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JPH0660367B2 - Method of manufacturing permanent magnet material - Google Patents
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JPH0660367B2 - Method of manufacturing permanent magnet material - Google Patents

Method of manufacturing permanent magnet material

Info

Publication number
JPH0660367B2
JPH0660367B2 JP61015941A JP1594186A JPH0660367B2 JP H0660367 B2 JPH0660367 B2 JP H0660367B2 JP 61015941 A JP61015941 A JP 61015941A JP 1594186 A JP1594186 A JP 1594186A JP H0660367 B2 JPH0660367 B2 JP H0660367B2
Authority
JP
Japan
Prior art keywords
permanent magnet
magnet material
fine powder
alloy
nitride
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
Application number
JP61015941A
Other languages
Japanese (ja)
Other versions
JPS62177147A (en
Inventor
武志 安保
嵩司 古谷
紀夫 吉川
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Daido Steel Co Ltd
Original Assignee
Daido Steel Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Daido Steel Co Ltd filed Critical Daido Steel Co Ltd
Priority to JP61015941A priority Critical patent/JPH0660367B2/en
Publication of JPS62177147A publication Critical patent/JPS62177147A/en
Publication of JPH0660367B2 publication Critical patent/JPH0660367B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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
    • H01F1/0577Alloys 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

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】 (産業上の利用分野) 本発明は、優れた磁気特性を有する窒素含有希土類系永
久磁石材料の製造方法に関する。
Description: TECHNICAL FIELD The present invention relates to a method for producing a nitrogen-containing rare earth-based permanent magnet material having excellent magnetic properties.

(従来の技術) 永久磁石材料は、一般家庭電気製品から精密機器、自動
車部品に至るまで、広い分野にわたって使用されてお
り、電子機器の小形化、高効率化の要求に伴ない、その
磁気特性の向上が益々求められるようになっている、 本発明者等も、永久磁石材料における磁気特性を高める
ために種々研究を行った結果、先にNd−Fe−B系を
代表とする一連の希土類−鉄系永久磁石材料を開発した
(例えば、時開昭60−144907号公報)。
(Prior Art) Permanent magnet materials are used in a wide range of fields from general household electric appliances to precision equipment and automobile parts. Due to the demand for miniaturization and high efficiency of electronic equipment, their magnetic properties As a result of various researches conducted by the present inventors to improve the magnetic properties of permanent magnet materials, a series of rare earths typified by the Nd-Fe-B system has been obtained. -Iron-based permanent magnet materials have been developed (for example, Tokkai Sho 60-144907).

(発明が解決しようとする問題点) しかしながら、より一層優れた磁気特性を有する永久磁
石材料を製造することは、常に求められる課題であっ
て、本発明者等も、前記の希土類−鉄系永久磁石材料に
ついて、更に高い磁気特性を得るべく検討を加えた結
果、窒素を構成成分として含有させたものについては、
永久磁石材料の製造方法について改良を加えることによ
り、所期の目的が達成されることを見出し、本発明を完
成するに至った。
(Problems to be Solved by the Invention) However, producing a permanent magnet material having further excellent magnetic properties is a problem that is always sought, and the present inventors have also found that the rare earth-iron-based permanent As a result of examining magnetic materials to obtain higher magnetic properties, as a result of including nitrogen as a constituent component,
The inventors have found that the intended purpose can be achieved by improving the manufacturing method of the permanent magnet material, and have completed the present invention.

したがって、本発明の目的は、優れた磁気特性を有する
窒素含有希土類−鉄系永久磁石材料を容易に製造する方
法を提供することにある。
Therefore, it is an object of the present invention to provide a method for easily producing a nitrogen-containing rare earth-iron based permanent magnet material having excellent magnetic properties.

(問題点を解決するための手段及び作用) 本発明の前記目的は、一般式 R1−α−β−γ−δFeαβγδ (式中、Rは、Yを含む希土類元素の少なくとも1種を
示し、Mは、Mn、Ni、Co、Ti、Al、Zr、H
f、V、Nb、Si、Ta、Cr、Mo及びWより選択
される少なくとも1種を示し、α、β、γ及びδは、そ
れぞれ 0.60≦α≦0.85 0.01≦β≦0.20 0.0001≦γ≦0.15 0<δ≦0.20 の値を示す。) で示される永久磁石材料の製造方法において、母合金の
微粉末に、Fe、Mn、Ni、Co、Ti、Zr、H
f、V、Nb、Si、Ta、Cr、Mo及びWより選択
される1種又はそれ以上の元素の窒化物の微粉末を添加
して成形し、燒結することによって達成される。
(Means and Actions for Solving Problems) The object of the present invention is to provide a compound represented by the general formula: R 1-α-β-γ-δ Fe α B β N γ M δ (wherein R is a rare earth element containing Y). At least one of the elements is shown, M is Mn, Ni, Co, Ti, Al, Zr, H
At least one selected from f, V, Nb, Si, Ta, Cr, Mo and W is shown, and α, β, γ and δ are each 0.60 ≦ α ≦ 0.85 0.01 ≦ β ≦ The value of 0.20 0.0001 ≦ γ ≦ 0.15 0 <δ ≦ 0.20 is shown. ) In the method for producing a permanent magnet material represented by, Fe, Mn, Ni, Co, Ti, Zr, and H are added to the fine powder of the mother alloy.
It is achieved by adding a fine powder of a nitride of one or more elements selected from f, V, Nb, Si, Ta, Cr, Mo and W, shaping and sintering.

本発明において、母合金としては、R−Fe系、R−F
e−B系、R−Fe−M系及びR−Fe−B−M系のも
のが用いられる。ここで、R及びMは前記したものを意
味する。これら母合金は平均粒径数ミクロン、例えば5
μ前後に微粉砕して用いられる。
In the present invention, as the master alloy, R-Fe system, R-F
The e-B type, the R-Fe-M type, and the R-Fe-B-M type are used. Here, R and M have the same meanings as described above. These master alloys have an average particle size of a few microns, eg 5
It is used by finely pulverizing it to around μ.

一方、母合金に添加される窒化物としては、Fe、M
n、Ni、Co、Ti、Zr、Hf、V、Nb、Si、
Ta、Cr、Mo及びWの窒化物があげられ、これら
は、2種又はそれ遺贈を併用してもよい。また、これら
の窒化物と共に、AlNまたはBNを併用することも可
能である。
On the other hand, as the nitride added to the mother alloy, Fe, M
n, Ni, Co, Ti, Zr, Hf, V, Nb, Si,
There are nitrides of Ta, Cr, Mo and W, and two or more of these may be used in combination. It is also possible to use AlN or BN together with these nitrides.

これら窒化物は、その平均粒径が100μより大きくな
ると母合金に均一に拡散し難くなるので、平均粒径10
0μ以下に微粉砕して用いられる。
If the average grain size of these nitrides is larger than 100 μ, it is difficult to uniformly diffuse into the master alloy.
It is used after finely pulverized to 0 μ or less.

本発明によれば、母合金に対するこれら窒化物の添加量
を制御することによって、最終的に得られる永久磁石材
料の組成が所定の範囲になるよう調節することができ
る。したがって、所定の組成を有する永久磁石材料を容
易に得ることができる。
According to the present invention, the composition of the finally obtained permanent magnet material can be adjusted within a predetermined range by controlling the addition amount of these nitrides to the mother alloy. Therefore, a permanent magnet material having a predetermined composition can be easily obtained.

本発明において、母合金の微粉末に前記の窒化物の微粉
末を添加した後、混合物は、例えばプレス成形機などに
よって成形される。成形は磁場中で行うのが好ましい。
成形により得られた成形体は、次いで、例えばアルゴン
雰囲気中で燒結させ、永久磁石材料が得られる。
In the present invention, after the above-mentioned nitride fine powder is added to the master alloy fine powder, the mixture is molded by, for example, a press molding machine. Molding is preferably carried out in a magnetic field.
The molded body obtained by molding is then sintered, for example, in an argon atmosphere to obtain a permanent magnet material.

本発明における前記一般式中Rで示されるYを含む希土
類元素としては、Sc、Y、La、 Ce、Pr、N
d、Pm、Sm、Eu、Gd、Tb、Dy、Ho、E
r、Tm、YbおよびLuがあげられ、これ等のものか
ら1種以上が選択される。本発明における磁石材料にお
いて、Feの量が多すぎると、残留磁束密度は向上する
が、保磁力が減少するため、優れた最大エネルギ積が得
難くなり、又少なすぎると残留磁束密度が低くなり最大
エネルギ積が減少するので、Feは60〜85原子%の
範囲に設定される。又B及びNは、希土類−鉄系永久磁
石のキユリー点を常温から上昇させたり或いは保磁力を
向上させたりする作用があるが、その量が多すぎると保
磁力或いは残留磁束密度が減少するので、それぞれ1〜
20原子%及び0.01〜15原子%の範囲に設定され
る。本発明においては、前記元素Mを添加することによ
り、保磁力の向上、及び残留磁束密度の温度係数の向上
に効果がある。しかし、あまりその量が多いと磁気特性
が劣化するので、20原子%以下に設定される。
Examples of the rare earth element containing Y represented by R in the general formula of the present invention include Sc, Y, La, Ce, Pr and N.
d, Pm, Sm, Eu, Gd, Tb, Dy, Ho, E
r, Tm, Yb and Lu are mentioned, and one or more kinds are selected from these. In the magnet material of the present invention, when the amount of Fe is too large, the residual magnetic flux density is improved, but the coercive force is reduced, so that it becomes difficult to obtain an excellent maximum energy product, and when it is too small, the residual magnetic flux density becomes low. Since the maximum energy product decreases, Fe is set in the range of 60 to 85 atomic%. Further, B and N have an action of raising the Curie point of the rare earth-iron-based permanent magnet from room temperature or improving the coercive force, but if the amount is too large, the coercive force or the residual magnetic flux density decreases. , Each 1
It is set in the range of 20 atomic% and 0.01 to 15 atomic%. In the present invention, the addition of the element M is effective in improving the coercive force and the temperature coefficient of the residual magnetic flux density. However, if the amount is too large, the magnetic properties deteriorate, so it is set to 20 atomic% or less.

(実施例) 次に、本発明を実施例によって説明する。(Examples) Next, the present invention will be described by examples.

実施例1. Nd15原子%−B8原子%−Fe残部なる組成の合金
を溶製し、ジェットミルによって平均粒径4.0μとな
るように微粉砕した。その微粉末に、TiN、SiN、
MoN、VN、MnN又はCrNの微粉末、又はZrN
とWNとBNの混合微粉末(平均粒径1〜5μ)を添加
した。得られた混合物を磁場中でプレス成形し、アルゴ
ン雰囲気中で1100℃の温度で1時間燒結し、その後
50℃/hrの冷却速度で、室温まで冷却した。
Example 1. An alloy having a composition of Nd 15 atomic% -B8 atomic% -Fe balance was melted and finely pulverized by a jet mill so as to have an average particle diameter of 4.0 µ. TiN, SiN,
Fine powder of MoN, VN, MnN or CrN, or ZrN
And fine powder of WN and BN mixed (average particle size 1 to 5 μm) were added. The obtained mixture was press-molded in a magnetic field, sintered in an argon atmosphere at a temperature of 1100 ° C. for 1 hour, and then cooled to room temperature at a cooling rate of 50 ° C./hr.

比較のために、合金の溶製時に上記の窒化物の構成成分
を添加したものを、同様に微粉砕して平均粒径4.0μ
の微粉末を得た。このものを同様にプレス成形し、燒結
処理をして比較試料を得た。
For comparison, an alloy obtained by adding the above-mentioned constituents of the nitride during melting of the alloy was similarly finely pulverized to have an average particle diameter of 4.0 μm.
Of fine powder was obtained. This product was similarly press-molded and sintered to obtain a comparative sample.

これらのものについて、残留磁束密度(Br)及び保磁
力(IHc)を調査したところ第1表の結果が得られ
た。
When the residual magnetic flux density (Br) and the coercive force (IHc) of these materials were investigated, the results shown in Table 1 were obtained.

実施例2. Nd16原子%−B8原子%−M1原子%−Fe残部
(M:Al、Mo、V)なる組成の合金を溶製し、ジェ
ットミルによって平均粒径4.0μとなるように微粉砕
した。その微粉末に、MoN微粉末又はVNとAlNの
混合微粉末を添加した。得られた混合物を磁場中でプレ
ス成形し、アルゴン雰囲気中で1100℃の温度で1時
間燒結し、その後50℃/hrの冷却速度で、室温まで
冷却した。 比較のために、合金の溶製時に、上記の窒
化物の構成成分を添加したものを同様に微粉砕して平均
粒径4.0μの微粉末を得た。このものを同様にプレス
成形し、燒結処理をして比較試料を得た。 これらのも
のについて、残留磁束密度(Br)及び保磁力(IH
c)を調査したところ第2表の結果が得られた。
Example 2. An alloy having a composition of Nd 16 atomic% -B8 atomic% -M1 atomic% -Fe balance (M: Al, Mo, V) was melted and finely pulverized by a jet mill so that the average particle diameter was 4.0 µ. MoN fine powder or a mixed fine powder of VN and AlN was added to the fine powder. The obtained mixture was press-molded in a magnetic field, sintered in an argon atmosphere at a temperature of 1100 ° C. for 1 hour, and then cooled to room temperature at a cooling rate of 50 ° C./hr. For the purpose of comparison, when the alloy was melted, the above-mentioned nitride constituents were similarly pulverized to obtain fine powder having an average particle size of 4.0 μ. This product was similarly press-molded and sintered to obtain a comparative sample. For these, the residual magnetic flux density (Br) and coercive force (IH
When c) was investigated, the results shown in Table 2 were obtained.

実施例3. Nd15原子%−B8原子%−Co12原子%−Fe残
部なる組成の合金を溶製し、ジェットミルによって平均
粒径4.0μとなるように微粉砕した。その微粉末に、
TiNの微粉末を添加した。得られた混合物を磁場中で
プレス成形し、アルゴン雰囲気中で1100℃の温度で
1時間燒結し、その後50℃/hrの冷却速度で、室温
まで冷却した。
Example 3. An alloy having a composition of Nd 15 atomic% -B8 atomic% -Co 12 atomic% -Fe balance was melted and finely pulverized by a jet mill so that the average particle diameter was 4.0 µ. To the fine powder,
A fine powder of TiN was added. The obtained mixture was press-molded in a magnetic field, sintered in an argon atmosphere at a temperature of 1100 ° C. for 1 hour, and then cooled to room temperature at a cooling rate of 50 ° C./hr.

比較のために、合金の溶製時に、上記の窒化物の構成成
分を添加したものを同様に微粉砕して平均粒径4.0μ
の微粉末を得た。このものを同様にプレス成形し、燒結
処理をして比較試料を得た。
For comparison, an alloy having the above-mentioned nitride constituents added thereto was finely pulverized at the time of melting the alloy to obtain an average particle diameter of 4.0 μm.
Of fine powder was obtained. This product was similarly press-molded and sintered to obtain a comparative sample.

これらのものについて、残留磁束密度(Br)及び保磁
力(IHc)を調査したところ第3表の結果が得られ
た。
When the residual magnetic flux density (Br) and the coercive force (IHc) of these materials were investigated, the results shown in Table 3 were obtained.

実施例4. 実施例1におけると同様にして母合金に窒化物を添加
し、永久磁石を製造した。永久磁石の組成、母合金の組
成、添加した窒化物、燒結密度、残留磁束密度及び保磁
力を比較試料と共に第4表に示す。
Example 4. A nitride was added to the mother alloy in the same manner as in Example 1 to manufacture a permanent magnet. Table 4 shows the composition of the permanent magnet, the composition of the mother alloy, the added nitride, the sintered density, the residual magnetic flux density, and the coercive force together with the comparative sample.

(発明の効果) 本発明においては、母合金の微粉末に窒化物の微粉末を
添加し、成形尾、燒結して希土類系永久磁石材料を製造
するから、磁石材料組成中に所定量の窒素を容易に含有
させることができるとともに、窒化物の添加量を制御す
ることによって、所望の合金組成を有する永久磁石材料
を容易に得ることができる。又前記第1表ないし第4表
に示すごとく、得られた希土類永久磁石材料は、その燒
結密度が上昇し、又、残留粒磁束密度及び保磁力が上昇
するとい効果を奏する。
(Effects of the Invention) In the present invention, a fine powder of a nitride is added to a fine powder of a mother alloy, and a rare earth-based permanent magnet material is manufactured by sintering and sintering, so that a predetermined amount of nitrogen is contained in the magnet material composition. Can be easily contained, and a permanent magnet material having a desired alloy composition can be easily obtained by controlling the addition amount of nitride. Further, as shown in Tables 1 to 4, the obtained rare earth permanent magnet materials have the effect of increasing the sintered density and the residual grain magnetic flux density and the coercive force.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】一般式 R1−α−β−γ−δFeαβγδ (式中、Rは、Yを含む希土類元素の少なくとも1種を
示し、Mは、Mn、Ni、Co、Ti、Al、Zr、H
f、V、Nb、Si、Ta、Cr、Mo及びWより選択
される少なくとも1種を示し、α、β、γ及びδは、そ
れぞれ 0.60≦α≦0.85 0.01≦β≦0.20 0.0001≦γ≦0.15 0<δ≦0.20 の値を示す。) で示される組成を有する永久磁石材料の製造方法におい
て、母合金の微粉末に、Fe、Mn、Ni、Co、T
i、Zr、Hf、V、Nb、Si、Ta、Cr、Mo及
びWより選択される1種又はそれ以上の元素の窒化物の
微粉末を添加して成形し、燒結することを特徴とする永
久磁石材料の製造方法。
1. A general formula R 1-α-β-γ-δ Fe α B β N γ M δ (wherein R represents at least one rare earth element including Y, and M represents Mn and Ni. , Co, Ti, Al, Zr, H
At least one selected from f, V, Nb, Si, Ta, Cr, Mo and W is shown, and α, β, γ and δ are each 0.60 ≦ α ≦ 0.85 0.01 ≦ β ≦ The value of 0.20 0.0001 ≦ γ ≦ 0.15 0 <δ ≦ 0.20 is shown. ) In the method for producing a permanent magnet material having a composition represented by the following formula, Fe, Mn, Ni, Co, T
Characterized by adding a fine powder of a nitride of one or more elements selected from i, Zr, Hf, V, Nb, Si, Ta, Cr, Mo and W, followed by molding and sintering. Manufacturing method of permanent magnet material.
【請求項2】添加する窒化物の微粉末が平均粒径100
μ以下であることを特徴とする特許請求の範囲第1項に
記載の永久磁石材料の製造方法。
2. The fine powder of nitride to be added has an average particle size of 100.
The method for producing a permanent magnet material according to claim 1, wherein the value is μ or less.
JP61015941A 1986-01-29 1986-01-29 Method of manufacturing permanent magnet material Expired - Lifetime JPH0660367B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP61015941A JPH0660367B2 (en) 1986-01-29 1986-01-29 Method of manufacturing permanent magnet material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61015941A JPH0660367B2 (en) 1986-01-29 1986-01-29 Method of manufacturing permanent magnet material

Publications (2)

Publication Number Publication Date
JPS62177147A JPS62177147A (en) 1987-08-04
JPH0660367B2 true JPH0660367B2 (en) 1994-08-10

Family

ID=11902783

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Publication number Priority date Publication date Assignee Title
US5186766A (en) * 1988-09-14 1993-02-16 Asahi Kasei Kogyo Kabushiki Kaisha Magnetic materials containing rare earth element iron nitrogen and hydrogen
JP2648634B2 (en) * 1990-05-10 1997-09-03 ハイウンチンシュー グーフウンユーシェンコンシー Manufacturing method of magnet
JPH04142703A (en) * 1990-09-25 1992-05-15 Natl Sci Council Rare earth element-transition metal-nitrogen-boron permanent magnet alloy and its manufacturing method
US5858123A (en) * 1995-07-12 1999-01-12 Hitachi Metals, Ltd. Rare earth permanent magnet and method for producing the same
CN111312507A (en) * 2020-03-04 2020-06-19 安徽大地熊新材料股份有限公司 Method for improving intensity of rare earth-iron-boron permanent magnet

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5665954A (en) * 1979-11-02 1981-06-04 Seiko Instr & Electronics Ltd Rare earth element magnet and its manufacture
JPH0669003B2 (en) * 1984-05-31 1994-08-31 大同特殊鋼株式会社 Powder for permanent magnet and method for manufacturing permanent magnet
JPS627831A (en) * 1985-07-04 1987-01-14 Sumitomo Special Metals Co Ltd Manufacture of permanent magnet material
JPS62134908A (en) * 1985-12-09 1987-06-18 Hitachi Metals Ltd R-b-fe system sintered magnet and manufacture thereof

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