JP3278431B2 - Rare earth metal-iron-boron anisotropic permanent magnet powder - Google Patents
Rare earth metal-iron-boron anisotropic permanent magnet powderInfo
- Publication number
- JP3278431B2 JP3278431B2 JP2000314786A JP2000314786A JP3278431B2 JP 3278431 B2 JP3278431 B2 JP 3278431B2 JP 2000314786 A JP2000314786 A JP 2000314786A JP 2000314786 A JP2000314786 A JP 2000314786A JP 3278431 B2 JP3278431 B2 JP 3278431B2
- Authority
- JP
- Japan
- Prior art keywords
- permanent magnet
- rare earth
- iron
- earth metal
- boron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims description 20
- 150000002910 rare earth metals Chemical class 0.000 title claims description 19
- 239000000843 powder Substances 0.000 title claims description 18
- 229910052796 boron Inorganic materials 0.000 title claims description 14
- 238000000034 method Methods 0.000 claims description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 229910052742 iron Inorganic materials 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000002441 X-ray diffraction Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 description 35
- 239000000956 alloy Substances 0.000 description 35
- 239000013078 crystal Substances 0.000 description 19
- 238000005266 casting Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- 238000000265 homogenisation Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 238000004512 die casting Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004781 supercooling Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 229910000521 B alloy Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—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
- H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、磁石特性に優れた
希土類金属−鉄−ボロン系異方性永久磁石用粉末に関す
る。The present invention relates to a rare earth metal-iron-boron based anisotropic permanent magnet powder having excellent magnet properties.
【０００２】[0002]
【従来の技術】従来、永久磁石用合金鋳塊は、溶融した
合金を金型に鋳造する金型鋳造法により製造されている
のが一般的である。しかし該金型鋳造法により合金溶融
物を凝固させる場合、合金溶融物の抜熱過程において、
抜熱初期では鋳型伝熱律速であるが、凝固が進行する
と、鋳型−凝固相間及び凝固相における伝熱が抜熱律速
となり、金型冷却能を向上させても鋳塊内部と鋳型近傍
の鋳塊では、冷却条件が異なり、特に鋳塊厚が厚いほど
このような現象が生じる。このように鋳塊の内部と表面
付近での冷却条件の相違が大きい場合には、特に磁石組
成における高残留磁束密度側の鋳造組織に、初晶γ−Ｆ
ｅが多く存在し、このため鋳塊の中央部に粒径１０〜１
００μｍのα−Ｆｅが残存し、同時に主相を取り巻く希
土類金属に富んだ相の大きさも大きくなる。また前記金
型鋳造法により得られる鋳塊組織中に、短軸方向０．１
〜５０μｍ、長軸方向０．１〜１００μｍの結晶粒径を
有する結晶が存在することが知られているが、該結晶の
含有率は僅かであって、磁石特性に良好な影響を及ぼす
には至っていない。一方、磁石粉末製造工程における均
質化処理過程においては、通常、１０００℃付近で均質
化処理されるが、前記金型鋳造法で得られる鋳塊の場合
には、粒径の大きいα−Ｆｅ及び希土類金属に富んだ大
きな相を含有するので、均質化が困難であり、またその
後の水素化処理による再結晶化の際に、異方化しにく
く、最終的に得られる永久磁石の磁気特性が低下すると
いう欠点がある。さらに、希土類金属元素、コバルト及
び必要に応じて、鉄、銅、ジルコニウムを添加し、ルツ
ボ中で溶解させた後、双ロール、単ロール、双ベルト等
を組み合わせたストリップキャスティング法等で０．０
１〜５ｍｍの厚さとなるように凝固させる希土類金属磁
石用合金の製造法が提案されている。該方法では、金型
鋳造法に比して組成の均一な鋳塊が得られるが、原料成
分が、希土類金属元素、コバルト及び必要に応じて、
鉄、銅、ジルコニウムを組み合わせた成分であるため
に、前記ストリップキャスティング法による磁石性能の
向上が充分に得られない等の問題がある。2. Description of the Related Art Conventionally, alloy ingots for permanent magnets are generally manufactured by a mold casting method of casting a molten alloy into a mold. However, when the alloy melt is solidified by the die casting method, during the heat removal process of the alloy melt,
Heat transfer is limited in the early stage of heat removal, but as solidification progresses, heat transfer between the mold and solidification phase and in the solidification phase becomes heat removal rate. Ingots have different cooling conditions, and such a phenomenon occurs particularly as the thickness of the ingot increases. As described above, when the difference in cooling conditions between the inside and the surface of the ingot is large, the primary crystal γ-F
e is present in a large amount, so that a grain size of 10 to 1
The α-Fe of 00 μm remains, and at the same time, the size of the rare earth metal-rich phase surrounding the main phase also increases. Further, in the ingot structure obtained by the die casting method, 0.1
It is known that there is a crystal having a crystal grain diameter of about 50 μm and a major axis direction of 0.1 to 100 μm. Not reached. On the other hand, in the homogenization process in the magnet powder manufacturing process, the homogenization process is usually performed at around 1000 ° C., but in the case of the ingot obtained by the die casting method, α-Fe and Contains a large phase rich in rare earth metals, which makes it difficult to homogenize, and is less likely to be anisotropic during subsequent recrystallization by hydrogenation, resulting in lower permanent magnet magnetic properties. There is a disadvantage of doing so. Further, after adding a rare earth metal element, cobalt and, if necessary, iron, copper, and zirconium and dissolving them in a crucible, 0.0 roll by a strip casting method or the like combining a twin roll, a single roll, a twin belt and the like.
A method for producing an alloy for a rare earth metal magnet which is solidified so as to have a thickness of 1 to 5 mm has been proposed. In this method, an ingot having a uniform composition is obtained as compared with the die casting method, but the raw material components are rare earth metal elements, cobalt and, if necessary,
Since the composition is a combination of iron, copper, and zirconium, there is a problem that the magnet performance cannot be sufficiently improved by the strip casting method.
【０００３】[0003]
【発明が解決しようとする課題】本発明の目的は、高い
異方性を示し、且つ永久磁石の特性に最も良い影響を与
える結晶組織を有する希土類金属−鉄−ボロン系異方性
永久磁石用粉末を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a rare earth metal-iron-boron anisotropic permanent magnet having a high anisotropy and having a crystal structure most affecting the properties of the permanent magnet. It is to provide a powder.
【０００４】[0004]
【課題を解決するための手段】本発明によれば、希土類
金属、ボロン及び鉄を含み、これらの配合割合が重量比
で２５〜４０：０．５〜２．０：残量であり、且つＸ線
回折により測定した下記式で示される配向度Ｆの値が６
０以上である粒径２００〜４００μｍの希土類金属−鉄
−ボロン系異方性永久磁石用粉末が提供される。According to the present invention, a rare earth element is provided.
Contains metals, boron and iron, and their proportions are weight ratio
25 to 40: 0.5 to 2.0: remaining amount and X-ray
When the value of the degree of orientation F measured by diffraction and represented by the following equation is 6:
A rare earth metal-iron-boron-based anisotropic permanent magnet powder having a particle size of 200 to 400 µm, which is 0 or more, is provided.
【０００５】[0005]
【数２】 (Equation 2)
【０００６】[0006]
【発明の実施の形態】以下本発明を更に詳細に説明す
る。本発明の希土類金属−鉄−ボロン系異方性永久磁石
用粉末（以下、異方性永久磁石用粉末１と称す）は、短
軸方向０．１〜５０μｍ、長軸方向０．１〜１００μｍ
の結晶粒径を有する結晶を９０容量％以上、好ましくは
９８容量％以上含有し、且つ前記主相結晶粒内に、包晶
核である粒径１０μｍ未満のα−Ｆｅ及び／又はγ−Ｆ
ｅを微細分散している希土類金属−鉄−ボロン系合金鋳
塊（以下、合金鋳塊２と称す）を水素化処理し、粉砕し
て得ることができる。その粉末粒径は、２００〜４００
μｍである。また、Ｘ線回折により測定した上記式で示
される配向度Ｆの値は６０以上である。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail. The rare earth metal-iron-boron based anisotropic permanent magnet powder (hereinafter referred to as anisotropic permanent magnet powder 1) of the present invention has a minor axis direction of 0.1 to 50 μm and a major axis direction of 0.1 to 100 μm.
Α-Fe and / or γ-F having a crystal grain size of 90% by volume or more, preferably 98% by volume or more, and having a grain size of less than 10 μm, which is a peritectic nucleus, in the main phase crystal grains.
It can be obtained by subjecting a rare earth metal-iron-boron-based alloy ingot in which e is finely dispersed (hereinafter, referred to as alloy ingot 2) to hydrogenation treatment and pulverization . The powder particle size is 200-400
μm . Further, the value of the degree of orientation F represented by the above equation measured by X-ray diffraction is 60 or more .
【０００７】前記合金鋳塊２において、特定の結晶粒径
を有する結晶の含有割合が、９０容量％未満の場合に
は、得られる合金鋳塊に優れた磁石特性を付与できず、
目的とする異方性永久磁石用粉末１が得られない。また
短軸方向及び長軸方向の長さが前記範囲外である場合、
若しくは該α−Ｆｅ及び／又はγ−Ｆｅの粒径が１０μ
ｍ以上であり、且つ微細分散されていない場合には、永
久磁石用粉末製造工程における均質化処理の際に、均質
化時間が長くなり、更に最終の磁石粉末の磁気特性が低
くなるので好ましくない。[0007] If the content ratio of crystals having a specific crystal grain size in the alloy ingot 2 is less than 90% by volume, excellent magnet properties cannot be imparted to the obtained alloy ingot,
The desired anisotropic permanent magnet powder 1 cannot be obtained. When the length in the short axis direction and the length in the long axis direction are out of the range,
Alternatively, the particle size of the α-Fe and / or γ-Fe is 10 μm.
m or more, and when not finely dispersed, it is not preferable because the homogenization time becomes longer during the homogenization treatment in the permanent magnet powder manufacturing process and the magnetic properties of the final magnet powder are further lowered. .
【０００８】前記合金鋳塊２の厚さは、０．０５〜１５
ｍｍの範囲であるのが好ましい。厚さが１５ｍｍを超え
る場合には、所望の結晶組織とするための後述する製造
法が困難となるので好ましくない。The thickness of the alloy ingot 2 is 0.05 to 15
It is preferably in the range of mm. If the thickness exceeds 15 mm, it is not preferable because a later-described manufacturing method for obtaining a desired crystal structure becomes difficult.
【０００９】前記異方性永久磁石用粉末１に用いる前記
合金鋳塊２を形成する原料成分は、希土類金属−鉄−ボ
ロン系であれば特に限定されるものではなく、通常製造
の際に不可避的に含まれる他の不純物成分を含んでいて
も良い。また希土類金属は、単体でも混合物であっても
良い。該希土類金属と、ボロンと、鉄との配合割合は、
通常の永久磁石用合金での配合割合と同様で良く、好ま
しくは重量比で、２５〜４０：０．５〜２．０：残量で
あるのが好ましい。The raw material components forming the alloy ingot 2 used for the anisotropic permanent magnet powder 1 are not particularly limited as long as they are a rare earth metal-iron-boron system, and are inevitable during normal production. It may contain other impurity components that are included. The rare earth metal may be a simple substance or a mixture. The compounding ratio of the rare earth metal, boron, and iron is
The mixing ratio may be the same as that of an ordinary permanent magnet alloy, and is preferably 25 to 40: 0.5 to 2.0: residual amount by weight.
【００１０】本発明の異方性永久磁石用粉末１を製造す
るには、まず希土類金属−鉄−ボロン系合金溶融物を、
冷却速度１０〜１０００℃／秒、好ましくは１００〜１
０００℃／秒、過冷度１０〜５００℃、好ましくは２０
０〜５００℃の冷却条件下で均一に凝固させる方法等に
より前記合金鋳塊２を得、次いで、水素雰囲気中で前記
合金鋳塊２に水素原子を侵入及び放出させることにより
主相結晶等を再結晶化させる水素化処理の後、粉砕する
方法により得ることができる。In order to produce the powder 1 for anisotropic permanent magnet of the present invention, first, a rare earth metal-iron-boron alloy melt is mixed with:
Cooling rate 10 to 1000 ° C./sec, preferably 100 to 1
000 ° C / sec, degree of supercooling 10 to 500 ° C, preferably 20
The alloy ingot 2 is obtained by, for example, a method of uniformly solidifying under cooling conditions of 0 to 500 ° C., and then the main phase crystals and the like are formed by invading and releasing hydrogen atoms into the alloy ingot 2 in a hydrogen atmosphere. It can be obtained by a pulverization method after the hydrogenation treatment for recrystallization.
【００１１】ここで、過冷度とは、（合金の融点）−
（合金溶融物の実際の温度）の値であって、冷却速度と
相関関係を有する。冷却速度及び過冷度が前記必須範囲
外の場合には、所望の組織を有する合金鋳塊が得られな
い。Here, the degree of supercooling is (melting point of alloy) −
(Actual temperature of the alloy melt) and has a correlation with the cooling rate. If the cooling rate and the degree of subcooling are out of the essential ranges, an alloy ingot having a desired structure cannot be obtained.
【００１２】前記製造方法を更に具体的に説明すると、
例えばまず、真空溶融法、高周波溶融法等により、好ま
しくはるつぼ等を用いて、不活性ガス雰囲気下、希土類
金属−鉄−ボロン系合金を溶融物とした後、該溶融物
を、例えば、単ロール、双ロール又は円板上等におい
て、前記条件下、好ましくは連続的に凝固させる等のス
トリップキャスティング法を用いた方法等により、所望
の結晶組織を有する永久磁石用合金鋳塊２を得る。即
ち、ストリップキャスティング法等で凝固させる場合に
は、合金鋳塊の厚さを、好ましくは０．０５〜１５ｍｍ
の範囲となるように、鋳造温度及び注湯速度等を適宜選
択し、前記条件下処理するのが最も容易な方法である。The above-mentioned manufacturing method will be described more specifically.
For example, first, a rare earth metal-iron-boron-based alloy is melted under an inert gas atmosphere by a vacuum melting method, a high-frequency melting method, or the like, preferably using a crucible or the like. On a roll, a twin roll, a disk, or the like, the alloy ingot 2 for a permanent magnet having a desired crystal structure is obtained by a method using a strip casting method such as continuous solidification under the above conditions, preferably continuously. That is, when solidifying by a strip casting method or the like, the thickness of the alloy ingot is preferably 0.05 to 15 mm.
It is the easiest method to appropriately select the casting temperature, the pouring speed and the like so as to fall within the range described above, and to carry out the treatment under the above conditions.
【００１３】次いで、得られた永久磁石用合金鋳塊２
に、水素原子を侵入及び放出させ再結晶化させるため
に、例えば１〜１０ｍｍ角程度に粉砕し、好ましくは５
〜５０時間、９００〜１１００℃にて、均質化処理を行
った後、好ましくは１気圧の水素雰囲気中において、８
００〜８５０℃で２〜５時間保持し水素原子を侵入さ
せ、次いで１０-2〜１０-3Torrにまで急速脱気して水素
原子を放出させ、それにより再結晶化た後、急冷する水
素化処理を行う。次に再結晶化した前記永久磁石用合金
鋳塊を２００〜４００μｍまで粉砕する方法等により、
異方性永久磁石用粉末１を得ることができる。Next, the obtained alloy ingot for permanent magnet 2
In order to infiltrate and release hydrogen atoms and recrystallize, for example, pulverize to about 1 to 10 mm square, preferably 5 to 10 mm square.
After performing a homogenization treatment at 900 to 1100 ° C. for up to 50 hours, preferably in a hydrogen atmosphere of 1 atm.
The temperature is maintained at 00 to 850 ° C. for 2 to 5 hours to allow hydrogen atoms to penetrate, and then rapidly degassed to 10 −2 to 10 −3 Torr to release hydrogen atoms, thereby recrystallizing and then rapidly cooling hydrogen. Perform the conversion process. Next, by a method of grinding the recrystallized permanent magnet alloy ingot to 200 to 400 μm, etc.
Powder 1 for anisotropic permanent magnet can be obtained.
【００１４】前記異方性永久磁石用粉末１は、通常の磁
石製造法により、例えば樹脂磁石、ボンド磁石等とする
ことができる。The anisotropic permanent magnet powder 1 can be made into, for example, a resin magnet, a bonded magnet or the like by a usual magnet manufacturing method.
【００１５】[0015]
【発明の効果】本発明の希土類金属−鉄−ボロン系異方
性永久磁石用粉末は、高い異方性を示し、磁石特性が極
めて優れており、樹脂磁石、ボンド磁石等の永久磁石用
原料として有用である。Effect of the Invention rare earth metals of the present invention - iron - powder for boron-based anisotropic permanent magnet, high have shown anisotropic, magnetic properties are extremely good, the resin magnet, a permanent magnet such as bonded magnet Useful as a raw material.
【００１６】[0016]
【実施例】以下本発明を実施例及び比較例により更に詳
細に説明するが、本発明はこれらに限定されるものでは
ない。実施例１ ネオジム１４原子％、ボロン６原子％、鉄８０原子％か
らなる各金属元素を配合した合金を、アルゴンガス雰囲
気中で、アルミナるつぼを使用して高周波溶融法により
溶融物とした。次いで、得られた溶融物の温度を１３５
０℃に保持した後、図１に示す装置を用いて以下の方法
に従って永久磁石用合金鋳塊を得た。得られた合金鋳塊
を組織分析した結果を表１に示す。図１は、単ロールを
用いたストリップキャスト法により永久磁石用合金鋳塊
を製造するための概略図であって、１は前記高周波溶融
法により溶融した溶融物の入ったるつぼである。１３５
０℃に保持された溶融物２を、タンディッシュ３上に連
続的に流し込み、次いで約１ｍ／ｓで回転するロール４
上において、冷却速度５００℃／秒、過冷度２００℃の
冷却条件となるように急冷凝固させ、ロール４の回転方
向に連続的に溶融物２を落下させて、厚さ０．２〜０．
４ｍｍの合金鋳塊５を製造した。The present invention will be described in more detail with reference to examples and comparative examples, but the present invention is not limited to these examples. Example 1 An alloy containing 14 atomic% of neodymium, 6 atomic% of boron and 80 atomic% of iron was made into a melt by a high frequency melting method using an alumina crucible in an argon gas atmosphere. Next, the temperature of the obtained melt is set to 135.
After maintaining the temperature at 0 ° C., an alloy ingot for permanent magnet was obtained according to the following method using the apparatus shown in FIG. Table 1 shows the results of microstructure analysis of the obtained alloy ingot. FIG. 1 is a schematic view for manufacturing an alloy ingot for permanent magnets by a strip casting method using a single roll, and 1 is a crucible containing a melt melted by the high frequency melting method. 135
A melt 2 kept at 0 ° C. is continuously poured onto a tundish 3 and then rolls 4 rotating at about 1 m / s
Above, the solidified material is rapidly solidified under cooling conditions of a cooling rate of 500 ° C./second and a supercooling degree of 200 ° C., and the melt 2 is continuously dropped in the rotation direction of the roll 4 to have a thickness of 0.2 to 0. .
A 4 mm alloy ingot 5 was produced.
【００１７】得られた合金鋳塊５を５ｍｍ角に粉砕し、
１０００℃にて、４０時間均質化処理を行い、処理開始
前、処理開始後５、１０、１５、２０、４０時間のα−
Ｆｅの面積率を走査型電子顕微鏡による像から画像解析
により測定した。結果を表２に示す。また同走査型電子
顕微鏡により結晶粒径を測定したところ、１０時間均質
化処理を行った際の長軸方向の平均結晶粒径は６０μｍ
であった。次いで均質化処理を行った合金鋳塊を真空加
熱炉に入れ、１気圧の水素雰囲気中で８２０℃にて３時
間保持した後、２分以内に１０-2Torrまで脱気し、冷却
器に移し急冷した。処理後の合金鋳塊を容器から取り出
し、平均粒径３００μｍに粉砕し、１５ｋＯｅの磁場中
にて０．５ｔ／ｃｍ2の圧力をかけ、一軸圧縮により圧
粉体を成形した。該圧粉体の結晶配向度をＸ線回折によ
り測定し、上述の配向度を求める式により配向度Ｆを算
出し、さらに磁気特性を測定した。結晶配向度を表３
に、磁気特性を表４に示す。The obtained alloy ingot 5 is pulverized into 5 mm square,
The homogenization treatment was performed at 1000 ° C. for 40 hours, and before the start of the treatment and 5, 10, 15, 20, 40 hours after the start of the treatment,
The area ratio of Fe was measured by image analysis from an image by a scanning electron microscope. Table 2 shows the results. When the crystal grain size was measured by the same scanning electron microscope, the average crystal grain size in the long axis direction after homogenization treatment for 10 hours was 60 μm.
Met. Next, the homogenized alloy ingot is placed in a vacuum heating furnace, kept at 820 ° C. for 3 hours in a hydrogen atmosphere at 1 atm, and then degassed to 10 −2 Torr within 2 minutes. Transferred and quenched. The alloy ingot after the treatment was taken out of the container, pulverized to an average particle diameter of 300 μm, applied with a pressure of 0.5 t / cm 2 in a magnetic field of 15 kOe, and formed into a green compact by uniaxial compression. The degree of crystal orientation of the green compact was measured by X-ray diffraction, the degree of orientation F was calculated by the above-described equation for determining the degree of orientation, and the magnetic properties were further measured. Table 3 shows the degree of crystal orientation.
Table 4 shows the magnetic characteristics.
【００１８】比較例１ 実施例１で製造した合金溶融物を、高周波溶融法により
溶解し、金型鋳造法により厚さ２５ｍｍの永久磁石用合
金鋳塊を得た。得られた合金鋳塊を実施例１と同様に分
析した。合金鋳塊の分析結果を表１に示す。得られた合
金鋳塊を実施例１と同様に均質化処理を行い、α−Ｆｅ
の面積率を測定した。結果を表２に示す。また実施例１
と同様に１０時間均質化処理を行った際の結晶粒径を測
定したところ、長軸方向の平均結晶粒径は２２０μｍで
あった。次いで、実施例１と同様に水素化処理を行い、
粉砕し、得られた粉末の結晶配向度及び磁気特性を測定
した。結晶配向度を表３に、磁気特性を表４に示す。 Comparative Example 1 The alloy melt produced in Example 1 was melted by a high frequency melting method to obtain a 25 mm thick alloy ingot for permanent magnets by a die casting method. The obtained alloy ingot was analyzed in the same manner as in Example 1. Table 1 shows the analysis results of the alloy ingot. The obtained alloy ingot was homogenized in the same manner as in Example 1 to obtain α-Fe
Was measured. Table 2 shows the results. Example 1
When the crystal grain size after the homogenization treatment was performed for 10 hours in the same manner as in the above, the average crystal grain size in the major axis direction was 220 μm. Next, hydrogenation treatment was performed in the same manner as in Example 1,
The powder was pulverized and the degree of crystal orientation and magnetic properties of the obtained powder were measured. Table 3 shows the degree of crystal orientation, and Table 4 shows the magnetic properties.
【００１９】[0019]
【表１】 [Table 1]
【００２０】[0020]
【表２】 [Table 2]
【００２１】[0021]
【表３】 [Table 3]
【００２２】[0022]
【表４】 [Table 4]
【図１】実施例１で用いたストリップキャスト法により
永久磁石用合金鋳塊を製造する際の概略図である。FIG. 1 is a schematic view when producing an alloy ingot for a permanent magnet by a strip casting method used in Example 1.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ // Ｃ２２Ｃ 33/02 Ｈ０１Ｆ 1/06 Ａ 38/00 ３０３ 1/04 Ｈ (58)調査した分野(Int.Cl.7，ＤＢ名) H01F 1/032 - 1/08 B22F 1/00 C22C 33/02 C22C 38/00 303 ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 identification symbol FI // C22C 33/02 H01F 1/06 A 38/00 303 1/04 H (58) Fields surveyed (Int. Cl. 7 , (DB name) H01F 1/032-1/08 B22F 1/00 C22C 33/02 C22C 38/00 303
Claims (1)
らの配合割合が重量比で２５〜４０：０．５〜２．０：
残量であり、且つＸ線回折により測定した下記式で示さ
れる配向度Ｆの値が６０以上である粒径２００〜４００
μｍの希土類金属−鉄−ボロン系異方性永久磁石用粉
末。 【数１】 1. The method according to claim 1, comprising a rare earth metal, boron and iron.
The weight ratio of these compounds is 25 to 40: 0.5 to 2.0:
It is the remaining amount and is shown by the following equation measured by X-ray diffraction.
Particle size 200 to 400 in which the value of the degree of orientation F is 60 or more
μm rare earth metal-iron-boron based anisotropic permanent magnet powder. (Equation 1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000314786A JP3278431B2 (en) | 2000-10-16 | 2000-10-16 | Rare earth metal-iron-boron anisotropic permanent magnet powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000314786A JP3278431B2 (en) | 2000-10-16 | 2000-10-16 | Rare earth metal-iron-boron anisotropic permanent magnet powder |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23829992A Division JP3213638B2 (en) | 1992-02-15 | 1992-09-07 | Method for producing powder for rare earth metal-iron-boron based anisotropic permanent magnet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001176712A JP2001176712A (en) | 2001-06-29 |
| JP3278431B2 true JP3278431B2 (en) | 2002-04-30 |
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Families Citing this family (3)
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|---|---|---|---|---|
| US7550047B2 (en) | 2001-12-19 | 2009-06-23 | Hitachi Metals, Ltd. | Rare earth element-iron-boron alloy and magnetically anisotropic permanent magnet powder and method for production thereof |
| JP2010255098A (en) * | 2009-03-30 | 2010-11-11 | Tdk Corp | Rare earth alloy powder, method for producing the same, compound for anisotropic bond magnet, and anisotropic bond magnet |
| JP6488744B2 (en) * | 2015-02-10 | 2019-03-27 | Tdk株式会社 | R-T-B sintered magnet |
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