JP2002088451A - Rare earth magnet and its manufacturing method - Google Patents
Rare earth magnet and its manufacturing methodInfo
- Publication number
- JP2002088451A JP2002088451A JP2001202124A JP2001202124A JP2002088451A JP 2002088451 A JP2002088451 A JP 2002088451A JP 2001202124 A JP2001202124 A JP 2001202124A JP 2001202124 A JP2001202124 A JP 2001202124A JP 2002088451 A JP2002088451 A JP 2002088451A
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- atomic
- rapidly solidified
- rare earth
- producing
- 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.)
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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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
-
- 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
- H01F1/058—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IVa elements, e.g. Gd2Fe14C
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、希土類磁石および
その製造方法に関する。The present invention relates to a rare earth magnet and a method for manufacturing the same.
【０００２】[0002]
【従来の技術】従来、Ｒ−Ｆｅ−Ｂ型希土類焼結磁石を
製造する場合において、焼結体の結晶粒径を微細化する
とともに磁石の耐熱性を向上させることを目的として、
Ｎｂ（ニオブ）を原料合金に添加することが提案されて
いた。Ｎｂは、焼結時における結晶粒の粗大化を抑制
し、磁石の着磁特性を改善することが知られている。2. Description of the Related Art Conventionally, in the production of R-Fe-B type rare earth sintered magnets, the purpose of the present invention is to reduce the crystal grain size of the sintered body and improve the heat resistance of the magnet.
It has been proposed to add Nb (niobium) to a raw material alloy. Nb is known to suppress the coarsening of crystal grains during sintering and improve the magnetizing characteristics of the magnet.
【０００３】特開平７−９４３１１号公報は、Ｎｄ−Ｆ
ｅ−Ｃｏ−Ｂ型焼結磁石に０．１〜２．０重量％のＮｂ
を添加し、磁石特性および耐熱性を改善する技術を開示
している。[0003] Japanese Patent Application Laid-Open No. 7-94311 discloses an Nd-F
0.1-2.0 wt% Nb in e-Co-B type sintered magnet
To improve magnet properties and heat resistance.
【０００４】また、特公平６−６９００３号公報は、超
急冷法によって希土類磁石合金を作製する場合におい
て、１〜１０原子％の金属元素（Ｔｉ、Ｚｒ、Ｈｆ、Ｎ
ｂなどの金属元素）を原料合金に添加すれば、保磁力な
どの磁石特性を改善できることを開示している。Further, Japanese Patent Publication No. 6-69003 discloses that when a rare earth magnet alloy is produced by a rapid quenching method, 1 to 10 atomic% of a metal element (Ti, Zr, Hf, N
It discloses that by adding a metal element (such as b) to the raw material alloy, magnet properties such as coercive force can be improved.
【０００５】[0005]
【発明が解決しようとする課題】特開平７−９４３１１
号公報に記載されている従来技術によれば、インゴット
鋳造方法によって合金を作製しているため、原料合金の
溶湯を冷却する際、冷却速度が遅い。そのため、ＮｂＦ
ｅＢ2などの非磁性ホウ化物が粗大に形成されやすい。
このような非磁性ホウ化物が生成されると、焼結プロセ
ス後における希土類磁石が硬化するため、切断加工や表
面研磨加工などの処理能率が大きく低下してしまう。Problems to be Solved by the Invention Japanese Patent Application Laid-Open No. 7-94311
According to the prior art described in Japanese Patent Application Laid-Open Publication No. H11-107, since the alloy is manufactured by the ingot casting method, the cooling rate is low when cooling the melt of the raw material alloy. Therefore, NbF
Non-magnetic borides such as eB 2 are likely to be formed coarsely.
When such a nonmagnetic boride is generated, the rare-earth magnet after the sintering process is hardened, so that the processing efficiency such as cutting and surface polishing is greatly reduced.
【０００６】一方、特公平６−６９００３号公報に記載
されている従来技術では、添加するＮｂなどの金属量が
多いため、ＮｂＦｅＢ2などの非磁性ホウ化物が生成さ
れやすい。その結果、焼結プロセス後における希土類磁
石の残留磁束密度が低下するとともに、磁石の加工能率
も低下してしまう。On the other hand, in the prior art described in Japanese Patent Publication No. 6-69003, non-magnetic borides such as NbFeB 2 are easily generated because the amount of metal such as Nb is large. As a result, the residual magnetic flux density of the rare earth magnet after the sintering process decreases, and the processing efficiency of the magnet also decreases.
【０００７】本発明はかかる諸点に鑑みてなされたもの
であり、その主な目的は、永久磁石特性および加工性の
両方に優れた希土類磁石およびその製造方法を提供する
ことにある。The present invention has been made in view of the above points, and a main object of the present invention is to provide a rare earth magnet excellent in both permanent magnet properties and workability, and a method for manufacturing the same.
【０００８】[0008]
【課題を解決するための手段】本発明の急冷凝固合金
は、組成式が（Ｆｅ1-mＴm）100-x-y-zＱxＲyＭz（Ｔは
ＣｏおよびＮｉからなる群から選択された１種以上の元
素、ＱはＢおよびＣからなる群から選択された１種以上
の元素、Ｒは１種以上の希土類金属元素、ＭはＮｂおよ
びＭｏからなる群から選択された少なくとも１種の元
素）で表現され、組成比率ｘ、ｙ、ｚおよびｍが、それ
ぞれ、２≦ｘ≦２８（原子％）、８≦ｙ≦３０（原子
％）、０．１≦ｚ＜１．０（原子％）、および０≦ｍ≦
０．５を満足する。Means for Solving the Problems] rapidly solidified alloys of the present invention, composition formula (Fe 1-m T m) 100-xyz Q x R y M z (T is selected from the group consisting of Co and Ni One or more elements, Q is one or more elements selected from the group consisting of B and C, R is one or more rare earth metal elements, and M is at least one element selected from the group consisting of Nb and Mo. And the composition ratios x, y, z, and m are 2 ≦ x ≦ 28 (atomic%), 8 ≦ y ≦ 30 (atomic%), and 0.1 ≦ z <1.0 (atomic %), And 0 ≦ m ≦
0.5 is satisfied.
【０００９】原料合金の溶湯を急冷して製造する際の冷
却速度が１０2Ｋ／秒以上１０4Ｋ／秒以下の範囲内にあ
ることが好ましい。[0009] It is preferable that the cooling rate when the molten alloy of the raw material alloy is rapidly cooled is in the range of 10 2 K / sec to 10 4 K / sec.
【００１０】ある好ましい実施形態においては、Ｎｂを
必須元素として含有する。[0010] In a preferred embodiment, Nb is contained as an essential element.
【００１１】ある好ましい実施形態においては、短軸方
向サイズが０．１μｍ以上１００μｍ以下で長軸方向サ
イズが５μｍ以上５００μｍ以下のＲ2Ｆｅ14Ｂ型化合
物結晶粒と、前記結晶粒の粒界に分散して存在するＲリ
ッチ相とを含有しており、厚さが０．０３ｍｍ以上１０
ｍｍ以下である。In a preferred embodiment, R 2 Fe 14 B type compound crystal grains having a minor axis size of 0.1 μm or more and 100 μm or less and a major axis size of 5 μm or more and 500 μm or less are provided. Containing an R-rich phase present in a dispersed state and having a thickness of 0.03 mm or more and 10
mm or less.
【００１２】本発明による希土類磁石は、上記いずれか
の急冷凝固合金から形成されたことを特徴とする。[0012] A rare earth magnet according to the present invention is characterized by being formed from any of the rapidly solidified alloys described above.
【００１３】本発明の希土類磁石は、原子比率で０．１
％以上１．０％以下のＮｂおよび／またはＭｏが添加さ
れた急冷凝固合金から形成されている。The rare earth magnet of the present invention has an atomic ratio of 0.1
% Of Nb and / or Mo of 1.0% or less.
【００１４】本発明による希土類磁石の製造方法は、組
成式が（Ｆｅ1-mＴm）100-x-y-zＱxＲyＭz（ＴはＣｏお
よびＮｉからなる群から選択された１種以上の元素、Ｑ
はＢおよびＣからなる群から選択された１種以上の元
素、Ｒは１種以上の希土類金属元素、ＭはＮｂおよびＭ
ｏからなる群から選択された少なくとも１種の元素）で
表現され、組成比率ｘ、ｙ、ｚ、およびｍが、それぞ
れ、２≦ｘ≦２８（原子％）、８≦ｙ≦３０（原子
％）、０．１≦ｚ＜１．０原子％、および０≦ｍ≦０．
５を満足する合金の溶湯を急冷し、凝固させることによ
って急冷凝固合金を作製する工程と、前記急冷凝固合金
から永久磁石を作製する工程とを包含する。The method for producing a rare earth magnet according to the present invention is characterized in that the composition formula is (Fe 1 -m T m ) 100 -xyz Q x R y M z (T is at least one selected from the group consisting of Co and Ni). Element, Q
Is one or more elements selected from the group consisting of B and C, R is one or more rare earth metal elements, M is Nb and M
o, and the composition ratios x, y, z, and m are respectively 2 ≦ x ≦ 28 (atomic%) and 8 ≦ y ≦ 30 (atomic%). ), 0.1 ≦ z <1.0 at%, and 0 ≦ m ≦ 0.
The method includes a step of rapidly cooling and solidifying a molten alloy satisfying No. 5 to produce a rapidly solidified alloy, and a step of producing a permanent magnet from the rapidly solidified alloy.
【００１５】前記急冷凝固合金を作製する工程におい
て、冷却速度を１０2Ｋ／秒以上１０4Ｋ／秒以下の範囲
内にすることが好ましい。[0015] In the step of producing the rapidly solidified alloy, it is preferable that the cooling rate be in the range of 10 2 K / sec to 10 4 K / sec.
【００１６】ある好ましい実施形態では、前記急冷凝固
合金を作製する工程において、前記合金の溶湯をストリ
ップキャスト法によって急冷する。In a preferred embodiment, in the step of producing the rapidly solidified alloy, a molten metal of the alloy is rapidly cooled by a strip casting method.
【００１７】ある好ましい実施形態では、前記急冷凝固
合金に水素を吸蔵させた後、前記水素を放出させる脆化
工程を包含する。[0017] In a preferred embodiment, the method includes an embrittlement step of releasing hydrogen after absorbing the hydrogen into the rapidly solidified alloy.
【００１８】[0018]
【発明の実施の形態】本発明者は、原料合金の溶湯を１
０2〜１０4Ｋ／秒の冷却速度で急冷し、凝固合金を作製
する場合、ＮｂやＭｏを僅かに（全体の１．０原子％未
満）添加しただけでも、それらの添加物が合金組織中に
均一に分散する結果、添加金属のホウ化物生成に起因し
た焼結磁石の残留磁束密度低下や加工性劣化を抑制しつ
つ、保磁力を増加させ、かつ、減磁曲線の角形性を良好
なものとすることができることを見出した。BEST MODE FOR CARRYING OUT THE INVENTION The inventor of the present invention has prepared a
When quenching at a cooling rate of 0 2 to 10 4 K / sec to produce a solidified alloy, even if Nb or Mo is slightly added (less than 1.0 atomic% of the whole), the addition of the alloy causes an alloy structure. As a result, the coercive force is increased and the squareness of the demagnetization curve is improved while suppressing the reduction of the residual magnetic flux density and the deterioration of workability of the sintered magnet due to boride formation of the added metal It was found that it can be.
【００１９】従来のインゴット鋳造法による場合、保磁
力増加のためには、比較的多くのＮｂなどを添加するこ
とが必要であると考えられていた。しかしながら、スト
リップキャスト法によって急冷凝固合金を作製する場
合、従来通り必要とされていた量だけＮｂを添加する
と、最終的に得られる焼結磁石の硬度が極めて上昇し、
焼結磁石に必須の表面研磨・切断などの加工が著しく困
難になることがわかった。In the case of the conventional ingot casting method, it has been considered that it is necessary to add a relatively large amount of Nb or the like in order to increase the coercive force. However, when producing a rapidly solidified alloy by the strip casting method, if Nb is added in an amount required conventionally, the hardness of the finally obtained sintered magnet is extremely increased,
It has been found that processing such as surface polishing and cutting, which is essential for sintered magnets, becomes extremely difficult.
【００２０】そこで、添加するＮｂなどの量を従来必要
とされていた量よりも少なくしたところ、インゴット鋳
造法による場合に比較して保磁力を画期的に増大させ、
しかも、残留磁束密度の低下や加工性の低下を極力抑え
ることに成功した。Therefore, when the amount of Nb or the like to be added is made smaller than conventionally required, the coercive force is remarkably increased as compared with the case of the ingot casting method.
In addition, it succeeded in minimizing a decrease in residual magnetic flux density and a decrease in workability.
【００２１】このように、添加すべきＮｂやＭｏの最適
量が合金溶湯の冷却速度に強く依存して変化する理由は
未だ解明されてはいないが、冷却速度の範囲を限定する
ことによって合金組織の微細化が実現する結果、微量で
あってもＮｂなどの添加による効果が充分に発揮される
ためであると考えられる。Although the reason why the optimum amount of Nb or Mo to be added strongly depends on the cooling rate of the molten alloy has not been elucidated, it is not clear yet. It is considered that the effect of the addition of Nb or the like is sufficiently exerted even in a small amount as a result of the realization of finer particles.
【００２２】本発明では、組成式が（Ｆｅ1-mＴm）
100-x-y-zＱxＲyＭzで表現される原料合金の溶湯を用意
する。ここで、ＴはＣｏおよびＮｉからなる群から選択
された１種以上の元素、ＱはＢおよびＣからなる群から
選択された１種以上の元素、Ｒは１種以上の希土類金属
元素、ＭはＮｂおよびＭｏからなる群から選択された少
なくとも１種の元素である。そして、組成比率ｘ、ｙ、
ｚ、およびｍが、それぞれ、２≦ｘ≦２８（原子％）、
８≦ｙ≦３０（原子％）、０．１≦ｚ＜１．０原子％、
および０≦ｍ≦０．５を満足する。In the present invention, the composition formula is (Fe 1-m T m )
100-xyz Q x R y M z preparing a melt of the material alloy represented by. Here, T is one or more elements selected from the group consisting of Co and Ni, Q is one or more elements selected from the group consisting of B and C, R is one or more rare earth metal elements, M Is at least one element selected from the group consisting of Nb and Mo. And the composition ratio x, y,
z and m are respectively 2 ≦ x ≦ 28 (atomic%);
8 ≦ y ≦ 30 (atomic%), 0.1 ≦ z <1.0 atomic%,
And 0 ≦ m ≦ 0.5.
【００２３】なお、保磁力向上のためには、Ｄｙおよび
／またはＴｂを１．０ａｔ％以上含有することが好まし
い。In order to improve coercive force, it is preferable that Dy and / or Tb be contained in an amount of 1.0 at% or more.
【００２４】このように、ＮｂやＭｏが添加された合金
の溶湯を公知のストリップキャスト装置などの液体急冷
装置を用いて冷却し、凝固させる。本発明では、このと
きの冷却速度を１．０×１０2Ｋ／秒以上１．０×１０4
Ｋ／秒以下の範囲内に制御する。この冷却速度は、合金
の溶湯が冷却ロールの表面に接触してから、合金温度が
約５００℃くで低下する間に達成されることが望まし
い。より好ましい冷却速度の範囲は２×１０2Ｋ／秒以
上１×１０3Ｋ／秒以下であり、更に好ましい冷却速度
の範囲は、３×１０2Ｋ／秒以上６×１０2Ｋ／秒以下で
ある。As described above, the melt of the alloy to which Nb or Mo is added is cooled and solidified by using a known liquid quenching device such as a strip casting device. In the present invention, the cooling rate at this time is set to 1.0 × 10 2 K / sec or more and 1.0 × 10 4 K / sec or more.
Control is performed within the range of K / sec or less. This cooling rate is desirably achieved during the time the alloy temperature drops to about 500 ° C. after the molten alloy contacts the surface of the chill roll. A more preferable range of the cooling rate is 2 × 10 2 K / sec to 1 × 10 3 K / sec, and a still more preferable range of the cooling rate is 3 × 10 2 K / sec to 6 × 10 2 K / sec. It is.
【００２５】なお、添加するＮｂおよび／またはＭｏの
量の範囲は、後述する実験結果などを考慮すると、０．
１≦ｚ＜１．０（原子％）であることが好ましく、０．
２０≦ｚ＜０．９５（原子％）であることがより好まし
く、０．３５≦ｚ＜０．７５（原子％）であることが更
に好ましい。Incidentally, the range of the amount of Nb and / or Mo to be added is set to 0.1 in consideration of the experimental results described later.
It is preferable that 1 ≦ z <1.0 (atomic%).
It is more preferable that 20 ≦ z <0.95 (atomic%), and it is even more preferable that 0.35 ≦ z <0.75 (atomic%).
【００２６】以下、本発明による希土類磁石の製造方法
の一実施形態を詳細に説明する。Hereinafter, an embodiment of the method for manufacturing a rare earth magnet according to the present invention will be described in detail.
【００２７】まず、Ｒ（但しＲはＹを含む希土類元素の
うち、少なくとも１種）：８〜３０原子％、Ｂ：２〜２
８原子％、Ｎｂ：０．１〜１．０原子％、残部：Ｆｅ、
および不可避的不純物を含有するＲ−Ｆｅ−Ｂ系合金の
溶湯を作製する。ただし、Ｆｅの一部をＣｏ、Ｎｉの１
種または２種にて置換してもよいし、Ｂの一部をＣで置
換しても良い。さらに、Ｂの一部をＳｉ、Ｐ、および／
またはＳなとで置換してもよい。First, R (where R is at least one of the rare earth elements including Y): 8 to 30 atomic%, B: 2-2
8 atomic%, Nb: 0.1 to 1.0 atomic%, balance: Fe,
In addition, a melt of an R-Fe-B-based alloy containing unavoidable impurities is produced. However, part of Fe is Co and Ni is 1
Species or two kinds may be substituted, or part of B may be substituted with C. Further, part of B is Si, P, and / or
Alternatively, it may be replaced with S.
【００２８】次に、この合金溶湯をストリップキャスト
法によって１０2〜１０4Ｋ／秒の冷却速度にて厚さ０．
０３ｍｍ〜１０ｍｍの薄板状に急冷凝固する。このよう
にしてＲ2Ｆｅ14Ｂ型正方晶を主たる相とし、Ｒリッチ
相が５μｍ以下の微細なサイズで分離した組織を有する
鋳片に鋳造した後、鋳片を吸排気可能な容器に収容す
る。更に、容器内を真空引きした後、容器内に圧力０．
０３ＭＰａ〜１．０ＭＰａのＨ2ガスを供給し、崩壊合
金粉を形成する。このような崩壊合金粉は、脱水素処理
後、不活性ガス気流中で微粉砕されることが好ましい。Next, this alloy melt was subjected to a strip casting method at a cooling rate of 10 2 to 10 4 K / sec.
Rapid solidification into a thin plate of 03 mm to 10 mm. In this way, the R 2 Fe 14 B-type tetragonal crystal is used as a main phase, and the R-rich phase is cast into a slab having a microstructure separated at a fine size of 5 μm or less. I do. Further, after the inside of the container was evacuated, a pressure of 0.
Supplying a H 2 gas of 03MPa～1.0MPa, to form the disintegration alloy powder. It is preferable that such a disintegrated alloy powder is finely pulverized in an inert gas stream after the dehydrogenation treatment.
【００２９】本発明で使用する磁石材料の鋳片は、特定
組成の合金溶湯を単ロール法または双ロール法によるス
トリップキャスト法によって急冷することにより、好適
に製造される。作製する鋳片の板厚に応じて、単ロール
法と双ロール法とを使い分けることができる。鋳片が厚
い場合は双ロール法を用いることが好ましく、薄い場合
は単ロール法を用いることが好ましい。The slab of the magnetic material used in the present invention is preferably produced by quenching a molten alloy having a specific composition by a strip casting method using a single roll method or a twin roll method. The single roll method and the twin roll method can be used depending on the thickness of the cast slab to be produced. When the slab is thick, it is preferable to use the twin roll method, and when it is thin, it is preferable to use the single roll method.
【００３０】鋳片の厚さが０．０３ｍｍ未満になると急
冷効果が大きくなるため、結晶粒径が小さくなりすぎる
おそれがある。結晶粒径が小さすぎると、粉末化された
ときに粒子個々が多結晶化し、結晶方位を揃えられなく
なるため、磁気特性の劣化を招来する。逆に鋳片の厚さ
が１０ｍｍを超えると、冷却速度が遅くなるため、α−
Ｆｅ相が多量に析出しやすく、Ｎｄリッチ相の偏在も生
じる。鋳片の厚さのより好ましい範囲は、０．１ｍｍ以
上５ｍｍ以下である。If the thickness of the slab is less than 0.03 mm, the quenching effect becomes large, and the crystal grain size may be too small. If the crystal grain size is too small, the individual particles become polycrystallized when powdered, and the crystal orientation cannot be aligned, resulting in deterioration of magnetic properties. Conversely, when the thickness of the slab exceeds 10 mm, the cooling rate becomes slow, so that α-
A large amount of the Fe phase is likely to precipitate, and the Nd-rich phase is unevenly distributed. A more preferable range of the thickness of the slab is 0.1 mm or more and 5 mm or less.
【００３１】水素吸蔵処理は、例えば、次のようにして
行われ得る。すなわち、所定の大きさに破断した鋳片を
原料ケース内に挿入した後、原料ケースを密閉可能な水
素炉に挿入し、その水素炉を密閉する。次に、その水素
炉内を十分に真空引きした後、圧力が３０ｋＰａ〜１．
０ＭＰａの水素ガスを容器内に供給し、鋳片に水素を吸
蔵させる。合金鋳片は水素の吸蔵によって自然崩壊す
る。The hydrogen storage process can be performed, for example, as follows. That is, after the slab broken into a predetermined size is inserted into the raw material case, the raw material case is inserted into a sealable hydrogen furnace, and the hydrogen furnace is sealed. Next, after the inside of the hydrogen furnace is sufficiently evacuated, the pressure is set to 30 kPa to 1.
A hydrogen gas of 0 MPa is supplied into the container, and hydrogen is absorbed in the cast slab. The alloy slab spontaneously disintegrates due to the storage of hydrogen.
【００３２】水素の吸蔵によって脆化した合金を冷却し
た後、真空中で脱水素処理を行う。脱水素処理によって
得られた合金粉末には微細亀裂が存在するため、その後
にボール・ミル、ジェットミル等で短時間で微粉砕さ
れ、２〜６μｍの粒径（FSSSサイズ）を持った合金粉末
を作製することができる。水素粉砕処理の好ましい態様
については、特開平７−１８３６６号公報に開示されて
いる。After the alloy embrittled by the occlusion of hydrogen is cooled, a dehydrogenation treatment is performed in a vacuum. Since the alloy powder obtained by the dehydrogenation treatment has fine cracks, it is then finely pulverized in a short time using a ball mill, jet mill, etc., and has a particle size (FSSS size) of 2 to 6 μm. Can be produced. A preferred embodiment of the hydrogen crushing treatment is disclosed in JP-A-7-18366.
【００３３】上述の微粉砕は、雰囲気ガスとして不活性
ガス（例えば、Ｎ2やＡｒなど）を用いたジェット・ミ
ルによって行うことが好ましいが、有機溶媒（例えば、
ベンゼンやトルエン等）を用いたボールミルやアトライ
ターによって行っても良い。The above-mentioned pulverization is preferably carried out by a jet mill using an inert gas (for example, N 2 or Ar) as an atmospheric gas.
It may be performed by a ball mill or an attritor using benzene or toluene.
【００３４】なお、以上の粉砕工程に際して、粉末に含
有される酸素の量が低く抑えられるように不活性雰囲気
ガス中の酸素濃度を低く（例えば５００ｐｐｍ以下）に
管理してもよい。In the above-mentioned pulverizing step, the oxygen concentration in the inert atmosphere gas may be controlled to be low (for example, 500 ppm or less) so that the amount of oxygen contained in the powder is kept low.
【００３５】上記合金粉末には脂肪酸エステルなどを主
成分とする液体潤滑剤を添加することが好ましい。添加
量は例えば０．１５〜５．０質量％である。脂肪酸エス
テルとしては、カプロン酸メチル、カプリル酸メチル、
ラウリン酸メチルなとが挙げられる。潤滑剤には結合剤
などの成分が含まれていても良い。重要な点は、後の工
程で潤滑剤が揮発し、除去され得ることにある。また、
潤滑剤それ自体が合金粉末と均一に混合しにくい固形状
のものである場合は、溶剤で希釈して用いれば良い。溶
剤としては、イソパラフィンに代表される石油系溶剤や
ナフテン系溶剤等を用いることができる。潤滑剤添加の
タイミングは任意であり、微粉砕前、微粉砕中、微粉砕
後のいずれであっても良い。液体潤滑剤は、粉末粒子の
表面を被覆し、粒子の酸化防止効果を発揮するととも
に、プレスに際して成形体の密度を均一化し、磁界中で
の配向度を向上させる機能を発揮する。It is preferable to add a liquid lubricant mainly containing a fatty acid ester or the like to the alloy powder. The addition amount is, for example, 0.15 to 5.0% by mass. Fatty acid esters include methyl caproate, methyl caprylate,
Methyl laurate. The lubricant may include components such as a binder. The important point is that the lubricant can volatilize and be removed in a later step. Also,
If the lubricant itself is a solid that is difficult to mix uniformly with the alloy powder, it may be diluted with a solvent before use. As the solvent, a petroleum solvent represented by isoparaffin, a naphthene solvent, or the like can be used. The timing of adding the lubricant is arbitrary, and may be before, during, or after pulverization. The liquid lubricant covers the surfaces of the powder particles, exhibits an effect of preventing the particles from being oxidized, and also has a function of making the density of the molded body uniform during pressing and improving the degree of orientation in a magnetic field.
【００３６】次に、プレス装置を用いて磁界配向および
圧縮成形を行う。磁性粉末の充填密度は、磁界配向を可
能にする範囲（真密度の例えば３０〜４０％）内に設定
される。Next, magnetic field orientation and compression molding are performed using a press device. The packing density of the magnetic powder is set in a range (for example, 30 to 40% of the true density) that enables the magnetic field orientation.
【００３７】成形体は、プレス装置から取り出された
後、脱バインダー工程、焼結工程、時効処理工程などの
公知の製造プロセスを経て最終的に永久磁石製品とな
る。After the molded body is taken out of the pressing device, it undergoes a known manufacturing process such as a binder removal step, a sintering step, and an aging step, and finally becomes a permanent magnet product.
【００３８】（実施例と比較例）まず、下記の表１の上
段側に示す組成を持つ薄片状合金（試料Ｎｏ．１〜８）
をストリップキャスト法によって作製した。このときの
合金溶湯の冷却速度は、ロール接触側と反対側とで異な
るが、２×１０2〜８×１０2Ｋ／秒程度の範囲内にあっ
た。また、下記表１の下段側に示す組成を持つ薄片状合
金（試料Ｎｏ．９〜１６）をインゴット鋳造法によって
作製した。(Examples and Comparative Examples) First, flaky alloys having the compositions shown in the upper part of Table 1 below (Sample Nos. 1 to 8)
Was produced by a strip casting method. The cooling rate of the molten alloy at this time was different between the roll contact side and the opposite side, but was in the range of about 2 × 10 2 to 8 × 10 2 K / sec. Further, flaky alloys (samples Nos. 9 to 16) having compositions shown in the lower part of Table 1 below were produced by ingot casting.
【００３９】[0039]
【表１】 [Table 1]
【００４０】上記表１において、各元素の組成比率の単
位は「原子％」である。試料Ｎｏ．１〜１６では、Ｎｂ
の添加量が０．００原子％から２．８７原子％までの範
囲で変化しているが、他の元素の組成比率は実質的に等
しく設定されている。なお、本発明の実施例および比較
例は、それぞれ、試料Ｎｏ．２〜５、および試料Ｎｏ．
１、６〜１６に対応している。参考のため、上記試料Ｎ
ｏ．1〜１６の組成を重量％に換算した値を下記の表２
に示す。In the above Table 1, the unit of the composition ratio of each element is “atomic%”. Sample No. In 1-16, Nb
Varies from 0.00 atomic% to 2.87 atomic%, but the composition ratios of the other elements are set to be substantially equal. Note that the examples and comparative examples of the present invention correspond to sample Nos. Nos. 2 to 5 and sample Nos.
1, 6 to 16. For reference, the sample N
o. Table 2 below shows the values obtained by converting the compositions of Nos. 1 to 16 into% by weight.
Shown in
【００４１】[0041]
【表２】 [Table 2]
【００４２】表１および表２に示す組成を有する各急冷
合金に対し、水素吸蔵／放出による脆化・粗粉砕を行な
った後、更にジェットミル粉砕装置により、平均粒径
（ＦＳＳＳサイズ）が約３．５μｍになるように微粉砕
した。こうして得た微粉砕粉をプレス装置で成形し、粉
末成形体を作製した後、低圧アルゴン雰囲気（１００Ｔ
ｏｒｒ＝およそ１３．３ｋＰａ）中にて焼結した。この
焼結により、２７ｍｍ×５２ｍｍ×５２ｍｍのサイズを
持った焼結磁石が作製された。After each of the quenched alloys having the compositions shown in Tables 1 and 2 was subjected to embrittlement and coarse pulverization by hydrogen absorption / release, the average particle size (FSSS size) was further reduced by a jet mill pulverizer. It was pulverized to 3.5 μm. The finely pulverized powder thus obtained is molded by a press device to form a powder compact, and then is subjected to a low-pressure argon atmosphere (100T).
orr = about 13.3 kPa). By this sintering, a sintered magnet having a size of 27 mm × 52 mm × 52 mm was produced.
【００４３】上記焼結磁石の各々について得られた保磁
力Ｈcjおよび残留磁束密度Ｂrの測定値を表１に示す。
また、保磁力ＨcjのＮｂ添加量（原子％）依存性、およ
び残留磁束密度ＢrのＮｂ添加量（原子％）依存性を、
それぞれ、図１および図２に示す。参考のため、図１お
よび図２には比較例に関する測定データも表示されてい
る。この比較例は、実施例（試料Ｎｏ．２〜５）と同様
の合金組成を持ちながらインゴット鋳造法（合金溶湯の
冷却速度：５〜４０Ｋ／秒）によって作製された試料
（Ｎｏ．１０〜１３）と、ストリップキャスト法によっ
て作製されたが、Ｎｂ添加量が本発明で規定する所定範
囲を外れている試料（Ｎｏ．１、６〜８）の両方を含ん
でいる。[0043] Table 1 shows the measured values of the sintered coercive force obtained for each of the magnets H cj and remanence B r.
Further, Nb addition amount of the coercive force H cj (atomic%) dependent, and Nb amount of residual magnetic flux density B r (atomic%) dependent,
These are shown in FIGS. 1 and 2, respectively. For reference, FIGS. 1 and 2 also show measurement data for the comparative example. In this comparative example, samples (Nos. 10 to 13) produced by ingot casting (cooling rate of molten alloy: 5 to 40 K / sec) while having the same alloy composition as the examples (Samples Nos. 2 to 5). ) And samples (No. 1, 6 to 8) produced by the strip casting method, but the amount of Nb added is out of the predetermined range specified in the present invention.
【００４４】図１からわかるように、ストリップキャス
ト法による場合は、Ｎｂ添加による保磁力増大の効果が
極めて顕著であった。より詳細には、Ｎｂ添加量が０．
１〜１．０原子％という範囲において保磁力の増加が急
激に進行し、Ｎｂ添加量が１．０原子％以上になると、
保磁力増加が飽和する傾向にあった。また、Ｎｂの添加
によって磁石の耐熱性が向上することも確認できた。こ
れに対して、インゴット鋳造法による場合は、Ｎｂ添加
による保磁力増大の効果はほとんど生じていないことが
わかった。As can be seen from FIG. 1, in the case of the strip casting method, the effect of increasing the coercive force by adding Nb was extremely remarkable. More specifically, the amount of Nb added is 0.
When the coercive force rapidly increases in the range of 1 to 1.0 at% and the Nb addition amount becomes 1.0 at% or more,
The increase in coercive force tended to be saturated. It was also confirmed that the heat resistance of the magnet was improved by the addition of Nb. On the other hand, in the case of the ingot casting method, it was found that the effect of increasing the coercive force by adding Nb hardly occurred.
【００４５】残留磁束密度Ｂrは、図２からわかるよう
に、合金溶湯の冷却方法によらずＮｂ添加量の増加に伴
って減少した。The residual magnetic flux density B r, as can be seen from FIG. 2, and decreases with increasing Nb addition amount regardless of the method of cooling the molten alloy.
【００４６】図３は、ストリップキャスト法による急冷
合金の粉末から作製した焼結磁石について、研削抵抗と
Ｎｂ添加量との関係を示すグラフである。この研削抵抗
は、切断刃を駆動するモータの負荷電流から計算によっ
て求めた。研削抵抗は、図３からわかるように、Ｎｂの
増加に伴って単調に増大している。このことは、Ｎｂに
よって焼結磁石が硬化し、加工性低下を招くことを示し
ている。FIG. 3 is a graph showing the relationship between the grinding resistance and the amount of Nb added for a sintered magnet produced from a quenched alloy powder by the strip casting method. This grinding resistance was obtained by calculation from the load current of the motor that drives the cutting blade. As can be seen from FIG. 3, the grinding resistance monotonically increases with an increase in Nb. This indicates that the sintered magnet is hardened by Nb, resulting in a reduction in workability.
【００４７】以上のことから、原料合金に添加すべきＮ
ｂの量は、０．１原子％以上１．０原子％未満であるこ
とが好ましいことがわかる。Ｎｂを１．０原子％以上添
加すると、Ｎｂの硼化物生成が顕著となり、飽和磁化の
低下および加工性の低下が問題になるからである。ま
た、Ｎｂの添加量が０．１原子％を下回ると、Ｎｂ添加
による保磁力増大効果などの発現が不充分となるので望
ましくない。Ｎｂ添加量のより好ましい範囲は、０．２
０原子％以上０．９５原子％未満であり、更に好ましい
範囲は０．３５原子％以上０．７５原子％未満である。From the above, N to be added to the raw material alloy
It is understood that the amount of b is preferably at least 0.1 atomic% and less than 1.0 atomic%. This is because if Nb is added in an amount of 1.0 atomic% or more, boride generation of Nb becomes remarkable, and a decrease in saturation magnetization and a decrease in workability become problems. On the other hand, if the addition amount of Nb is less than 0.1 atomic%, the effect of increasing the coercive force due to the addition of Nb becomes insufficient, which is not desirable. A more preferred range of the Nb addition amount is 0.2
0 atomic% or more and less than 0.95 atomic%, and a more preferable range is 0.35 atomic% or more and less than 0.75 atomic%.
【００４８】なお、Ｍ元素として、ＮｂやＭｏの代わり
に、または、これらの元素とともにら、ＶやＺｒを用い
ることもできる。ただし、ＶやＺｒは磁気特性を不安定
化するため、ＶやＺｒよりもＮｂやＭｏを添加すること
が好ましい。As the M element, V or Zr can be used instead of Nb or Mo or together with these elements. However, since V and Zr destabilize the magnetic properties, it is preferable to add Nb or Mo rather than V or Zr.
【００４９】[0049]
【発明の効果】本発明によれば、ＮｂやＭｏを急冷合金
の微細組織中に均一に分散させることにより、僅かな添
加量（０．１原子％以上１．０原子％未満）であっても
焼結時の粒成長を効果的に抑制できるため、希土類焼結
磁石の残留磁束密度や加工性をほとんど低下させること
なく、保磁力を充分に増大させ、しかも、減磁曲線の角
形性を良好なものとすることが可能になる。According to the present invention, Nb and Mo are uniformly dispersed in the microstructure of the quenched alloy so that a small amount (0.1 atomic% or more and less than 1.0 atomic%) can be obtained. Can effectively suppress the grain growth during sintering, so that the coercive force can be sufficiently increased and the squareness of the demagnetization curve can be increased without substantially reducing the residual magnetic flux density and workability of the rare earth sintered magnet. It becomes possible to be good.
【図１】本発明の実施例および比較例について、保磁力
ＨcjのＮｂ添加量（原子％）依存性を示すグラフであ
る。FIG. 1 is a graph showing the dependency of coercive force H cj on the amount of added Nb (atomic%) in Examples and Comparative Examples of the present invention.
【図２】本発明の実施例および比較例について、残留磁
束密度ＢrのＮｂ添加量（原子％）依存性を示すグラフ
である。For Examples and Comparative Examples of the present invention; FIG is a graph showing the residual Nb addition amount of the magnetic flux density B r (atomic%) dependent.
【図３】本発明の実施例に関して求めた研削抵抗（Ｎ：
ニュートン）のＮｂ添加量（原子％）依存性を示すグラ
フである。FIG. 3 shows the grinding force (N:
9 is a graph showing the dependence of Nb on the amount (atomic%) of Nb.
Claims (10)
yＭz（ＴはＣｏおよびＮｉからなる群から選択された１
種以上の元素、ＱはＢおよびＣからなる群から選択され
た１種以上の元素、Ｒは１種以上の希土類金属元素、Ｍ
はＮｂおよびＭｏからなる群から選択された少なくとも
１種の元素）で表現され、組成比率ｘ、ｙ、ｚ、および
ｍが、それぞれ、 ２≦ｘ≦２８（原子％）、 ８≦ｙ≦３０（原子％）、 ０．１≦ｚ＜１．０（原子％）、および ０≦ｍ≦０．５ を満足する急冷凝固合金。1. The composition formula is (Fe 1 -m T m ) 100-xyz Q x R
y M z (T is 1 selected from the group consisting of Co and Ni
At least one kind of element, Q is at least one kind of element selected from the group consisting of B and C, R is at least one kind of rare earth metal element, M
Is represented by at least one element selected from the group consisting of Nb and Mo), and the composition ratios x, y, z, and m are respectively 2 ≦ x ≦ 28 (atomic%), 8 ≦ y ≦ 30 (At.%), 0.1 ≦ z <1.0 (at.%), And 0 ≦ m ≦ 0.5.
冷却速度が１０2Ｋ／秒以上１０4Ｋ／秒以下の範囲内に
ある請求項１に記載の急冷凝固合金。2. The rapidly solidified alloy according to claim 1, wherein a cooling rate in producing the melt of the raw material alloy by quenching is in the range of 10 2 K / sec to 10 4 K / sec.
に記載の急冷凝固合金。3. The method according to claim 1, wherein Nb is contained as an essential element.
2. The rapidly solidified alloy according to item 1.
μｍ以下で長軸方向サイズが５μｍ以上５００μｍ以下
のＲ2Ｆｅ14Ｂ型化合物結晶粒と、前記結晶粒の粒界に
分散して存在するＲリッチ相とを含有しており、厚さが
０．０３ｍｍ以上１０ｍｍ以下の請求項１に記載の急冷
凝固合金。4. The minor axis direction size is 0.1 μm or more and 100
It contains R 2 Fe 14 B-type compound crystal grains having a major axis size of 5 μm or more and 500 μm or less, and an R-rich phase dispersed and present at grain boundaries of the crystal grains, and has a thickness of 0 μm or less. 2. The rapidly solidified alloy according to claim 1, having a length of 0.03 mm or more and 10 mm or less.
凝固合金から形成された希土類磁石。5. A rare earth magnet formed from the rapidly solidified alloy according to claim 1.
Ｎｂおよび／またはＭｏが添加された急冷凝固合金から
形成された希土類−鉄−ホウ素型磁石。6. A rare earth-iron-boron type magnet formed from a rapidly solidified alloy to which Nb and / or Mo having an atomic ratio of 0.1% or more and 1.0% or less is added.
yＭz（ＴはＣｏおよびＮｉからなる群から選択された１
種以上の元素、ＱはＢおよびＣからなる群から選択され
た１種以上の元素、Ｒは１種以上の希土類金属元素、Ｍ
はＮｂおよびＭｏからなる群から選択された少なくとも
１種の元素）で表現され、組成比率ｘ、ｙ、ｚ、および
ｍが、それぞれ、 ２≦ｘ≦２８（原子％）、 ８≦ｙ≦３０（原子％）、 ０．１≦ｚ＜１．０（原子％）、および ０≦ｍ≦０．５ を満足する合金の溶湯を急冷し、凝固させることによっ
て急冷凝固合金を作製する工程と、 前記急冷凝固合金から永久磁石を作製する工程と、を包
含する希土類磁石の製造方法。7. The composition formula is (Fe 1-m T m ) 100-xyz Q x R
y M z (T is 1 selected from the group consisting of Co and Ni
At least one kind of element, Q is at least one kind of element selected from the group consisting of B and C, R is at least one kind of rare earth metal element, M
Is represented by at least one element selected from the group consisting of Nb and Mo), and the composition ratios x, y, z, and m are respectively 2 ≦ x ≦ 28 (atomic%), 8 ≦ y ≦ 30 (Atomic%), 0.1 ≦ z <1.0 (atomic%), and a step of producing a rapidly solidified alloy by rapidly cooling and solidifying a molten alloy satisfying 0 ≦ m ≦ 0.5; Producing a permanent magnet from the rapidly solidified alloy.
て、急冷速度を１０2Ｋ／秒以上１０4Ｋ／秒以下の範囲
内にする請求項７に記載の希土類磁石の製造方法。8. The method for producing a rare earth magnet according to claim 7, wherein, in the step of producing the rapidly solidified alloy, the rapid cooling rate is set in a range from 10 2 K / sec to 10 4 K / sec.
て、前記合金の溶湯をストリップキャスト法によって急
冷する請求項８に記載の希土類磁石の製造方法。9. The method for producing a rare earth magnet according to claim 8, wherein in the step of producing the rapidly solidified alloy, the molten metal of the alloy is rapidly cooled by a strip casting method.
後、前記水素を放出させる脆化工程を包含する請求項７
から９のいずれかに記載の希土類磁石の製造方法。10. An embrittlement step of releasing hydrogen after absorbing the hydrogen into the rapidly solidified alloy.
10. The method for producing a rare earth magnet according to any one of items 1 to 9.
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| JP2000207675 | 2000-07-10 | ||
| JP2000-207675 | 2000-07-10 | ||
| JP2001202124A JP3815983B2 (en) | 2000-07-10 | 2001-07-03 | Rare earth magnet and manufacturing method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013191607A (en) * | 2012-03-12 | 2013-09-26 | Nitto Denko Corp | Rare earth permanent magnet and method for producing rare earth permanent magnet |
| JP2013191616A (en) * | 2012-03-12 | 2013-09-26 | Nitto Denko Corp | Rare earth permanent magnet and method of manufacturing the same |
| US9607760B2 (en) | 2012-12-07 | 2017-03-28 | Samsung Electronics Co., Ltd. | Apparatus for rapidly solidifying liquid in magnetic field and anisotropic rare earth permanent magnet |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08269643A (en) * | 1995-03-29 | 1996-10-15 | Sumitomo Special Metals Co Ltd | Cast strip for r-fe-b magnetic alloy and its production |
| JPH1022155A (en) * | 1996-07-05 | 1998-01-23 | Hitachi Metals Ltd | Manufacture of rare-earth permanent magnet and rare-earth permanent magnet |
| JPH10189320A (en) * | 1996-12-25 | 1998-07-21 | Daido Steel Co Ltd | Anisotropic magnet alloy powder, and its manufacture |
| JPH10280010A (en) * | 1997-04-08 | 1998-10-20 | Hitachi Metals Ltd | Production of rare earth permanent magnet alloy powder |
| JPH1197223A (en) * | 1997-09-17 | 1999-04-09 | Hitachi Metals Ltd | R-fe-b sintered permanent magnet |
| JPH11233323A (en) * | 1998-02-13 | 1999-08-27 | Daido Steel Co Ltd | Manufacture of anisotropic magnet material and manufacture of bond magnet using the same |
-
2001
- 2001-07-03 JP JP2001202124A patent/JP3815983B2/en not_active Expired - Lifetime
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08269643A (en) * | 1995-03-29 | 1996-10-15 | Sumitomo Special Metals Co Ltd | Cast strip for r-fe-b magnetic alloy and its production |
| JPH1022155A (en) * | 1996-07-05 | 1998-01-23 | Hitachi Metals Ltd | Manufacture of rare-earth permanent magnet and rare-earth permanent magnet |
| JPH10189320A (en) * | 1996-12-25 | 1998-07-21 | Daido Steel Co Ltd | Anisotropic magnet alloy powder, and its manufacture |
| JPH10280010A (en) * | 1997-04-08 | 1998-10-20 | Hitachi Metals Ltd | Production of rare earth permanent magnet alloy powder |
| JPH1197223A (en) * | 1997-09-17 | 1999-04-09 | Hitachi Metals Ltd | R-fe-b sintered permanent magnet |
| JPH11233323A (en) * | 1998-02-13 | 1999-08-27 | Daido Steel Co Ltd | Manufacture of anisotropic magnet material and manufacture of bond magnet using the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013191607A (en) * | 2012-03-12 | 2013-09-26 | Nitto Denko Corp | Rare earth permanent magnet and method for producing rare earth permanent magnet |
| JP2013191616A (en) * | 2012-03-12 | 2013-09-26 | Nitto Denko Corp | Rare earth permanent magnet and method of manufacturing the same |
| US9607760B2 (en) | 2012-12-07 | 2017-03-28 | Samsung Electronics Co., Ltd. | Apparatus for rapidly solidifying liquid in magnetic field and anisotropic rare earth permanent magnet |
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| Publication number | Publication date |
|---|---|
| JP3815983B2 (en) | 2006-08-30 |
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