of the R element is prevented, and a high-performance magnet is obtained.
以下、本発明について実施例に基づき詳細に説明する。 Hereinafter, the present invention will be described in detail based on examples.
参考例 一般式で、Sm(Co0.741Cu0.065Fe0.18Ni0.014)7.3なる合
金を低周波溶解炉で、溶解し合金インゴットを作成し
た。このインゴットを粉砕し、1160℃×１時間の焼結を
行った。ここで、本発明により種々の厚さの酸化膜を付
与したものと、比較例として酸化膜を付与しない通常品
に分け、以下の熱処理を行ない、磁気特性の評価を行っ
た。Reference Example In the general formula, an alloy of Sm (Co 0.741 Cu 0.065 Fe 0.18 Ni 0.014 ) 7.3 was melted in a low frequency melting furnace to prepare an alloy ingot. This ingot was crushed and sintered at 1160 ° C for 1 hour. Here, an oxide film having various thicknesses according to the present invention and a normal product having no oxide film as a comparative example were divided into the following heat treatments to evaluate the magnetic properties.
熱処理方法−溶体化処理：1140℃×2.5時間 時効処理 ：800℃×２時間＋ 400℃×６時間 結果を第１表に示す。Heat treatment method-solution treatment: 1140 ° C x 2.5 hours Aging treatment: 800 ° C x 2 hours + 400 ° C x 6 hours The results are shown in Table 1.
第１表からわかるように、本発明によりエネルギー積，
保磁力が大きく増加していることがわかる。また酸化膜
厚さは５００〜３０００Å程度が適当であり、これより
厚くなると、Ｒ元素の蒸発防止効果よりも酸化膜自体に
よる性能劣化の効果が大きくなってしまう。 As can be seen from Table 1, the energy product according to the present invention,
It can be seen that the coercive force is greatly increased. Further, it is suitable that the oxide film thickness is about 500 to 3000 Å, and if it is thicker than this, the effect of performance deterioration due to the oxide film itself becomes larger than the effect of preventing evaporation of the R element.
実施例 一般式で、Sm(Co0.569Cu0.075Fe0.34Zr0.016)7.8なる合
金を低周波溶解炉で溶解し、合金インゴットを作成し
た。このインゴットを、本発明による約２０００Åの酸
化膜を付与したものと、比較例として通常の酸化膜を付
与しないものに分け、以下の熱処理方法で樹脂ポンド法
により、異方性磁石を作成し特性評価を行ない、次に１
００℃における温度特性試験を行った。Example In the general formula, an alloy of Sm (Co 0.569 Cu 0.075 Fe 0.34 Zr 0.016 ) 7.8 was melted in a low frequency melting furnace to prepare an alloy ingot. This ingot is divided into one with an oxide film of about 2000Å according to the present invention and one without a normal oxide film as a comparative example. Anisotropic magnets are prepared by the resin pond method by the following heat treatment method, Evaluate, then 1
A temperature characteristic test at 00 ° C. was performed.
熱処理方法−溶体化処理：1135℃×２４時間 時効処理 ：820℃×２４時間 まず、特性評価結果を示す。Heat treatment method-solution treatment: 1135 ° C x 24 hours Aging treatment: 820 ° C x 24 hours First, the results of characteristic evaluation are shown.
本発明法−Ｂｒ ：９３５０Ｇ ｂＨｃ ：７２００Ｇ (BH)max：19.5ＭＧＯｅ 比較例 −Ｂｒ ：９２９０Ｇ ｂＨｃ ：６９７０Ｇ (BH)max：18.3ＭＧＯｅ 続いて、第２図に温度特性試験の結果を示す。第２図
は本発明品の結果であり、第２図は比較例である従来
品の結果である。一般に樹脂ボンド磁石は、耐熱性が悪
いと考えられるが、本発明によれば、磁気特性だけでな
く、耐熱性の改良も可能である。Inventive Method-Br: 9350G bHc: 7200G (BH) max: 19.5MGOe Comparative Example-Br: 9290G bHc: 6970G (BH) max: 18.3MGOe Subsequently, FIG. 2 shows the results of the temperature characteristic test. FIG. 2 shows the result of the product of the present invention, and FIG. 2 shows the result of the conventional product which is a comparative example. Generally, resin-bonded magnets are considered to have poor heat resistance, but according to the present invention, not only magnetic properties but also heat resistance can be improved.
以上述べたように本発明によれば、磁気性能、特にエネ
ルギー積，保磁力ｂＨｃと耐熱性の向上という効果を有
する。As described above, according to the present invention, magnetic properties, particularly energy product, coercive force bHc and heat resistance are improved.
第１図は、希土類磁石中での希土類元素の酸化過程を示
す図。 …斜線部は、希土類磁石の表面部 …希土類磁石の粒界 第２図は、１００℃における、樹脂ボンド型希土類磁石
の安定性を示す。FIG. 1 is a diagram showing the oxidation process of rare earth elements in a rare earth magnet. ... The shaded area is the surface of the rare earth magnet ... Grain boundary of the rare earth magnet Fig. 2 shows the stability of the resin-bonded rare earth magnet at 100 ° C.
Claims (1)
造する方法において、該製造に要する熱処理工程を実施
するに際し、粉砕前のインゴット状態において磁石合金
素材の表面にあらかじめ厚さ５００〜３０００Åの酸化
膜を付与した後に前記熱処理を行うことを特徴とする、
希土類永久磁石の製造方法。1. A method for producing a rare earth permanent magnet by a resin bonding method, wherein when a heat treatment step required for the production is carried out, an oxide film having a thickness of 500 to 3000 Å is previously formed on the surface of a magnet alloy material in an ingot state before pulverization. Characterized by performing the heat treatment after applying
Manufacturing method of rare earth permanent magnet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59073997A JPH0611006B2 (en) | 1984-04-13 | 1984-04-13 | Rare earth permanent magnet manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59073997A JPH0611006B2 (en) | 1984-04-13 | 1984-04-13 | Rare earth permanent magnet manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60218805A JPS60218805A (en) | 1985-11-01 |
| JPH0611006B2 true JPH0611006B2 (en) | 1994-02-09 |
Family
ID=13534274
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59073997A Expired - Lifetime JPH0611006B2 (en) | 1984-04-13 | 1984-04-13 | Rare earth permanent magnet manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0611006B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6084720B2 (en) * | 2016-03-09 | 2017-02-22 | 株式会社東芝 | Automobile |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5155722A (en) * | 1974-11-12 | 1976-05-17 | Tohoku Metal Ind Ltd | Kidorui kobarutoshoketsugataeikyujishakuzairyono seizohoho |
| JPS53110920A (en) * | 1977-03-10 | 1978-09-28 | Namiki Precision Jewel Co Ltd | Method of making rare earth cobalt based permanent magnet alloy |
-
1984
- 1984-04-13 JP JP59073997A patent/JPH0611006B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60218805A (en) | 1985-11-01 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |