JP2000223305A - Rare-earth r-fe-co-b magnetic powder, its manufacturing method, and bonded magnet made of the powder - Google Patents

Rare-earth r-fe-co-b magnetic powder, its manufacturing method, and bonded magnet made of the powder

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Publication number
JP2000223305A
JP2000223305A JP11024066A JP2406699A JP2000223305A JP 2000223305 A JP2000223305 A JP 2000223305A JP 11024066 A JP11024066 A JP 11024066A JP 2406699 A JP2406699 A JP 2406699A JP 2000223305 A JP2000223305 A JP 2000223305A
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Japan
Prior art keywords
magnet powder
powder
diameter
recrystallized grains
recrystallized
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JP11024066A
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JP3427765B2 (en
Inventor
Koichiro Morimoto
耕一郎 森本
Kazunori Igarashi
和則 五十嵐
Yoshinari Ishii
義成 石井
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Mitsubishi Materials Corp
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Mitsubishi Materials Corp
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    • 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

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  • 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)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide R-Fe-Co-B magnetic powder having superior magnetic characteristics. SOLUTION: This magnetic powder contains 10-20 atomic percent of R, 0.1-50 atomic percent of cobalt(Co), 3-20 atomic percent of boron(B), 0.001-5.0 atomic percent of one or more elements selected from among gallium(Ga), zirconium(Zr), and hafnium(Hf), 0.1-2.0 atomic percent of one or more elements and selected from among aluminum(Al), vanadium(V), and silicon(Si) and as necessary, iron, and unavoidable impurities. Recrystallized grains having average diameters of 0.05-3 μm adjoin to each other and gather, and such recrystallized grains that the longest diameter divided by the shortest diameter is greater than 2 make up of not less than 50 volume percent of the all recrystallized grains. The ratio of the longest diameter X to the shortest diameter y (x/y) of each grain is from 2 to 10, and the shortest diameter y is from 60 to 150 μm. The direction of easy magnetization in this magnetic powder is the same as the shortest-diameter direction of the grains.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】この発明は、優れた磁気的異
方性を有するＲ（但し、Ｒは、Ｙを含む希土類元素のう
ち少くとも１種を示す），Ｆｅ，Ｃｏ，およびＢを主成
分とするＲ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末およびその製造
方法並びにこの粉末を用いたボンド磁石に関するもので
ある。BACKGROUND OF THE INVENTION The present invention mainly relates to R (having at least one kind of rare earth element including Y), Fe, Co and B having excellent magnetic anisotropy. The present invention relates to an R-Fe-Co-B-based magnet powder as a component, a method for producing the same, and a bonded magnet using the powder.

【０００２】[0002]

【従来の技術】Ｒ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末は高い磁
気特性および比較的安定な温度特性を有するところか
ら、これを樹脂結合してボンド磁石を作製している。こ
のボンド磁石は、寸法精度が高いこと、薄肉で複雑形状
の磁石を容易に製造できること、他の部品との一体成形
が可能であることなどの特徴を有することから、ＯＡ、
ＦＡ機器などの小型モーターなど各種部品として広く使
用されている。2. Description of the Related Art Since R-Fe-Co-B magnet powder has high magnetic characteristics and relatively stable temperature characteristics, it is bonded to a resin to form a bonded magnet. This bonded magnet has features such as high dimensional accuracy, easy production of a thin and complicated-shaped magnet, and the ability to be integrally molded with other parts.
Widely used as various parts such as small motors for FA equipment.

【０００３】前記Ｒ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末を製造
する方法の一つとして、水素化・脱水素処理する方法
（一般に、ＨＤＤＲ法と呼ばれている）が知られてお
り、この方法は、Ｒ−Ｆｅ−Ｃｏ−Ｂ系鋳造合金または
これを粉砕して得られた粗粉末を１０Ｔｏｒｒ以上の水
素ガス雰囲気中または水素ガス分圧：１０Ｔｏｒｒ以上
の水素ガスと不活性ガスの混合ガス雰囲気中で温度：５
００〜１０００℃に保持して鋳造合金またはその合金の
粗粉末に水素を吸蔵させた後、水素ガス圧力：１×１０
-1Ｔｏｒｒ以下の真空雰囲気または水素ガス分圧：１×
１０-1Ｔｏｒｒ以下の不活性ガス雰囲気になるまで温
度：５００〜１０００℃で脱水素処理したのち急却し、
ついで粉砕することにより製造するものである。[0003] As one of the methods for producing the R-Fe-Co-B magnet powder, a method of hydrogenation and dehydrogenation (generally called HDDR method) is known. Is an R-Fe-Co-B based cast alloy or a coarse powder obtained by pulverizing the same in a hydrogen gas atmosphere of 10 Torr or more, or a mixed gas atmosphere of hydrogen gas and hydrogen gas having a hydrogen gas partial pressure of 10 Torr or more. Inside temperature: 5
After holding the hydrogen in the cast alloy or the coarse powder of the alloy while maintaining the temperature at 00 to 1000 ° C., the hydrogen gas pressure is 1 × 10 5
-1 Torr or less vacuum atmosphere or hydrogen gas partial pressure: 1 ×
After dehydrogenation treatment at a temperature of 500 to 1000 ° C. until an inert gas atmosphere of 10 −1 Torr or less is obtained, urgently proceed.
Then, it is manufactured by grinding.

【０００４】この方法で得られたＲ−Ｆｅ−Ｃｏ−Ｂ系
磁石粉末は、正方晶構造をとるＲ2（Ｆｅ，Ｃｏ）14Ｂ
型金属間化合物相を主相とする再結晶粒が相互に隣接し
て集合した再結晶粒集合組織を有し、この再結晶粒集合
組織を構成する再結晶粒の平均粒径は０．０５〜３μｍ
でかつ再結晶粒の最短径ａと最長径ｂの比（ｂ／ａ）の
値が２未満である再結晶粒は全再結晶粒の５０容量％以
上を占め、このＲ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末の望まし
い組成は、原子百分率で、Ｒ：１０〜２０％、Ｃｏ：
０．１〜５０％、Ｂ：３〜２０％、Ｇａ，ＺｒおよびＨ
ｆのうち１種または２種以上の合計：０．００１〜５．
０％を含有し、さらに、Ａｌ，ＶおよびＳｉのうち１種
または２種以上の合計：０．０１〜２．０％を含有し、
残りがＦｅおよび不可避不純物からなる組成であること
も知られている。The R-Fe-Co-B-based magnet powder obtained by this method has a tetragonal structure of R 2 (Fe, Co) 14 B.
A recrystallized grain having a main phase of the intermetallic compound phase as a main phase has a recrystallized grain texture in which the recrystallized grains constitute the recrystallized grain texture with an average grain size of 0.05. ~ 3 μm
And the ratio of the shortest diameter a to the longest diameter b of the recrystallized grains (b / a) is less than 2, accounts for 50% by volume or more of all recrystallized grains. A desirable composition of the B-based magnet powder is as follows: R: 10 to 20%, Co:
0.1-50%, B: 3-20%, Ga, Zr and H
f or a total of one or more of f: 0.001 to 5.
0%, and further contains one or more of Al, V and Si: 0.01 to 2.0%,
It is also known that the balance is composed of Fe and unavoidable impurities.

【０００５】これらＲ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末は、
樹脂と混合した後、圧縮成形、射出成形、押し出し成
形、ロール圧延などの方法により所定形状に成形し、ボ
ンド磁石を製造することができる。この成形の際に、外
部より磁界を加えない製造法では、磁石粉末粒子の磁化
容易軸が無秩序に分布し、磁石のいずれの方向において
も磁気特性の等しい等方性ボンド磁石が得られる。成形
時に外部磁界を加えると、磁石粉末粒子の磁化容易軸が
磁界方向に揃い、その方向が他の方向よりも高い磁気特
性を示す異方性ボンド磁石が得られる。[0005] These R-Fe-Co-B magnet powders are:
After being mixed with the resin, the mixture is molded into a predetermined shape by a method such as compression molding, injection molding, extrusion molding, or roll rolling, so that a bonded magnet can be manufactured. In the manufacturing method in which a magnetic field is not externally applied during the molding, an easy axis of magnetization of the magnet powder particles is randomly distributed, and an isotropic bonded magnet having the same magnetic properties in any direction of the magnet can be obtained. When an external magnetic field is applied at the time of molding, an easy axis of magnetization of the magnet powder particles is aligned with the direction of the magnetic field, and an anisotropic bonded magnet in which the direction has higher magnetic characteristics than other directions is obtained.

【０００６】磁界なしで製造される生産性が高く製造コ
ストの安い等方性ボンド磁石は残留磁束密度Ｂｒおよび
磁気エネルギー積（ＢＨ）ｍａｘが低いところから、こ
れらを一層向上させることが求められている。また磁界
中成形して得られる異方性ボンド磁石に対してもより高
特性が求められており、特に圧縮方向と平行に配向磁界
を印加して製造される（以下、この圧縮方向と平行に配
向磁界を印加して成形することを平行磁界中成形と云
う）異方性ボンド磁石、例えば、円柱や円筒の形状を持
ち、その軸方向が配向方向である磁石は、Ｒ−Ｆｅ−Ｃ
ｏ−Ｂ系磁石粉末の外部磁界方向への整列（配向）度を
改善して磁石の残留磁束密度Ｂｒおよび磁気エネルギー
積（ＢＨ）ｍａｘを向上させる余地が大きく残されてい
る。なぜならば、平行磁界中成形では、外部磁界をかけ
ることにより配向した粉末粒子の粒鎖が形成されても、
加圧されることにより粉末粒子の粒鎖が座屈し、配向が
乱れるためである。この平行磁界中成形における磁石粉
末の整列度を改善する方法として、Ｒ−Ｆｅ−Ｃｏ−Ｂ
系鋳造合金に熱間塑性加工を施してＲ2 （Ｆｅ，Ｃｏ）
14Ｂ型金属間化合物相のｃ軸が配向した合金を製造し、
これに水素化・脱水素処理を施すことにより磁石粉末粒
子内のｃ軸配向をより先鋭化させた磁石粉末を製造し、
この磁石粉末を使用する方法が知られている（特開平４
−１８８８０５号公報参照）。An isotropic bonded magnet manufactured without a magnetic field and having high productivity and low manufacturing cost has low residual magnetic flux density Br and magnetic energy product (BH) max. I have. Higher properties are also required for anisotropic bonded magnets obtained by molding in a magnetic field. In particular, the anisotropic bonded magnets are manufactured by applying an orientation magnetic field in parallel to the compression direction. Forming by applying an orientation magnetic field is referred to as molding in a parallel magnetic field.) An anisotropic bonded magnet, for example, a magnet having the shape of a cylinder or a cylinder, and whose axial direction is the orientation direction, is R-Fe-C.
There is much room for improving the degree of alignment (orientation) of the oB-based magnet powder in the direction of the external magnetic field to improve the residual magnetic flux density Br and the magnetic energy product (BH) max of the magnet. Because, in the molding in the parallel magnetic field, even if the grain chains of the oriented powder particles are formed by applying the external magnetic field,
This is because the pressing causes the chain of the powder particles to buckle and the orientation to be disturbed. As a method for improving the degree of alignment of the magnet powder in the molding in a parallel magnetic field, R-Fe-Co-B
R 2 is subjected to hot plastic working system cast alloy (Fe, Co)
14 An alloy in which the c-axis of the B-type intermetallic compound phase is oriented,
This is subjected to a hydrogenation / dehydrogenation treatment to produce a magnet powder having a sharper c-axis orientation in the magnet powder particles,
A method using this magnet powder is known (Japanese Unexamined Patent Application Publication No.
-188805).

【０００７】[0007]

【発明が解決しようとする課題】しかし、前記の方法で
製造した磁石粉末は、無磁界中で成形したボンド磁石の
Ｂｒおよび（ＢＨ）ｍａｘを向上させる効果は全く無
く、また平行磁界中成形における粉末粒子の配向の乱れ
を防止する効果もまだ小さい。さらに、前記の方法で磁
石粉末を製造するには、Ｒ−Ｆｅ−Ｃｏ−Ｂ系鋳造合金
を素地中に第二相として存在するＲ−ｒｉｃｈ相が融液
化する温度域で塑性加工しなければならず（このＲ−Ｆ
ｅ−Ｃｏ−Ｂ系鋳造合金はＲ−ｒｉｃｈ相が融液化する
温度域以下では軟化せず、Ｒ2 （Ｆｅ，Ｃｏ）14Ｂ型金
属間化合物相にｃ軸配向を生じせしめる高い加工度まで
塑性加工を行うことができないからである）、かかる温
度域でＲ−Ｆｅ−Ｃｏ−Ｂ系鋳造合金に熱間塑性加工を
施すと、Ｒ2 （Ｆｅ，Ｃｏ）14Ｂ型金属間化合物相の粒
界にＲ−ｒｉｃｈ相が不均一に分布した金属組織が形成
され、かかる金属組織を有する磁石粉末は減磁曲線の角
型性が劣化し、その結果、十分な磁気特性が得られない
ので好ましくない。However, the magnet powder produced by the above method has no effect of improving the Br and (BH) max of the bonded magnet formed in the absence of a magnetic field. The effect of preventing the disorder of the orientation of the powder particles is still small. Further, in order to produce the magnet powder by the above method, the R-Fe-Co-B-based cast alloy must be plastically worked in a temperature range in which the R-rich phase present as the second phase in the base material melts. Not (this R-F
The e-Co-B-based cast alloy does not soften below the temperature range where the R-rich phase melts, and has a high workability that causes c-axis orientation in the R 2 (Fe, Co) 14 B type intermetallic compound phase. If the R-Fe-Co-B cast alloy is subjected to hot plastic working in such a temperature range, the R 2 (Fe, Co) 14 B type intermetallic compound phase cannot be formed. Since a metal structure in which the R-rich phase is non-uniformly distributed is formed at the grain boundaries, and the magnet powder having such a metal structure deteriorates the squareness of the demagnetization curve, and as a result, sufficient magnetic characteristics cannot be obtained. Not preferred.

【０００８】[0008]

【課題を解決するための手段】そこで、本発明者等は、
無磁界中成形および平行磁界中成形によるボンド磁石の
磁気特性を向上させるための磁石粉末を得るべく研究を
行った結果、Ｒ：１０〜２０％、Ｃｏ：０．１〜５０
％、Ｂ：３〜２０％を含有し、さらにＧａ，Ｚｒおよび
Ｈｆのうち１種または２種以上の合計量：０．００１〜
５．０％を含有し、さらに必要に応じてＡｌ，Ｖおよび
Ｓｉのうち１種または２種以上の合計量：０．０１〜
２．０％を含有し、残りがＦｅおよび不可避不純物から
なる組成を有するＲ−Ｆｅ−Ｃｏ−Ｂ系合金溶湯を鋳造
して板厚：６０〜１５０μｍの範囲内のフィルム状の鋳
造体を作製すると、急冷されてＲ2 （Ｆｅ，Ｃｏ） 14Ｂ
型金属間化合物相のｃ軸が板厚方向に鋭く配向したＲ−
ｒｉｃｈ相が均一に分布した金属組織を有するフィルム
状の鋳造体が得られ、このフィルム状の鋳造体に公知の
ＨＤＤＲ処理を施すと、ｃ軸配向が維持されながらＲ2
（Ｆｅ，Ｃｏ）14Ｂ型金属間化合物相を主相とする平均
粒径：０．０５〜３μｍでかつ再結晶粒の最短径ａと最
長径ｂの比（ｂ／ａ）の値が２未満である再結晶粒が相
互に隣接して集合した再結晶粒集合組織が得られ、この
再結晶粒集合組織を有するフィルム状の鋳造体を粉砕し
てフィルム状の鋳造体の厚みが粉末粒子の厚さの最短径
ｙ：６０〜１５０μｍとなり、粉末粒子の最長径ｘと最
短径ｙの比（ｘ／ｙ）が２〜１０でかつ粉末粒子の前記
最短径ｙ方向にｃ軸配向した偏平状粉末が得られること
を見出だした。そしてこの偏平状磁石粉末を用いた無磁
界中成形によるボンド磁石は、成形加圧時に粉末粒子が
その厚み方向、すなわち磁化容易方向が加圧方向と平行
に機械的に整列するため、その方向のＢｒおよび（Ｂ
Ｈ）ｍａｘが従来粉末の無磁界中成形によるボンド磁石
にそれらに比べて著しく向上するという研究結果が得ら
れたのである。また平行磁界中成形によるボンド磁石に
おいても、前記した磁石粉末の偏平形状に起因する機械
的整列の効果により、加圧時の配向の乱れが小さくな
り、従来粉末の平行磁界中成形によるボンド磁石に比べ
てＢｒおよび（ＢＨ）ｍａｘが増大するとの結果を得た
のである。Means for Solving the Problems Accordingly, the present inventors have
Bonded magnet by molding in no magnetic field and molding in parallel magnetic field
Research to obtain magnet powder to improve magnetic properties
As a result, R: 10 to 20%, Co: 0.1 to 50
%, B: 3 to 20%, Ga, Zr and
The total amount of one or more of Hf: 0.001 to
5.0%, and optionally, Al, V and
Total amount of one or more of Si: 0.01 to
2.0%, with the balance being Fe and unavoidable impurities
Of molten R-Fe-Co-B alloy having the following composition
And the thickness of the film: 60 to 150 μm
When the structure is made, it is quenched and RTwo(Fe, Co) 14B
R-type in which the c-axis of the intermetallic compound phase is sharply oriented in the thickness direction
Film having metal structure in which rich phase is uniformly distributed
A cast in the shape of a film is obtained, and a known
When the HDDR process is performed, the R axis is maintained while maintaining the c-axis orientation.Two
(Fe, Co)14Average with B-type intermetallic compound phase as main phase
Particle size: 0.05-3 μm and the shortest diameter a of recrystallized grains
Recrystallized grains having a ratio (b / a) of major axis b of less than 2 are phases
A recrystallized grain texture aggregated adjacent to each other is obtained.
Pulverizing a film-shaped casting having a recrystallized grain texture
The thickness of the cast film is the shortest diameter of the thickness of the powder particles.
y: 60 to 150 μm, and the longest diameter x of the powder particles
The ratio (x / y) of the minor axis y is 2 to 10 and the powder particles
Obtain a flat powder with c-axis orientation in the shortest diameter y direction
Was found. And the non-magnetic using this flat magnet powder
In the bonded magnets produced by Kokusai molding, powder particles are
Its thickness direction, that is, the easy magnetization direction is parallel to the pressing direction
In order to mechanically align with Br and (B
H) A bonded magnet made by molding a conventional powder in a magnetic field-free condition
The research results showed that
It was. Also for bonded magnets formed in a parallel magnetic field
Also, the machine caused by the flat shape of the magnet powder described above
Alignment effect reduces the orientation disturbance during pressurization.
Compared to conventional bonded magnets formed by powder molding in a parallel magnetic field.
Obtained that Br and (BH) max increased
It is.

【０００９】この発明はかかる研究結果にもとづいてな
されたものであって、（１）ＲとＦｅとＣｏとＢを主成
分とするＲ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末であって、この
磁石粉末は、原子百分率で、Ｒ：１０〜２０％、Ｃｏ：
０．１〜５０％、Ｂ：３〜２０％、Ｇａ，ＺｒおよびＨ
ｆのうち１種または２種以上の合計：０．００１〜５．
０％を含有し、残りがＦｅおよび不可避不純物からなる
組成を有し、さらにこの磁石粉末は、正方晶構造をとる
Ｒ2 （Ｆｅ，Ｃｏ）14Ｂ型金属間化合物相を主相とする
再結晶粒が相互に隣接して集合した再結晶粒集合組織を
有し、この再結晶粒集合組織を構成する再結晶粒の平均
粒径は０．０５〜３μｍでかつ再結晶粒の最短径ａと最
長径ｂの比（ｂ／ａ）の値が２未満である再結晶粒が全
再結晶粒の５０容量％以上を占め、さらにこの磁石粉末
は、粉末粒子の最長径ｘと最短径ｙの比（ｘ／ｙ）が２
〜１０でかつ前記最短径ｙは６０〜１５０μｍであり、
磁化容易方向が粉末の最短径方向に揃っているＲ−Ｆｅ
−Ｃｏ−Ｂ系磁石粉末、（２）ＲとＦｅとＣｏとＢを主
成分とするＲ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末であって、こ
の磁石粉末は、原子百分率で、Ｒ：１０〜２０％、Ｃ
ｏ：０．１〜５０％、Ｂ：３〜２０％、Ｇａ，Ｚｒおよ
びＨｆのうち１種または２種以上の合計：０．上記Ｒと
ＦｅとＣｏとＢを主成分とするＲ−Ｆｅ−Ｃｏ−Ｂ系磁
石粉末は、原子百分率で、Ｒ：１０〜２０％、Ｃｏ：
０．１〜５０％、Ｂ：３〜２０％、Ｇａ，ＺｒおよびＨ
ｆのうち１種または２種以上の合計：０．００１〜５．
０％を含有し、さらに、Ａｌ，ＶおよびＳｉのうち１種
または２種以上の合計：０．０１〜２．０％を含有し、
残りがＦｅおよび不可避不純物からなる組成を有し、さ
らにこの磁石粉末は、正方晶構造をとるＲ2 （Ｆｅ，Ｃ
ｏ）14Ｂ型金属間化合物相を主相とする再結晶粒が相互
に隣接して集合した再結晶粒集合組織を有し、この再結
晶粒集合組織を構成する再結晶粒の平均粒径は０．０５
〜３μｍでかつ再結晶粒の最短径ａと最長径ｂの比（ｂ
／ａ）の値が２未満である再結晶粒が全再結晶粒の５０
容量％以上を占め、さらにこの磁石粉末は、粉末粒子の
最長径ｘと最短径ｙの比（ｘ／ｙ）が２〜１０でかつ前
記最短径ｙは６０〜１５０μｍであり、磁化容易方向が
粉末の最短径方向に揃っているＲ−Ｆｅ−Ｃｏ−Ｂ系磁
石粉末、に特徴を有するものである。The present invention has been made based on the results of such research, and (1) an R-Fe-Co-B magnet powder containing R, Fe, Co, and B as main components; The powder has an atomic percentage of R: 10-20%, Co:
0.1-50%, B: 3-20%, Ga, Zr and H
f or a total of one or more of f: 0.001 to 5.
0%, the balance being Fe and unavoidable impurities. Further, this magnet powder has a reusable phase mainly composed of an R 2 (Fe, Co) 14 B type intermetallic compound phase having a tetragonal structure. It has a recrystallized grain texture in which crystal grains are aggregated adjacent to each other, and the average grain size of the recrystallized grains constituting the recrystallized grain texture is 0.05 to 3 μm and the shortest diameter a of the recrystallized grains is The ratio (b / a) of the recrystallized grains having a value (b / a) of less than 2 occupies 50% by volume or more of all the recrystallized grains. Further, this magnet powder has the longest diameter x and the shortest diameter y of the powder particles. Ratio (x / y) is 2
And the shortest diameter y is 60 to 150 μm,
R-Fe whose easy magnetization direction is aligned with the shortest diameter direction of the powder
-Co-B-based magnet powder, (2) R-Fe-Co-B-based magnet powder containing R, Fe, Co, and B as main components, wherein the magnet powder has an atomic percentage of R: 10 to 10. 20%, C
o: 0.1 to 50%, B: 3 to 20%, total of one or more of Ga, Zr and Hf: 0. The R-Fe-Co-B-based magnet powder containing R, Fe, Co, and B as main components has an atomic percentage of R: 10 to 20% and Co:
0.1-50%, B: 3-20%, Ga, Zr and H
f or a total of one or more of f: 0.001 to 5.
0%, and further contains one or more of Al, V and Si: 0.01 to 2.0%,
The balance has a composition consisting of Fe and unavoidable impurities, and this magnet powder is composed of R 2 (Fe, C
o) having a recrystallized grain texture in which recrystallized grains mainly composed of a 14 B-type intermetallic compound phase are aggregated adjacent to each other, and the average grain size of the recrystallized grains constituting the recrystallized grain texture Is 0.05
３3 μm and the ratio of the shortest diameter a to the longest diameter b of the recrystallized grains (b
/ A) is less than 2 in all recrystallized grains.
%, And the ratio of the longest diameter x to the shortest diameter y (x / y) of the powder particles is 2 to 10 and the shortest diameter y is 60 to 150 μm. R-Fe-Co-B-based magnet powder that is aligned in the shortest diameter direction of the powder.

【００１０】前記（１）または（２）記載のＲ−Ｆｅ−
Ｃｏ−Ｂ系磁石粉末は、使用するＲ−Ｆｅ−Ｃｏ−Ｂ系
磁石粉末の全磁石粉末の中に２０〜１００容量％存在す
ることが好ましい、したがって、この発明は、（３）前
記（１）または（２）記載のＲ−Ｆｅ−Ｃｏ−Ｂ系磁石
粉末が全磁石粉末の中に２０〜１００容量％存在するＲ
−Ｆｅ−Ｃｏ−Ｂ系磁石粉末、に特徴を有するものであ
る。The R-Fe- according to the above (1) or (2)
The Co-B-based magnetic powder is preferably present in an amount of 20 to 100% by volume in the total magnet powder of the R-Fe-Co-B-based magnetic powder to be used. Therefore, the present invention provides (3) (1) ) Or R wherein the R-Fe-Co-B-based magnet powder according to (2) is present in an amount of 20 to 100% by volume in the total magnet powder.
-Fe-Co-B based magnet powder.

【００１１】前記（１）記載のＲ−Ｆｅ−Ｃｏ−Ｂ系磁
石粉末は、原子百分率で、Ｒ：１０〜２０％、Ｃｏ：
０．１〜５０％、Ｂ：３〜２０％、Ｇａ，ＺｒおよびＨ
ｆのうち１種または２種以上の合計：０．００１〜５．
０％を含有し、残りがＦｅおよび不可避不純物からなる
組成を有する合金溶湯を、冷却金型の上に６０〜１５０
μｍの範囲内の厚さになるように鋳造して厚さ方向にＲ
2 （Ｆｅ，Ｃｏ）14Ｂ型金属間化合物相のｃ軸が配向し
たフィルム状の鋳造体を作製し、このフィルム状の鋳造
体を１０Ｔｏｒｒ以上の水素ガス雰囲気中または水素ガ
ス分圧：１０Ｔｏｒｒ以上の水素ガスと不活性ガスの混
合ガス雰囲気中で温度：５００〜１０００℃に保持して
前記フィルム状の鋳造体に水素を吸蔵させた後、水素ガ
ス圧力：１×１０-1Ｔｏｒｒ以下の真空雰囲気または水
素ガス分圧：１×１０-1Ｔｏｒｒ以下の不活性ガス雰囲
気になるまで温度：５００〜１０００℃で脱水素処理し
たのち、冷却し、ついで粉砕することにより製造するこ
とができる。The R-Fe-Co-B-based magnet powder described in the above (1) has an atomic percentage of R: 10 to 20%, Co:
0.1-50%, B: 3-20%, Ga, Zr and H
f or a total of one or more of f: 0.001 to 5.
An alloy melt containing 0% and the balance of Fe and unavoidable impurities is placed on a cooling mold by 60-150.
μm and cast in the thickness direction.
A film-like casting is prepared in which the c-axis of the 2 (Fe, Co) 14 B-type intermetallic compound phase is oriented, and this film-like casting is placed in a hydrogen gas atmosphere of 10 Torr or more or a hydrogen gas partial pressure: 10 Torr or more. After hydrogen is absorbed into the film-like casting by maintaining the temperature at 500 to 1000 ° C. in a mixed gas atmosphere of hydrogen gas and an inert gas, the hydrogen gas pressure is 1 × 10 −1 Torr or less. Atmosphere or hydrogen gas partial pressure: Dehydrogenation treatment at a temperature of 500 to 1000 ° C. until an inert gas atmosphere of 1 × 10 −1 Torr or less is obtained, followed by cooling and pulverization.

【００１２】また、前記（２）記載のＲ−Ｆｅ−Ｃｏ−
Ｂ系磁石粉末は、原子百分率で、Ｒ：１０〜２０％、Ｃ
ｏ：０．１〜５０％、Ｂ：３〜２０％、Ｇａ，Ｚｒおよ
びＨｆのうち１種または２種以上の合計：０．００１〜
５．０％を含有し、さらに、Ａｌ，ＶおよびＳｉのうち
１種または２種以上の合計：０．０１〜２．０％を含有
し、残りがＦｅおよび不可避不純物からなる組成を有す
る合金溶湯を、冷却金型の上に６０〜１５０μｍの範囲
内の厚さになるように鋳造して厚さ方向にＲ2（Ｆｅ，
Ｃｏ）14Ｂ型金属間化合物相のｃ軸が配向したフィルム
状の鋳造体を作製し、このフィルム状の鋳造体を１０Ｔ
ｏｒｒ以上の水素ガス雰囲気中または水素ガス分圧：１
０Ｔｏｒｒ以上の水素ガスと不活性ガスの混合ガス雰囲
気中で温度：５００〜１０００℃に保持して水素を吸蔵
させた後、水素ガス圧力：１×１０-1Ｔｏｒｒ以下の真
空雰囲気または水素ガス分圧：１×１０-1Ｔｏｒｒ以下
の不活性ガス雰囲気になるまで温度：５００〜１０００
℃で脱水素処理したのち、冷却し、ついで粉砕すること
により製造することができる。Further, R-Fe-Co- described in the above (2)
The B-based magnet powder has an atomic percentage of R: 10 to 20%, C:
o: 0.1 to 50%, B: 3 to 20%, total of one or more of Ga, Zr and Hf: 0.001 to
Alloy containing 5.0%, and further containing one or more of Al, V, and Si: 0.01 to 2.0%, with the balance being Fe and unavoidable impurities The molten metal is cast on a cooling mold so as to have a thickness in the range of 60 to 150 μm, and R 2 (Fe,
Co) A film-shaped casting in which the c-axis of the 14B type intermetallic compound phase is oriented is produced, and this film-shaped casting is
in a hydrogen gas atmosphere of at least orr or hydrogen gas partial pressure: 1
After storing hydrogen in a mixed gas atmosphere of hydrogen gas and inert gas at 0 Torr or more while maintaining the temperature at 500 to 1000 ° C., hydrogen gas pressure: 1 × 10 −1 Torr or less in a vacuum atmosphere or hydrogen gas Pressure: 1 to 10 -1 Torr or less until an inert gas atmosphere is reached. Temperature: 500 to 1000
After dehydrogenating at ℃, it can be produced by cooling and then pulverizing.

【００１３】前記（１）または（２）記載の組成を有す
るＲ−Ｆｅ−Ｃｏ−Ｂ系合金溶湯から厚さ方向にＲ
2 （Ｆｅ，Ｃｏ）14Ｂ型金属間化合物相のｃ軸が配向し
たフィルム状の鋳造体を作製するには、前記Ｒ−Ｆｅ−
Ｃｏ−Ｂ系合金溶湯を冷却金型の上に６０〜１５０μｍ
の範囲内の厚さになるように鋳造して作製する。一層具
体的には、図２に示されるように、冷却金型として冷却
ロール４を使用し、ルツボ２内の合金溶湯１をノズル３
から回転する冷却ロール４の表面に落下させ、急冷して
冷却ロール４の表面に６０〜１５０μｍの範囲内の厚さ
のフィルム状の鋳造体５を形成する。この時、フィルム
状の鋳造体５の厚さが６０μｍ未満であるとアモルファ
ス組織または超微細な等方性の結晶組織となるが、フィ
ルム状の鋳造体５の厚さが６０μｍ以上となると、厚さ
方向にＲ2 （Ｆｅ，Ｃｏ）14Ｂ型金属間化合物相のｃ軸
が配向したフィルム状の鋳造体が得られる。しかし、フ
ィルム状の鋳造体５の厚さが１５０μｍを越えると、溶
湯凝固の際に結晶成長による厚さ方向のｃ軸配向が不十
分となるので好ましくない。From the R-Fe-Co-B alloy melt having the composition described in (1) or (2) above, R
In order to produce a film-like casting in which the c-axis of the 2 (Fe, Co) 14 B-type intermetallic compound phase is oriented, the R-Fe-
Co-B alloy melt is placed on a cooling mold by 60-150 μm
It is manufactured by casting so as to have a thickness within the range described above. More specifically, as shown in FIG. 2, a cooling roll 4 is used as a cooling mold, and a molten alloy 1 in a crucible 2 is
The cooling roll 4 is dropped on the surface of the rotating cooling roll 4 and rapidly cooled to form a film-like casting 5 having a thickness in the range of 60 to 150 μm on the surface of the cooling roll 4. At this time, if the thickness of the film-like casting 5 is less than 60 μm, an amorphous structure or an ultrafine isotropic crystal structure is obtained, but if the thickness of the film-like casting 5 becomes 60 μm or more, the thickness increases. Thus, a film-shaped casting in which the c-axis of the R 2 (Fe, Co) 14 B type intermetallic compound phase is oriented in the direction of the length is obtained. However, if the thickness of the film-like cast body 5 exceeds 150 μm, the c-axis orientation in the thickness direction due to crystal growth during solidification of the molten metal becomes insufficient, which is not preferable.

【００１４】つぎに、この発明のＲ−Ｆｅ−Ｃｏ−Ｂ系
磁石粉末の成分組成、結晶粒径および結晶粒形状を上記
の如く限定した理由について説明する。 Ａ．成分組成 （ａ）Ｒ Ｒは、Ｎｄ，Ｐｒ，Ｔｂ，Ｄｙ，Ｌａ，Ｃｅ，Ｈｏ，Ｅ
ｒ，Ｅｕ，Ｓｍ，Ｇｄ，Ｔｍ，Ｙｂ，ＬｕおよびＹのう
ち１種または２種以上であり、一般にＮｄを主体とし、
これにその他の希土類元素を添加して用いられるが、特
にＴｂ，ＤｙおよびＰｒは保磁力ｉＨｃを向上させる効
果があり、Ｒの含有量が１０％より低くても、また２０
％より高くても磁石粉末の保磁力が低下し、優れた磁気
特性が得られない。したがって、Ｒの含有量は１０〜２
０％に定めた。Next, the reason why the component composition, crystal grain size, and crystal grain shape of the R-Fe-Co-B magnet powder of the present invention are limited as described above will be described. A. Component composition (a) R R is Nd, Pr, Tb, Dy, La, Ce, Ho, E
one or more of r, Eu, Sm, Gd, Tm, Yb, Lu, and Y, generally mainly Nd;
Tb, Dy, and Pr are particularly effective in improving the coercive force iHc, and may be used by adding other rare earth elements thereto, even if the R content is lower than 10% or 20%.
%, The coercive force of the magnet powder is reduced, and excellent magnetic properties cannot be obtained. Therefore, the content of R is 10-2.
It was set to 0%.

【００１５】（ｂ）Ｂ Ｂの含有量が３％より低くても、また２０％より高くて
も磁石粉末の保磁力が低下し、優れた磁気特性が得られ
ないので、Ｂ含有量は３〜２０％と定めた。(B) BB If the B content is lower than 3% or higher than 20%, the coercive force of the magnet powder is reduced and excellent magnetic properties cannot be obtained. ２０20%.

【００１６】（ｃ）Ｃｏ Ｃｏを添加することにより磁石粉末の保磁力および磁気
的温度特性（例えば、キュリー点）が向上し、さらに耐
食性を向上させる効果があるが、その含有量が０．１％
未満では所望の効果が得られず、一方、５０％を超えて
含有してもかえって磁気特性が低下するので好ましくな
い。したがって、Ｃｏの含有量は０．１〜５０％に定め
た。Ｃｏの含有量は、０．１〜２０％の間では、最も保
磁力が高くなるのでＣｏ：０．１〜２０％とするのが一
層好ましい。(C) Co The addition of Co improves the coercive force and magnetic temperature characteristics (eg, Curie point) of the magnet powder, and has the effect of further improving the corrosion resistance. %
If the content is less than 50%, the desired effect cannot be obtained. On the other hand, if the content exceeds 50%, the magnetic properties are rather deteriorated. Therefore, the content of Co is set to 0.1 to 50%. When the content of Co is between 0.1 and 20%, the coercive force becomes highest, so that it is more preferable that the content of Co be 0.1 to 20%.

【００１７】（ｄ）Ｇａ，ＺｒおよびＨｆ これらの成分は、Ｒ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末の成分
として含有し、保磁力を向上させるとともに優れた磁気
的異方性および耐食性を安定的に付与する作用を有する
が、その含有量が０．００１％未満では所望の効果が得
られず、一方、５．０％を超えて含有すると磁気特性が
低下する。したがって、Ｇａ，ＺｒおよびＨｆのうち１
種または２種以上の合計は０．００１〜５．０％に定め
た。(D) Ga, Zr and Hf These components are contained as components of the R-Fe-Co-B-based magnet powder to improve the coercive force and stably provide excellent magnetic anisotropy and corrosion resistance. However, if the content is less than 0.001%, the desired effect cannot be obtained. On the other hand, if the content exceeds 5.0%, the magnetic properties deteriorate. Therefore, one of Ga, Zr and Hf
The total of the species or two or more species is set to 0.001 to 5.0%.

【００１８】（ｅ）Ａｌ，ＶおよびＳｉ Ｇａ，Ｚｒ，Ｈｆのうち１種または２種以上：０．００
１〜５．０％含有するＲ−Ｆｅ−Ｃｏ−Ｂ系永久磁石粉
末合金に、Ａｌ，ＶおよびＳｉのうち１種または２種以
上を添加することにより最大エネルギー積を安定して高
めることができるので必要に応じて添加するが、その含
有量が０．０１％未満では所望の効果が得られず、一
方、２．０％を超えて添加しても、磁化の値を高めるこ
とができないので好ましくない。したがって、Ａｌ，Ｖ
およびＳｉのうち１種または２種以上は合計量で０．０
１〜２．０％に定めた。(E) One or more of Al, V and SiGa, Zr, Hf: 0.00
It is possible to stably increase the maximum energy product by adding one or more of Al, V and Si to an R-Fe-Co-B-based permanent magnet powder alloy containing 1 to 5.0%. It can be added as necessary, but if its content is less than 0.01%, the desired effect cannot be obtained. On the other hand, if it exceeds 2.0%, the value of magnetization cannot be increased. It is not preferable. Therefore, Al, V
One or more of Si and Si in a total amount of 0.0
It was set to 1 to 2.0%.

【００１９】Ｂ．再結晶粒 （ｆ）再結晶粒径およびその形状 Ｒ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末の組織を構成するＲ
2 （Ｆｅ，Ｃｏ）14Ｂ型相の再結晶粒の粒径が０．０５
μｍより小さいと着磁が困難になるので好ましくなく、
一方、３μｍより大きいと保磁力や角型性が低下し、高
磁気特性が得られないので好ましくない。B. Recrystallized grain (f) Recrystallized grain size and its shape R constituting the structure of the R-Fe-Co-B magnet powder
The particle size of the recrystallized grains of the 2 (Fe, Co) 14 B type phase is 0.05
If it is smaller than μm, it becomes difficult to magnetize,
On the other hand, if it is larger than 3 μm, the coercive force and the squareness decrease, and high magnetic properties cannot be obtained, which is not preferable.

【００２０】したがって、再結晶粒径は０．０５〜３μ
ｍに定めた。この場合、再結晶粒径は単磁区粒径の寸法
（０．３μｍ）に近い０．１〜０．６μｍとする方が一
層好ましい。上記寸法を有する個々の再結晶粒は、最短
粒径ａと最長粒径ｂの比が（ｂ／ａ）＜２の形状を有す
ることが好ましく、この形状を有する再結晶粒は、全再
結晶粒の５０容量％以上存在することが必要である。Therefore, the recrystallized particle size is 0.05 to 3 μm.
m. In this case, the recrystallized grain size is more preferably 0.1 to 0.6 μm which is close to the size of the single magnetic domain grain size (0.3 μm). The individual recrystallized grains having the above dimensions preferably have a shape in which the ratio of the shortest particle size a to the longest particle size b is (b / a) <2. It is necessary that 50% by volume or more of the grains be present.

【００２１】上記最短粒径ａと最長粒径ｂの比ｂ／ａが
２より小さい再結晶粒形状を有することにより、Ｒ−Ｆ
ｅ−Ｃｏ−Ｂ系磁石粉末の保磁力が改善されると共に耐
食性も向上し、さらに保磁力の温度係数も小さくなる。
したがって上記個々の再結晶粒のｂ／ａの値は２未満に
定めた。By having a recrystallized grain shape in which the ratio b / a of the shortest particle diameter a to the longest particle diameter b is smaller than 2, R-F
The coercive force of the e-Co-B-based magnet powder is improved, the corrosion resistance is improved, and the temperature coefficient of the coercive force is reduced.
Therefore, the value of b / a of the individual recrystallized grains is set to less than 2.

【００２２】Ｃ．磁石粉末およびその形状 （ｇ）磁石粉末粒子の最短径 ＨＤＤＲ処理に供するフィルム状の鋳造体の厚さが６０
μｍ未満では超急冷されてアモルファスまたは超微細な
Ｒ2 （Ｆｅ，Ｃｏ）14Ｂ型金属間化合物相のｃ軸が等方
的に分布した組織を有するフィルム状の鋳造体が得られ
るので好ましくなく、一方、フィルム状の鋳造体の厚さ
が１５０μｍを越えると溶湯凝固の際に、結晶成長によ
る厚さ方向のｃ軸配向が不十分となるので好ましくな
い。したがって、フィルム状の鋳造体の厚さを６０〜１
５０μｍに定めた。一層好ましい厚さは７０〜１１０μ
ｍである。この６０〜１５０μｍの厚さのＲ2 （Ｆｅ，
Ｃｏ）14Ｂ型金属間化合物相のｃ軸が配向したフィルム
状の鋳造体をＨＤＤＲ処理した後、粉砕することによっ
てフィルム状の鋳造体の厚さがそのまま磁石粉末粒子の
最短径ｙになり、最短径ｙが６０〜１５０μｍ（好まし
くは７０〜１１０μｍ）の範囲内の磁石粉末粒子が得ら
れる。C. Magnet Powder and Shape (g) Shortest Diameter of Magnet Powder Particles The thickness of a film-shaped casting to be subjected to HDDR processing is 60.
If the thickness is less than μm, the film is super-quenched to obtain a film-like cast having a structure in which the c-axis of the amorphous or ultrafine R 2 (Fe, Co) 14 B-type intermetallic compound phase is isotropically distributed. On the other hand, if the thickness of the film-shaped casting exceeds 150 μm, the c-axis orientation in the thickness direction due to crystal growth becomes insufficient during solidification of the molten metal, which is not preferable. Therefore, the thickness of the film-like casting is set to 60 to 1
It was set to 50 μm. More preferred thickness is 70-110μ
m. This 60 to 150 μm thick R 2 (Fe,
Co) 14 after the c-axis of the B-type intermetallic compound phase has HDDR process the films shaped cast body orientation, it becomes shortest diameter y of the magnetic powder particles the thickness of the film-like casting by grinding, The magnet powder particles having the shortest diameter y in the range of 60 to 150 μm (preferably 70 to 110 μm) are obtained.

【００２３】（ｈ）磁石粉末粒子の最長径と最短径の比 ＨＤＤＲ処理しかつＲ2 （Ｆｅ，Ｃｏ）14Ｂ型金属間化
合物相のｃ軸が配向した厚さ：６０〜１５０μｍのフィ
ルム状の鋳造体を粉砕して磁石粉末粒子の最長径ｘと最
短径ｙの比（ｘ／ｙ）が２〜１０のこの発明のＲ−Ｆｅ
−Ｃｏ−Ｂ系磁石粉末を作製する。最長径ｘと最短径ｙ
の比（ｘ／ｙ）を２〜１０に限定した理由は、ｘ／ｙが
２未満では成形時の磁石粉末粒子の機械的配向の効果が
十分でなく、一方、１０を越えると磁石粉末粒子が大き
くなり過ぎて成形性が低下するので好ましくないことに
よるものである。磁石粉末粒子の最長径ｘと最短径ｙの
比（ｘ／ｙ）の一層好ましい範囲は、３〜７である。(H) Ratio of the longest diameter to the shortest diameter of the magnet powder particles A film having a thickness of 60 to 150 μm which has been subjected to HDDR treatment and the c axis of the R 2 (Fe, Co) 14 B type intermetallic compound phase is oriented. Of the present invention wherein the ratio (x / y) of the longest diameter x and the shortest diameter y of the magnet powder particles is 2 to 10
-Co-B based magnet powder is produced. Longest diameter x and shortest diameter y
The reason why the ratio (x / y) is limited to 2 to 10 is that if x / y is less than 2, the effect of mechanical orientation of the magnet powder particles at the time of molding is not sufficient. Is too large and the moldability decreases, which is not preferable. A more preferable range of the ratio (x / y) between the longest diameter x and the shortest diameter y of the magnet powder particles is 3 to 7.

【００２４】この発明のＲ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末
の構成を一層理解し安くするために、Ｒ−Ｆｅ−Ｃｏ−
Ｂ系磁石粉末の模型図面を用いて説明する。図１はこの
発明のＲ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末の説明図である。
図１において、６は一個の磁石粉末粒子であり、この磁
石粉末粒子は最短径ｙが６０〜１５０μｍの範囲内にあ
り、さらに最長径ｘと最短径ｙの比（ｘ／ｙ）が２〜１
０の範囲内にある。この磁石粉末粒子の内部組織は平均
粒径が０．０５〜３μｍの再結晶粒７が相互に隣接して
集合した再結晶粒集合組織を有し、この再結晶粒７は最
短粒径ａと最長粒径ｂの比が（ｂ／ａ）＜２の形状を有
している。この発明のＲ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末を
用いてボンド磁石を製造するには、図１に示される磁石
粉末粒子を２０〜１００％含有するＲ−Ｆｅ−Ｃｏ−Ｂ
系磁石粉末を用いて製造する。In order to further understand and reduce the constitution of the R-Fe-Co-B-based magnet powder of the present invention, R-Fe-Co-B
This will be described with reference to a model drawing of the B-based magnet powder. FIG. 1 is an explanatory view of the R-Fe-Co-B-based magnet powder of the present invention.
In FIG. 1, reference numeral 6 denotes one magnet powder particle having a shortest diameter y in the range of 60 to 150 μm and a ratio (x / y) of the longest diameter x to the shortest diameter y of 2 to 2 μm. 1
It is in the range of 0. The internal structure of the magnet powder particles has a recrystallized grain texture in which recrystallized grains 7 having an average particle diameter of 0.05 to 3 μm are aggregated adjacent to each other. It has a shape in which the ratio of the longest particle size b is (b / a) <2. In order to manufacture a bonded magnet using the R-Fe-Co-B-based magnet powder of the present invention, R-Fe-Co-B containing 20 to 100% of the magnet powder particles shown in FIG.
Manufactured using a system magnet powder.

【００２５】[0025]

【発明の実施の形態】実施例１ 高周波溶解して表１に示される成分組成を有し、温度：
１３５０℃に保持された合金溶湯Ａ〜Ｊを用意した。合
金溶湯Ａ〜Ｊを、図２に示されるように、ルツボ２から
温度：２０〜３０℃の範囲内の所定の温度に保持された
真空中で周速：１０〜３０ｍ／sec.の範囲内の所定の値
で回転する冷却ロール４の表面に落下させ、急冷して冷
却ロール４の表面に表２〜５に示される厚さを有し、Ｒ
2 （Ｆｅ，Ｃｏ）14Ｂ型金属間化合物相のｃ軸が配向し
たフィルム状の鋳造体を作製した。DESCRIPTION OF THE PREFERRED EMBODIMENTS Example 1 High frequency melting was carried out to have the component composition shown in Table 1 and temperature:
Molten alloys A to J maintained at 1350 ° C. were prepared. As shown in FIG. 2, the molten alloys A to J are placed in a vacuum maintained at a predetermined temperature within the range of 20 to 30 ° C. from the crucible 2 in a vacuum at a peripheral speed of 10 to 30 m / sec. Is dropped on the surface of the cooling roll 4 rotating at a predetermined value, and is rapidly cooled to have a thickness shown in Tables 2 to 5 on the surface of the cooling roll 4.
A film-like cast was prepared in which the c-axis of the 2 (Fe, Co) 14 B-type intermetallic compound phase was oriented.

【００２６】得られたフィルム状の鋳造体を１気圧の水
素雰囲気中で室温から８３０℃まで昇温し、８３０℃で
４時間保持の水素雰囲気中熱処理を施し、ついで、８３
０℃、真空度：１×１０-1Torr以下になるまで脱水素を
行った後、直ちにアルゴンガスを流入して急冷する条件
のＨＤＤＲ処理を施すことにより、再結晶粒が相互に隣
接して集合した再結晶集合組織を有するＨＤＤＲ処理体
を作製した。このＨＤＤＲ処理体を平均再結晶粒径、再
結晶粒の最短径ａと最長径ｂの比（ｂ／ａ）を測定し、
その結果を表２〜５に示した。さらに得られたＨＤＤＲ
処理体を粉砕することにより、表２〜５に示に示される
最短径ｙおよび最長径ｘと最短径ｙの比（ｘ／ｙ）を有
する本発明磁石粉末１〜２０を作製した。なお、本発明
磁石粉末の平均結晶粒径および個々の結晶粒の最長径ｂ
／最短径ａの値は透過電子顕微鏡により観察し、本発明
磁石粉末の寸法は金属顕微鏡で測定した。The obtained film-shaped casting is heated from room temperature to 830 ° C. in a hydrogen atmosphere at 1 atm, and is subjected to a heat treatment in a hydrogen atmosphere maintained at 830 ° C. for 4 hours.
After dehydrogenation at 0 ° C. and a degree of vacuum of 1 × 10 −1 Torr or less, the recrystallized grains are adjacent to each other by immediately performing an HDDR process under the condition of flowing argon gas and rapidly cooling. An HDDR treated body having an assembled recrystallized texture was produced. The average recrystallized grain size of the HDDR-treated body and the ratio (b / a) of the shortest diameter a to the longest diameter b of the recrystallized grains were measured.
The results are shown in Tables 2 to 5. Further obtained HDDR
The magnet powders 1 to 20 of the present invention having the shortest diameter y and the ratio of the longest diameter x to the shortest diameter y (x / y) shown in Tables 2 to 5 were produced by pulverizing the treated body. The average crystal grain size of the magnet powder of the present invention and the longest diameter b of each crystal grain
/ The value of the shortest diameter a was observed with a transmission electron microscope, and the dimensions of the magnet powder of the present invention were measured with a metallographic microscope.

【００２７】このようにして得られた本発明磁石粉末１
〜２０比較磁石粉末１〜２および従来磁石粉末をビスマ
レイミドトリアジン樹脂をと混合してコンパウンド（混
合物）を作製し、このコンパウンドを金型に充填し、圧
縮方向に平行に１００００エルステッドの磁場をかけな
がら圧力：６ton ／cm2 で圧縮成形する平行磁界中成形
および磁界なしで成形する無磁界中成形を行うことによ
り直径：１２mm、長さ：８mmの寸法を有する成形体を作
製し、ついでこの成形体を真空雰囲気中、温度：１５０
℃、１時間保持の加熱を行ってボンド磁石を作製し、こ
れらボンド磁石の磁気特性を測定し、その結果を表２〜
５に示した。The magnetic powder 1 of the present invention thus obtained
A compound (mixture) is prepared by mixing a comparative magnet powder 1-2 and a conventional magnet powder with a bismaleimide triazine resin, and the compound is filled in a mold, and a magnetic field of 10,000 Oersted is applied in parallel to the compression direction. A compact having a size of 12 mm in diameter and 8 mm in length was produced by performing compacting in a parallel magnetic field in which compression was performed at a pressure of 6 ton / cm 2 and compaction in a non-magnetic field in the absence of a magnetic field. Body in vacuum atmosphere, temperature: 150
C. for 1 hour to produce bonded magnets, and measured the magnetic properties of these bonded magnets.
5 is shown.

【００２８】従来例１ 本発明磁石粉末１と同一の成分組成を有する合金溶湯を
鋳造して縦：２００mm、横：４００mm、高さ：１０mmの
寸法を有するインゴットを作製し、このインゴットをカ
プセルにいれ、脱気し、密封し、これを９５０℃で加工
度：３０％の熱間圧延を４回行い、最終加工度：７６％
の圧延材を作製し、この圧延材を実施例１と同じ条件の
ＨＤＤＲ処理を行うことにより従来磁石粉末を作製し、
この従来磁石粉末を用いて実施例１と同様にしてボンド
磁石を作製し、得られたボンド磁石の磁気特性を測定
し、その結果を表５に示した。Conventional Example 1 An alloy melt having the same composition as the magnetic powder 1 of the present invention was cast to produce an ingot having dimensions of 200 mm in length, 400 mm in width and 10 mm in height, and this ingot was used as a capsule. Then, it was degassed, sealed, and subjected to hot rolling four times at 950 ° C. at a working ratio of 30% to a final working ratio of 76%.
And a conventional magnet powder was prepared by subjecting the rolled material to HDDR treatment under the same conditions as in Example 1.
Using this conventional magnet powder, a bonded magnet was produced in the same manner as in Example 1, and the magnetic properties of the obtained bonded magnet were measured. The results are shown in Table 5.

【００２９】[0029]

【表１】 [Table 1]

【００３０】[0030]

【表２】 [Table 2]

【００３１】[0031]

【表３】 [Table 3]

【００３２】[0032]

【表４】 [Table 4]

【００３３】[0033]

【表５】 [Table 5]

【００３４】表１および表５に示される結果から、
（イ）本発明磁石粉末１〜２と従来磁石粉末を比較する
と、共に同じ成分組成の合金溶湯Ａから製造したもので
あるにもかかわらず、本発明磁石粉末１〜２で作製した
ボンド磁石の磁気特性は平行磁界中成形および無磁界中
成形ともに従来磁石粉末で作製したボンド磁石の磁気特
性よりも格段に優れている、（ロ）しかしながら、粉末
粒子の最短径ｙがこの発明から外れた比較磁石粉末１〜
２で作製したボンド磁石の磁気特性は本発明磁石粉末１
〜２で作製したボンド磁石の磁気特性よりも低下するこ
とが分かる。同様にして、本発明磁石粉末３〜２０で作
製したボンド磁石は従来よりも優れた磁気特性を有する
ことを確認した。From the results shown in Tables 1 and 5,
(A) Comparing the magnet powders 1 and 2 of the present invention and the conventional magnet powders, it can be seen that although the magnet powders were both manufactured from the molten alloy A having the same component composition, the bond magnets manufactured by the magnet powders 1 and 2 of the present invention were The magnetic properties are significantly better in both parallel magnetic field molding and non-magnetic field molding than the bonded magnets made with conventional magnet powder. (B) However, the shortest diameter y of the powder particles is out of the range of the present invention. Magnet powder 1
The magnetic properties of the bonded magnet prepared in 2 are the same as those of the magnet powder 1 of the present invention.
It can be seen that the magnetic properties are lower than the magnetic properties of the bonded magnets manufactured in Nos. 1 to 2. Similarly, it was confirmed that the bonded magnets prepared with the magnet powders 3 to 20 of the present invention had better magnetic properties than the conventional one.

【００３５】[0035]

【発明の効果】この発明は、ＣｏとともにＧａ，Ｚｒ，
Ｈｆのうち１種または２種以上を含有するＲ−Ｆｅ−Ｃ
ｏ−Ｂ系磁石粉末を熱間塑性加工を施すことなくＨＤＤ
Ｒ処理することにより顕著な磁気的異方性を示すという
優れた効果をもたらすものである。According to the present invention, Ga, Zr,
R-Fe-C containing one or more of Hf
HDD without hot plastic working of OB magnet powder
By performing the R treatment, an excellent effect of exhibiting remarkable magnetic anisotropy can be obtained.

【図面の簡単な説明】[Brief description of the drawings]

【図１】この発明のＲ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末の説
明図である。FIG. 1 is an explanatory view of an R—Fe—Co—B-based magnet powder of the present invention.

【図２】ｃ軸が配向したフィルム状の鋳造体を作製する
方法を示す説明図である。FIG. 2 is an explanatory view showing a method for producing a film-shaped casting in which the c-axis is oriented.

【符号の説明】[Explanation of symbols]

１ 合金溶湯 ２ ルツボ ３ ノズル ４ 冷却ロール ５ フィルム状の鋳造体 ６ 粉末粒子 ７ 再結晶粒 REFERENCE SIGNS LIST 1 molten alloy 2 crucible 3 nozzle 4 cooling roll 5 film-like casting 6 powder particle 7 recrystallized particle

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｂ２２Ｆ 9/04 Ｂ２２Ｆ 3/00 Ｆ (72)発明者 石井 義成 埼玉県大宮市北袋町１−297 三菱マテリ アル株式会社総合研究所内 Ｆターム(参考） 4K017 BA06 BB06 BB09 BB12 BB18 CA03 DA04 EA03 EC02 ED01 EE02 EK07 FB02 4K018 BA05 BA18 BB01 BB04 BB06 BC40 BD01 KA46 5E040 AA04 AA19 BB03 CA01 HB07 HB09 HB11 HB17 NN01 NN06 NN17 NN18 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) B22F 9/04 B22F 3/00 F (72) Inventor Yoshinari Ishii 1-297 Kitabukurocho, Omiya City, Saitama Prefecture Mitsubishi Materi 4K017 BA06 BB06 BB09 BB12 BB18 CA03 DA04 EA03 EC02 ED01 EE02 EK07 FB02 4K018 BA05 BA18 BB01 BB04 BB04 BC40 BD01 KA46 5E040 AA04 AA19 BB03 CA01 HB07 HB09 NN11B

Claims (6)

【特許請求の範囲】[Claims] 【請求項１】 Ｙを含む希土類元素のうち少なくとも１
種（以下、Ｒで示す）とＦｅとＣｏとＢを主成分とする
Ｒ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末であって、 この磁石粉末は、原子百分率で、Ｒ：１０〜２０％、Ｃ
ｏ：０．１〜５０％、Ｂ：３〜２０％、Ｇａ，Ｚｒおよ
びＨｆのうち１種または２種以上の合計：０．００１〜
５．０％を含有し、残りがＦｅおよび不可避不純物から
なる組成を有し、 さらにこの磁石粉末は、正方晶構造をとるＲ2 （Ｆｅ，
Ｃｏ）14Ｂ型金属間化合物相を主相とする再結晶粒が相
互に隣接して集合した再結晶粒集合組織を有し、この再
結晶粒集合組織を構成する再結晶粒の平均粒径は０．０
５〜３μｍでかつ再結晶粒の最短径ａと最長径ｂの比
（ｂ／ａ）の値が２未満である再結晶粒が全再結晶粒の
５０容量％以上を占め、 さらにこの磁石粉末は、粉末粒子の最長径ｘと最短径ｙ
の比（ｘ／ｙ）が２〜１０でかつ前記最短径ｙは６０〜
１５０μｍであり、 さらにこの磁石粉末は磁化容易方向が粉末の最短径方向
に揃っていることを特徴とする希土類−Ｆｅ−Ｃｏ−Ｂ
系磁石粉末。1. At least one of rare earth elements containing Y
An R—Fe—Co—B-based magnet powder containing a seed (hereinafter referred to as R), Fe, Co, and B as main components, the magnet powder having an atomic percentage of R: 10 to 20%, C:
o: 0.1 to 50%, B: 3 to 20%, total of one or more of Ga, Zr and Hf: 0.001 to
The magnet powder has a composition of 5.0%, the balance being Fe and unavoidable impurities. Further, this magnet powder is composed of R 2 (Fe,
Co) 14 B type intermetallic compound phase recrystallized grains as the main phase has a recrystallized grain texture that is set adjacent to each other, an average particle diameter of the recrystallized grains forming the recrystallized grain texture Is 0.0
Recrystallized grains having a value of 5 to 3 μm and a ratio (b / a) of the shortest diameter a to the longest diameter b of the recrystallized grains of less than 2 account for 50% by volume or more of all recrystallized grains. Is the longest diameter x and the shortest diameter y of the powder particles
Is 2 to 10 and the shortest diameter y is 60 to
Rare earth-Fe-Co-B, wherein the magnet powder has an easy magnetization direction aligned with the shortest diameter direction of the powder.
System magnet powder. 【請求項２】 上記ＲとＦｅとＣｏとＢを主成分とする
Ｒ−Ｆｅ−Ｃｏ−Ｂ系磁石粉末は、原子百分率で、Ｒ：
１０〜２０％、Ｃｏ：０．１〜５０％、Ｂ：３〜２０
％、Ｇａ，ＺｒおよびＨｆのうち１種または２種以上の
合計：０．００１〜５．０％を含有し、さらに、Ａｌ，
ＶおよびＳｉのうち１種または２種以上の合計：０．０
１〜２．０％を含有し、残りがＦｅおよび不可避不純物
からなる組成を有し、 さらにこの磁石粉末は、正方晶構造をとるＲ2 （Ｆｅ，
Ｃｏ）14Ｂ型金属間化合物相を主相とする再結晶粒が相
互に隣接して集合した再結晶粒集合組織を有し、この再
結晶粒集合組織を構成する再結晶粒の平均粒径は０．０
５〜３μｍでかつ再結晶粒の最短径ａと最長径ｂの比
（ｂ／ａ）の値が２未満である再結晶粒が全再結晶粒の
５０容量％以上を占め、 さらにこの磁石粉末は、粉末粒子の最長径ｘと最短径ｙ
の比（ｘ／ｙ）が２〜１０でかつ前記最短径ｙは６０〜
１５０μｍであり、 さらにこの磁石粉末は磁化容易方向が粉末の最短径方向
に揃っていることを特徴とする希土類−Ｆｅ−Ｃｏ−Ｂ
系磁石粉末。2. The R—Fe—Co—B-based magnet powder containing R, Fe, Co, and B as main components has an atomic percentage of R:
10-20%, Co: 0.1-50%, B: 3-20
%, A total of one or more of Ga, Zr and Hf: 0.001 to 5.0%.
Total of one or more of V and Si: 0.0
1% to 2.0%, with the balance being Fe and unavoidable impurities. Further, this magnet powder is composed of R 2 (Fe,
Co) 14 B type intermetallic compound phase recrystallized grains as the main phase has a recrystallized grain texture that is set adjacent to each other, an average particle diameter of the recrystallized grains forming the recrystallized grain texture Is 0.0
Recrystallized grains having a value of 5 to 3 μm and a ratio (b / a) of the shortest diameter a to the longest diameter b of the recrystallized grains of less than 2 account for 50% by volume or more of all recrystallized grains. Is the longest diameter x and the shortest diameter y of the powder particles
Is 2 to 10 and the shortest diameter y is 60 to
Rare earth-Fe-Co-B, wherein the magnet powder has an easy magnetization direction aligned with the shortest diameter direction of the powder.
System magnet powder. 【請求項３】 請求項１または２記載の希土類−Ｆｅ−
Ｃｏ−Ｂ系磁石粉末が全磁石粉末の中に２０〜１００容
量％存在することを特徴とする希土類−Ｆｅ−Ｃｏ−Ｂ
系磁石粉末。3. The rare earth element according to claim 1 or 2,
Rare earth-Fe-Co-B, wherein the Co-B based magnet powder is present in an amount of 20 to 100% by volume in the whole magnet powder.
System magnet powder. 【請求項４】 請求項１、２または３記載の希土類−Ｆ
ｅ−Ｃｏ−Ｂ系異方性磁石粉末を樹脂バインダーで結合
したことを特徴とする希土類−Ｆｅ−Ｃｏ−Ｂ系ボンド
磁石。4. The rare earth-F according to claim 1, 2 or 3.
A rare earth-Fe-Co-B-based bonded magnet, wherein e-Co-B-based anisotropic magnet powder is bonded with a resin binder. 【請求項５】 原子百分率で、Ｒ：１０〜２０％、Ｃ
ｏ：０．１〜５０％、Ｂ：３〜２０％、Ｇａ，Ｚｒおよ
びＨｆのうち１種または２種以上の合計：０．００１〜
５．０％を含有し、残りがＦｅおよび不可避不純物から
なる組成を有する合金溶湯を、冷却金型の上に６０〜１
５０μｍの範囲内の厚さになるように鋳造して厚さ方向
にＲ2 （Ｆｅ，Ｃｏ）14Ｂ型金属間化合物相のｃ軸が配
向したフィルム状の鋳造体を作製し、このフィルム状の
鋳造体を１０Ｔｏｒｒ以上の水素ガス雰囲気中または水
素ガス分圧：１０Ｔｏｒｒ以上の水素ガスと不活性ガス
の混合ガス雰囲気中で温度：５００〜１０００℃に保持
して水素を吸蔵させた後、水素ガス圧力：１×１０-1Ｔ
ｏｒｒ以下の真空雰囲気または水素ガス分圧：１×１０
-1Ｔｏｒｒ以下の不活性ガス雰囲気になるまで温度：５
００〜１０００℃で脱水素処理したのち、冷却し、つい
で粉砕することを特徴とする希土類−Ｆｅ−Ｃｏ−Ｂ系
磁石粉末の製造方法。5. Atomic percentage, R: 10 to 20%, C
o: 0.1 to 50%, B: 3 to 20%, total of one or more of Ga, Zr and Hf: 0.001 to
An alloy melt containing 5.0% and a balance of Fe and unavoidable impurities is placed on a cooling mold by 60 to 1%.
The film is cast to a thickness in the range of 50 μm to prepare a film-shaped casting in which the c-axis of the R 2 (Fe, Co) 14 B type intermetallic compound phase is oriented in the thickness direction. Is held in a hydrogen gas atmosphere of 10 Torr or more or in a mixed gas atmosphere of hydrogen gas and an inert gas of hydrogen gas partial pressure: 10 Torr or more at a temperature of 500 to 1000 ° C. to occlude hydrogen. Gas pressure: 1 × 10 -1 T
vacuum atmosphere or hydrogen gas partial pressure of 1 × 10 or less
Temperature until inert gas atmosphere of -1 Torr or less: 5
A method for producing a rare earth-Fe-Co-B-based magnet powder, comprising dehydrogenating at 00 to 1000 ° C, cooling, and then pulverizing. 【請求項６】 前記合金溶湯は、原子百分率で、Ｒ：１
０〜２０％、Ｃｏ：０．１〜５０％、Ｂ：３〜２０％、
Ｇａ，ＺｒおよびＨｆのうち１種または２種以上の合
計：０．００１〜５．０％を含有し、さらに、Ａｌ，Ｖ
およびＳｉのうち１種または２種以上の合計：０．０１
〜２．０％を含有し、残りがＦｅおよび不可避不純物か
らなる組成を有することを特徴とする請求項５記載の希
土類−Ｆｅ−Ｃｏ−Ｂ系磁石粉末の製造方法。6. The alloy melt according to claim 1, wherein R: 1 is an atomic percentage.
0-20%, Co: 0.1-50%, B: 3-20%,
One, two or more of Ga, Zr and Hf: 0.001 to 5.0% in total;
Total of one or more of Si and Si: 0.01
The method for producing a rare-earth-Fe-Co-B-based magnet powder according to claim 5, wherein the composition contains about 2.0% and the balance consists of Fe and unavoidable impurities.
JP02406699A 1999-02-01 1999-02-01 Rare earth-Fe-Co-B based magnet powder, method for producing the same, and bonded magnet using the powder Expired - Fee Related JP3427765B2 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102389974A (en) * 2011-05-12 2012-03-28 朱惠冲 Method for producing magnetron cathode material for preventing recrystallized grains from being coarsened
JP2018056525A (en) * 2016-09-30 2018-04-05 ミネベアミツミ株式会社 Method for manufacturing rare earth iron-based permanent magnet

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102389974A (en) * 2011-05-12 2012-03-28 朱惠冲 Method for producing magnetron cathode material for preventing recrystallized grains from being coarsened
JP2018056525A (en) * 2016-09-30 2018-04-05 ミネベアミツミ株式会社 Method for manufacturing rare earth iron-based permanent magnet

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