JPH10321452A - Heat resistant bonded magnet and manufacturing method thereof - Google Patents

Heat resistant bonded magnet and manufacturing method thereof

Info

Publication number
JPH10321452A
JPH10321452A JP10016211A JP1621198A JPH10321452A JP H10321452 A JPH10321452 A JP H10321452A JP 10016211 A JP10016211 A JP 10016211A JP 1621198 A JP1621198 A JP 1621198A JP H10321452 A JPH10321452 A JP H10321452A
Authority
JP
Japan
Prior art keywords
heat
resin
magnet
bonded magnet
magnet powder
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.)
Pending
Application number
JP10016211A
Other languages
Japanese (ja)
Inventor
Katsunori Iwasaki
克典 岩崎
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.)
Proterial Ltd
Original Assignee
Hitachi Metals 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 Hitachi Metals Ltd filed Critical Hitachi Metals Ltd
Priority to JP10016211A priority Critical patent/JPH10321452A/en
Publication of JPH10321452A publication Critical patent/JPH10321452A/en
Pending legal-status Critical Current

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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
    • H01F1/0555Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
    • H01F1/0558Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together bonded together

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

PROBLEM TO BE SOLVED: To improve heat resistance by conducting forming and main thermosetting treatment using generally two-layer structure compound obtained by mixing and then subjecting rare earth magnet powder and resin part to primary thermosetting treatment, by adding again and mixing resin part to the roughly milled mixture and subjecting the resultant mixture to secondary thermosetting treatment. SOLUTION: In a heat resistant bond magnet manufacturing method for binding rare earth magnet powder with a resin part mainly consisting of thermosetting resin such as epoxy resin, molding and main thermosetting treatment are conducted using a generally two-layer structure compound obtained by mixing and then subjecting the magnet powder and the resin part to primary thermosetting treatment at a temperature of 100 to 160 deg.C, next adding again and mixing resin part to the mixed material, subjecting the resultant mixture to secondary thermosetting treatment at a temperature of 80 to 150 deg.. As a result, it is possible to prevent oxidization without decreasing the density of the rare earth bond magnet and to provide good heat resistance and high magnetic characteristics.

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】本発明は希土類磁石粉末を熱
硬化性樹脂等で結着してなる耐熱型の希土類ボンド磁石
およびその製造方法に関し、さらにはR−T−B系やR
−T−B−Nb系の磁石粉末をエポキシ樹脂等で結着し
てなるボンド磁石の耐熱性の改良に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a heat-resistant rare-earth bonded magnet obtained by binding rare-earth magnet powder with a thermosetting resin or the like, and a method for producing the same.
The present invention relates to improvement in heat resistance of a bonded magnet formed by bonding -TB-Nb-based magnet powder with an epoxy resin or the like.

【0002】[0002]

【従来の技術】希土類元素(R)、FeまたはFeとC
o等の遷移金属(T)、ホウ素(B)からなるR−T−
B系永久磁石はコストパフォーマンスに優れかつ高磁気
特性を有するものとして注目を集めている。そのうち樹
脂との組み合わせで製造される等方性ボンド磁石はニア
ネット製品が量産可能な上、着磁方向が自由に選択でき
る等有利な点が多く、使い勝手に優れた磁石として幅広
い市場を確立しつつある。同ボンド磁石はパソコン市場
を中心に、将来的な自動車用、家電用等への展開が加速
し今後さらに重要度が増すと考えられる。R−T−B系
等方性ボンド磁石用の磁石粉末は超急冷法により得るこ
とができる。得られた急冷薄片を適当な温度で熱処理す
ることにより磁気特性を調整しボンド磁石用の粉末とす
る。ついで、この磁石粉末を表面処理した後、製品用途
に応じて最適と考えられる樹脂と適正比率で混合してコ
ンパウンド化し、以下公知の圧縮成形法、射出成型法等
によりボンド磁石の成形体を得、加熱硬化を行う。熱硬
化性樹脂としてエポキシ樹脂が代表的であるがエポキシ
樹脂は他の樹脂と同様にガラス転移温度以上で軟化ある
いは劣化するためおのずからエポキシ樹脂を用いた圧縮
成形によるR−T−B系ボンド磁石製品の用途は制限さ
れ、製品の耐熱信頼性を考慮した場合エポキシ樹脂を用
いたR−T−B系ボンド磁石は比較的耐熱条件の緩やか
な環境下(例えば耐熱温度約150℃以下)で多用され
ている。
2. Description of the Related Art Rare earth elements (R), Fe or Fe and C
R-T- composed of a transition metal (T) such as o and boron (B)
B-based permanent magnets have attracted attention as being excellent in cost performance and having high magnetic properties. Among them, isotropic bonded magnets manufactured in combination with resin have many advantages, such as mass production of near-net products and the ability to freely select the magnetization direction, and have established a wide market as easy-to-use magnets. It is getting. These bond magnets are expected to become increasingly important in the future for automobiles and home appliances mainly in the personal computer market, and their importance will increase in the future. The magnet powder for the RTB-based isotropic bonded magnet can be obtained by a super-quenching method. The resulting quenched flakes are heat-treated at an appropriate temperature to adjust the magnetic properties to obtain a powder for a bonded magnet. Then, after this magnet powder is surface-treated, it is mixed with a resin which is considered to be optimal according to the product application at an appropriate ratio to be compounded, and a molded body of a bonded magnet is obtained by a known compression molding method, injection molding method or the like. And heat curing. Epoxy resin is a typical thermosetting resin, but since epoxy resin softens or deteriorates at a temperature equal to or higher than the glass transition temperature like other resins, it is natural to use R-T-B bonded magnet products by compression molding using epoxy resin. The use of R-T-B bonded magnets made of epoxy resin is often used under relatively mild heat-resistant conditions (for example, a heat-resistant temperature of about 150 ° C or less) in consideration of the heat-resistant reliability of products. ing.

【0003】[0003]

【発明が解決しようとする課題】ボンド磁石の耐熱性は
重要であり、例えばパソコンのCD−ROM用スピンド
ルモータ用のボンド磁石は近年のCD−ROMの高速化
による高回転数でかつ発熱量の増加傾向にある環境にお
いて使用されるため従来よりも厳しい耐熱性が要求され
てきている。ボンド磁石を用いた製品に要求される耐熱
性の他に、ボンド磁石を対象製品に組み込む工程におい
て、例えば省力化のため組立工程内にリフロー半だとい
った自動化ラインが組み込まれることが多く、この半だ
槽は通常200℃付近まで温度が上昇し、この温度上昇
の影響を受けてボンド磁石が熱減磁する可能性がある。
よって、この熱減磁に耐える耐熱性が必要である。また
自動車用途ではエンジン回りで約180℃までの耐熱性
が要求される他、フロントパネル内の計器用のボンド磁
石では高温下での長期信頼性が重要である。このように
R−T−B系ボンド磁石に対して約180℃までの耐熱
性向上が広い分野で期待されており、その解決が急がれ
ていた。
The heat resistance of a bonded magnet is important. For example, a bonded magnet for a spindle motor for a CD-ROM of a personal computer has a high rotation speed and a low heat generation due to the recent increase in the speed of the CD-ROM. Since it is used in an environment where there is an increasing tendency, heat resistance that is stricter than before has been required. In addition to the heat resistance required for products using bonded magnets, in the process of incorporating bonded magnets into target products, automation lines such as reflow half are often incorporated in the assembly process to save labor, for example. The temperature of the bath usually rises to around 200 ° C., and the bond magnet may be thermally demagnetized under the influence of this rise in temperature.
Therefore, heat resistance to withstand this thermal demagnetization is required. In addition, heat resistance around 180 ° C. around the engine is required for automotive applications, and long-term reliability at high temperatures is important for bonded magnets for instruments in the front panel. As described above, improvement in heat resistance up to about 180 ° C. for an RTB-based bonded magnet is expected in a wide field, and the solution has been urgently needed.

【0004】ボンド磁石の耐熱化には幾つかの要素技術
が必要となる。磁石粉末では、圧縮成形時に発生する成
形体の割れによって新生面が露出し、露出した磁石粉末
が酸化する問題が最も大きい。磁石粉末の酸化によりボ
ンド磁石特性が劣化してしまう。この問題は磁石粉末を
予め所定の粒度に粉砕、調整することである程度抑制で
きる。しかし粉砕粒径を細かくしすぎるとかさ密度が小
さくなりボンド磁石成形体の密度低下を招来する。さら
に、磁石粉末と樹脂部との反応を抑制することが重要で
ある。すなわち、ボンド磁石の磁気特性を高くするには
高密度化する必要がある。このためのコンパウンドはボ
ンド磁石成形体の空隙を小さくするため樹脂部の硬化度
を調整することによって若干粘性を有した状態に作られ
る。しかし圧縮成形時の磁石粉末との接触、特に圧縮成
形時に発生する新生面との接触面で反応を起こし磁気特
性が低下する。加熱硬化を不活性ガス雰囲気中で行えば
磁石粉末の酸化および樹脂との反応の進行は抑えられる
ものの、ボンド磁石製品が大気中で使用される場合、い
ずれ反応あるいは酸化が進むことになる。逆にコンパウ
ンドの粘性を犠牲にして圧縮成形前にすでに硬度を高く
することにより新生面との接触を小さくすることも可能
であるが、この場合高温下での不可逆減磁率を小さくで
きる反面ボンド磁石の密度が低いため磁気特性は低下す
る。この問題はR−T−B系の等方性ボンド磁石のみな
らず、R−T−B系の異方性ボンド磁石や他の公知の希
土類磁石粉末を充填した等方性または異方性の希土類ボ
ンド磁石でも同様に存在する。このように従来において
は高い磁気特性を維持したまま耐熱性を兼ね備えること
は非常に困難であった。
[0004] Several elemental technologies are required to increase the heat resistance of bonded magnets. In the case of the magnet powder, the problem is that the new surface is exposed due to cracks of the compact generated during compression molding, and the exposed magnet powder is most oxidized. Oxidation of the magnet powder deteriorates the properties of the bonded magnet. This problem can be suppressed to some extent by grinding and adjusting the magnet powder to a predetermined particle size in advance. However, if the pulverized particle size is too fine, the bulk density becomes small and the density of the bonded magnet molded body is reduced. Further, it is important to suppress the reaction between the magnet powder and the resin part. That is, it is necessary to increase the density in order to enhance the magnetic properties of the bonded magnet. The compound for this purpose is made slightly viscous by adjusting the degree of curing of the resin portion in order to reduce the voids in the bonded magnet molding. However, a reaction occurs at the contact with the magnet powder at the time of the compression molding, particularly at the contact surface with the new surface generated at the time of the compression molding, and the magnetic characteristics are reduced. If the heat curing is performed in an inert gas atmosphere, the oxidation of the magnet powder and the progress of the reaction with the resin can be suppressed, but when the bonded magnet product is used in the atmosphere, the reaction or oxidation will eventually progress. Conversely, it is possible to reduce the contact with the new surface by increasing the hardness before compression molding at the expense of the viscosity of the compound, but in this case, the bond magnet can reduce the irreversible demagnetization rate at high temperatures. Due to the low density, the magnetic properties deteriorate. This problem is caused not only by the RTB-based isotropic bonded magnet, but also by an RTB-based anisotropic bonded magnet or an isotropic or anisotropic filled with other known rare earth magnet powders. Rare earth bonded magnets also exist. As described above, conventionally, it has been extremely difficult to provide heat resistance while maintaining high magnetic properties.

【0005】上記従来の問題を踏まえて、本発明の課題
は高い磁気特性を有しかつ耐熱性に優れた希土類ボンド
磁石、さらにはR−T−B系、R−T−B−Nb系の耐
熱ボンド磁石を安定かつ容易に得ることである。
[0005] In view of the above-mentioned conventional problems, an object of the present invention is to provide a rare earth bonded magnet having high magnetic properties and excellent heat resistance, as well as an RTB-based and RTB-Nb-based magnet. It is to obtain a heat-resistant bonded magnet stably and easily.

【0006】[0006]

【課題を解決するための手段】本発明者は希土類磁石粉
末(例えばR−T−B−Nb系磁石粉末等)を充填した
耐熱ボンド磁石に関し、圧縮成形前のコンパウンドの樹
脂部における内側の硬化度を進行させるとともに表面側
の樹脂部の粘性(硬化度)を低くした略2層樹脂部構造
とすることにより、ボンド磁石の成形体密度を低下させ
ることなく磁気特性を保持しかつ高い耐熱性を付与でき
ることを見出し本発明に想到した。すなわち、本発明
は、希土類磁石粉末をエポキシ樹脂等の熱硬化性樹脂を
主体とした樹脂部で結着する耐熱ボンド磁石の製造方法
において、前記の磁石粉末と樹脂部とを混練後100〜
160℃で1次加熱硬化処理を施し、次にこの混練物を
粗粉砕したものに再度前記樹脂部を追添加して混練後、
80〜150℃で2次加熱硬化処理を施して得られた略
2層構造のコンパウンドを用いて成形、本加熱硬化処理
を行う耐熱ボンド磁石の製造方法である。1次加熱硬化
処理温度を100〜160℃としたのは略2層構造のコ
ンパウンドの内側の樹脂部の硬化度をこの段階で進行さ
せるためである。また、粗粉砕後に樹脂部を追添加する
のは外周側を構成する樹脂部が1次加熱硬化処理を受け
ないようにするためである。1次、2次の加熱硬化処理
を行わないコンパウンドを用いて成形後、本加熱硬化さ
せてボンド磁石を製作すると、コンパウンドの樹脂部が
硬化し粘性が失われているためボンド磁石の密度が小さ
くなる。すなわちボンド磁石の空隙が多くなり磁気特性
および機械的強度が低くなる。密度を高くするため成形
圧力を高くすると圧縮成形中にコンパウンドが破壊し、
新生面が新たに露出するため酸化による影響を強く受け
ることになる。この不具合を踏まえて、本発明では1次
加熱硬化後のコンパウンドを粗粉砕した後、そのコンパ
ウンド粒子の表面を粘性の低い樹脂で覆うために再度前
記樹脂部を足して混練を行う。この混練後80〜150
℃で2次加熱硬化処理を施し、コンパウンド粒子の表面
を被覆した樹脂部を圧縮成形時に給粉が容易な粘度に調
整する。80℃未満では外周側樹脂部の硬化度が不十分
であり、150℃を越えると硬化が進行しすぎるためコ
ンパウンドを2層にした有効性が消失し、いずれもボン
ド磁石の密度が低下してしまうので好ましくない。
Means for Solving the Problems The present inventor relates to a heat-resistant bonded magnet filled with rare earth magnet powder (for example, RTB-Nb-based magnet powder, etc.), and hardens the inside of the resin portion of the compound before compression molding. The resin composition on the front side has a low viscosity (hardening degree) with a substantially two-layer resin structure to maintain the magnetic properties without decreasing the density of the molded body of the bonded magnet and to have high heat resistance. Have been found, and the present invention has been made. That is, the present invention relates to a method for manufacturing a heat-resistant bonded magnet in which a rare-earth magnet powder is bound by a resin portion mainly composed of a thermosetting resin such as an epoxy resin, wherein the magnet powder and the resin portion are kneaded at 100 to
A primary heat-curing treatment is performed at 160 ° C., and then the kneaded material is roughly added and then kneaded by additionally adding the resin portion to the roughly kneaded material.
This is a method for manufacturing a heat-resistant bonded magnet in which molding is performed using a compound having a substantially two-layer structure obtained by performing a secondary heat-curing treatment at 80 to 150 ° C., and the main heat-curing treatment is performed. The primary heat curing temperature is set to 100 to 160 ° C. in order to advance the degree of curing of the resin portion inside the compound having a substantially two-layer structure at this stage. The reason why the resin portion is additionally added after the coarse pulverization is to prevent the resin portion constituting the outer peripheral side from undergoing the primary heat curing treatment. After molding using a compound that does not perform primary and secondary heat-curing treatments, and then performing main heat-curing to produce a bonded magnet, the resin part of the compound is cured and the viscosity is lost. Become. That is, the voids of the bonded magnet increase, and the magnetic properties and mechanical strength decrease. If the molding pressure is increased to increase the density, the compound will break during compression molding,
Because the new surface is newly exposed, it is strongly affected by oxidation. In view of this problem, in the present invention, the compound after the first heat curing is coarsely pulverized, and then the resin portion is added again to cover the surface of the compound particles with a low-viscosity resin and kneading is performed. 80-150 after this kneading
A second heat-curing treatment is performed at a temperature of ° C. to adjust the viscosity of the resin portion coated on the surface of the compound particles to facilitate powder feeding during compression molding. If the temperature is lower than 80 ° C., the degree of curing of the outer peripheral resin portion is insufficient, and if the temperature exceeds 150 ° C., the curing proceeds too much, the effectiveness of the two-layered compound is lost, and the density of the bonded magnet decreases in any case. It is not preferable.

【0007】上記の1次加熱硬化処理、2次加熱硬化処
理、本加熱硬化処理のうちの少なくとも1工程、より好
ましくは全行程を10ppm〜大気中相当の酸素を含む
雰囲気中で行うと180℃までの不可逆減磁率を従来よ
り向上できるのでよい。すなわち、本発明によればコン
パウンド作製時の2回にわたる加熱硬化処理および圧縮
成形後の成形体の加熱硬化処理が10ppm以上の酸素
を含む雰囲気中(上限は大気中)で行われる時良好な耐
熱性が得られる。従来の加熱硬化処理は酸化の影響を阻
止するためアルゴンガス、窒素ガス、真空中等で行われ
るが、耐熱性を兼ね備えたボンド磁石を得ることを目的
とした本発明では、むしろ加熱硬化処理を酸素が適量存
在する状態下で行った方が長期の耐熱信頼性を得る上で
優れているとの結論を得た。加熱硬化雰囲気中の酸素量
が10ppm未満では室温におけるボンド磁石特性は高
いが、180℃の酸化性雰囲気に長時間さらされる環境
下では酸化の影響が大きく磁気特性および不可逆減磁率
の低下が著しい。
[0007] At least one of the above-mentioned primary heat-curing treatment, secondary heat-curing treatment, and main heat-curing treatment, more preferably, the entire process is performed at 180 ° C. in an atmosphere containing 10 ppm to a substantial amount of oxygen in air. The irreversible demagnetization rate up to this point can be improved as compared with the conventional case. That is, according to the present invention, good heat resistance is obtained when the heat curing treatment twice and the heat curing treatment of the compact after compression molding are performed in an atmosphere containing 10 ppm or more of oxygen (the upper limit is in the air). Property is obtained. The conventional heat-curing treatment is performed in an argon gas, a nitrogen gas, a vacuum, or the like in order to prevent the influence of oxidation.However, in the present invention, which is intended to obtain a bonded magnet having heat resistance, the heat-curing treatment is performed with oxygen. It was concluded that conducting in the presence of a suitable amount was more effective in obtaining long-term heat-resistant reliability. When the oxygen content in the heat-curing atmosphere is less than 10 ppm, the bonded magnet properties at room temperature are high, but under the environment exposed to an oxidizing atmosphere at 180 ° C. for a long time, the influence of oxidation is large and the magnetic properties and the irreversible demagnetization rate are significantly reduced.

【0008】また、本発明は、希土類磁石粉末を実質的
に液状グリシジルアミン型エポキシ樹脂と芳香族アミン
硬化剤との混合物からなる樹脂部で結着するとともに、
その樹脂部の総量が前記磁石粉末に対して0.1〜8重
量%である耐熱ボンド磁石である。本発明によれば、公
知の希土類磁石粉末を用いた場合に、良好な耐熱性と高
い磁気特性とが具備される。
Further, the present invention provides a method for binding a rare earth magnet powder with a resin portion substantially comprising a mixture of a liquid glycidylamine type epoxy resin and an aromatic amine curing agent,
A heat-resistant bonded magnet in which the total amount of the resin part is 0.1 to 8% by weight based on the magnet powder. ADVANTAGE OF THE INVENTION According to this invention, when a well-known rare earth magnet powder is used, good heat resistance and high magnetic characteristics are provided.

【0009】また、本発明は、R214Bを主相とする
R−T−B系合金(RはYを含めた希土類元素のうちの
1種または2種以上であり、例えばNd+DyまたはN
d+PrまたはNd+Dy+Prから構成することがで
きる。TはFeまたはFeとCo、Bはホウ素)からな
る磁石粉末を、実質的に液状グリシジルアミン型エポキ
シ樹脂と芳香族アミン硬化剤との混合物からなる樹脂部
で結着するとともに、その樹脂部の総量が前記磁石粉末
に対して0.1〜8重量%である耐熱ボンド磁石であ
る。前記磁石粉末は、組成が原子%表示でRu100-U-V
V(RはYを含めた希土類元素の1種または2種以
上、TはFeまたはFeおよびCo)で表され、u=8
〜17原子%、v=4〜8原子%にあることが好まし
い。uが8原子%未満ではαFeを生じてR214B主
相が不安定となり、17原子%を越えると飽和磁化が顕
著に低下する。よって、u=8〜17原子%が好まし
い。vが4原子%未満では固有保磁力(iHc)が顕著
に低下し、8原子%を越えると残留磁束密度(Br)が
顕著に低下する。よって、v=4〜8原子%が好まし
い。遷移金属Tに占めるCo置換量は30原子%以下が
好ましい。30原子%を越えるとキュリー点が向上する
が主相の磁気異方性定数が低下し、高いiHcを得るこ
とが困難である。
Further, the present invention relates to an R-T-B-based alloy containing R 2 T 14 B as a main phase (R is one or more of rare earth elements including Y, for example, Nd + Dy or N
It can be composed of d + Pr or Nd + Dy + Pr. T is a magnetic powder composed of Fe or Fe and Co, and B is boron) bound with a resin part substantially composed of a mixture of a liquid glycidylamine type epoxy resin and an aromatic amine curing agent. A heat-resistant bonded magnet having a total amount of 0.1 to 8% by weight based on the magnet powder. The magnet powder, R u T 100-UV composition in atomic percentages
B V (R is one or more rare earth elements including Y, T is Fe or Fe and Co), and u = 8
1717 atomic%, and v = 4-8 atomic%. When u is less than 8 atomic%, αFe is generated to make the R 2 T 14 B main phase unstable, and when it exceeds 17 atomic%, the saturation magnetization is significantly reduced. Therefore, u is preferably 8 to 17 atomic%. When v is less than 4 atomic%, the intrinsic coercive force (iHc) is significantly reduced, and when it exceeds 8 atomic%, the residual magnetic flux density (Br) is significantly reduced. Therefore, v is preferably 4 to 8 atomic%. The substitution amount of Co in the transition metal T is preferably 30 atomic% or less. If it exceeds 30 atomic%, the Curie point is improved, but the magnetic anisotropy constant of the main phase is reduced, and it is difficult to obtain a high iHc.

【0010】また、本発明は、原子%表示でRX
100-x-y-zyNbz(RはYを含めた希土類元素のうち
の1種または2種以上、TはFeまたはFeとCo、B
はホウ素、Nbはニオブである)で表され、x=8〜1
5、y=4〜8、z=0.1〜2の範囲にあるR−T−
B−Nb系磁石粉末を、実質的に液状グリシジルアミン
型エポキシ樹脂と芳香族アミン硬化剤との混合物からな
る樹脂部で結着するとともに、その樹脂部の総量が前記
磁石粉末に対して0.1〜8重量%である耐熱ボンド磁
石である。前記磁石粉末のRは8〜15原子%であるこ
とが好ましい。Rが8原子%未満ではα−Feを生じて
2Fe14B相が不安定となり、15原子%を越えると
飽和磁化が顕著に低下する。Nbは0.1原子%未満で
は結晶粒の粗大化抑制による耐熱性改善効果が認められ
ず、2.0原子%を越えると飽和磁化が顕著に低下す
る。Bは4原子%未満では高い固有保持力(iHc)を
得ることが困難である。8原子%を越えると残留磁束密
度(Br)が低下する。遷移金属Tに占めるCo置換量
は上記と同様に30原子%以下が好ましい。本発明のボ
ンド磁石は、Nb添加により耐熱性を向上したR−T−
B−Nb系磁石粉末を、特長ある樹脂部で結着してな
り、特に後述の不可逆減磁率を5%以下にできるという
特長を有している。
Further, the present invention relates to a method for preparing R X T
100-xyz B y Nb z (R is one or more of rare earth elements including Y, T is Fe or Fe and Co, B
Is boron and Nb is niobium), and x = 8 to 1
5, R-T- in the range of y = 4 to 8, z = 0.1 to 2
The B-Nb-based magnet powder is bound with a resin portion substantially composed of a mixture of a liquid glycidylamine-type epoxy resin and an aromatic amine curing agent, and the total amount of the resin portion is 0.1% with respect to the magnet powder. The heat-resistant bonded magnet is 1 to 8% by weight. It is preferable that R of the magnet powder is 8 to 15 atomic%. If R is less than 8 at%, α-Fe is generated to make the R 2 Fe 14 B phase unstable, and if it exceeds 15 at%, the saturation magnetization is significantly reduced. If Nb is less than 0.1 at%, the effect of improving the heat resistance by suppressing the coarsening of the crystal grains is not recognized, and if it exceeds 2.0 at%, the saturation magnetization is significantly reduced. If B is less than 4 atomic%, it is difficult to obtain a high intrinsic coercive force (iHc). If it exceeds 8 atomic%, the residual magnetic flux density (Br) decreases. The substitution amount of Co in the transition metal T is preferably 30 atomic% or less as described above. The bonded magnet of the present invention has an R-T-
The B-Nb-based magnet powder is bound by a characteristic resin portion, and has a feature that the irreversible demagnetization rate described later can be reduced to 5% or less.

【0011】従来の粉末状エポキシ樹脂ではガラス転移
温度が高々150℃付近であるのを踏まえて本発明者が
種々の液状エポキシ樹脂を用いて鋭意検討した結果、混
練および硬化度のコントロールの容易さ等で最も優れて
おり、ガラス転移温度がR−T−B−Nb系磁石粉末の
キュリー温度より低くかつ結着樹脂分として十分に高い
240〜250℃である液状グリシジルアミン型エポキ
シ樹脂と芳香族アミン硬化剤との混合物からなる樹脂部
を採用することが耐熱性の改良に有効であることを知見
した。そして、その樹脂部の総量が前記磁石粉末に対し
て0.1〜8重量%である場合に実用に供し得る180
℃までの良好な耐熱性と高い磁気特性が得られることを
見出した。樹脂部の総樹脂量が0.1重量%未満ではコ
ンパウンド化が困難であり、8重量%を越えるとボンド
磁石の密度が顕著に低下する。なお、液状グリシジルア
ミン型エポキシ樹脂と芳香族アミン硬化剤との混合比率
は所望の硬化度を考慮して適宜選択することができる。
Based on the fact that the glass transition temperature of the conventional powdery epoxy resin is at most around 150 ° C., the present inventors have conducted extensive studies using various liquid epoxy resins, and have found that the kneading and the control of the degree of curing are easy. A liquid glycidylamine type epoxy resin having a glass transition temperature of 240 to 250 ° C. lower than the Curie temperature of the RTB-Nb-based magnet powder and sufficiently high as a binder resin component; It has been found that the use of a resin part composed of a mixture with an amine curing agent is effective for improving heat resistance. And, when the total amount of the resin part is 0.1 to 8% by weight based on the magnet powder, 180 can be provided for practical use.
It has been found that good heat resistance up to ℃ and high magnetic properties can be obtained. If the total resin content of the resin part is less than 0.1% by weight, compounding is difficult, and if it exceeds 8% by weight, the density of the bonded magnet is significantly reduced. The mixing ratio of the liquid glycidylamine type epoxy resin and the aromatic amine curing agent can be appropriately selected in consideration of a desired degree of curing.

【0012】本発明の耐熱ボンド磁石は、圧縮成形前の
コンパウンドにおいて上記磁石粉末を結着する樹脂部よ
りも硬化度の低い樹脂部が表面を覆った略2層構造とな
っているので、圧縮成形を経て得られるボンド磁石が実
用に供し得るに十分な密度を保持し、同時に上記磁石粉
末の酸化進行を抑えられて高い磁気特性を保持した耐熱
ボンド磁石である。略2層構造のコンパウンドは内側が
硬く、外周側が粘性に富んでいる(内側の樹脂部に比べ
て硬化度が低い)ためボンド磁石成形時に密度を高くす
ることが可能となる。最終的にパーミアンス係数2の形
状にされたボンド磁石を室温で50kOeのパルス磁場
で着磁後、20℃で磁束量を測定し、続いて大気中にお
いて180℃で1000時間の条件で放置後20℃に戻
した場合の磁束量を測定し、評価した不可逆減磁率が5
%以下であり良好な耐熱性を有している。また、本発明
の耐熱ボンド磁石の密度は5.0g/cc以上であり、
かつ20℃で測定した最大エネルギー積で5MGOe以
上を実現している。
The heat-resistant bonded magnet of the present invention has a substantially two-layer structure in which a resin portion having a lower degree of curing than the resin portion binding the magnet powder in the compound before compression molding covers the surface. This is a heat-resistant bonded magnet which has a density sufficient for a bonded magnet obtained through molding to be practically used, and at the same time, suppresses the progress of oxidation of the magnet powder and maintains high magnetic properties. Since the inside of the compound having a substantially two-layer structure is hard on the inner side and rich on the outer peripheral side (the degree of hardening is lower than that of the resin part on the inner side), it is possible to increase the density at the time of molding the bonded magnet. Finally, the magnetized bond magnet having a permeance coefficient of 2 was magnetized at room temperature with a pulsed magnetic field of 50 kOe, and the amount of magnetic flux was measured at 20 ° C. The irreversible demagnetization rate was evaluated by measuring the amount of magnetic flux when the temperature returned to
% Or less, and has good heat resistance. Further, the density of the heat-resistant bonded magnet of the present invention is 5.0 g / cc or more,
In addition, the maximum energy product measured at 20 ° C. achieves 5 MGOe or more.

【0013】[0013]

【発明の実施の形態】以下、実施例により本発明を説明
する。 (実施例1〜3)ボンド磁石粉末として原子%表示でN
11.5Fe80.76Nb1.8の組成のMQI(マグネクエ
ンチインターナショナル)製のMQP−O材を用い、バ
ンタムミルにて平均粒径110μmに粉砕した。粉砕前
のMQP−O材は超急冷法、粉砕、熱処理を経て平均結
晶粒径が0.01〜0.5μmの、実用に耐える高い保
磁力を有した磁石粉末である。バンタムミルによる前記
磁石粉末の粉砕粒径は1〜1000μmの範囲で適宜選
択できる。この粉砕粉に対して日本ユニカー(株)製シ
ランカップリング材を0.25重量%相当分添加し表面
処理を施した。次いで、油化シェル(株)製液状グリシ
ジルアミン型エポキシ樹脂(E630)と芳香族アミン
硬化剤であるDDS(ジアミノジフェニルスルフォン)
とからなる樹脂部混合物(重量比でE630:DDS=
100:43.2)を総量で前記表面処理粉末対比で
2.6重量%相当になるよう秤量し、その樹脂部混合物
を2回にわけて前記磁石粉末または混練物に添加して混
合後二軸混練機で混練する。まず、1回目の混練で樹脂
部総量のうちの80重量%分を前記磁石粉末と混練し、
得られた混練物に表1の条件で1次加熱硬化処理を行っ
た。表1の1次硬化、2次硬化は1次加熱硬化処理、2
次加熱硬化処理を表わしている。続いて、2回目の混練
時に樹脂部総量の残り20重量%分を添加し混練後、2
次加熱硬化処理を行い、次いで所定の成形金型において
磁場なしで圧縮成形した。得られた等方性のボンド磁石
成形体に本加熱硬化処理(大気中で180℃×1時間保
持後、190℃×4時間保持し、室温まで冷却する処
理)を行い本発明の耐熱ボンド磁石を得た。このボンド
磁石の密度、20℃における磁気特性、同ボンド磁石を
パーミアンス係数2(厚み/直径=0.7)の円柱形状
の試料に仕上げた後不可逆減磁率(α)を測定した。不
可逆減磁率(α)は、室温で試料を50kOeのパルス
磁場で着磁後20℃において測定した初期磁束量と、引
き続いて試料を大気中で180℃×1000時間加熱後
20℃まで冷却して測定した磁束量とから求めた磁束量
変化率であり、下記式により算出した。不可逆減磁率
(α)=(20℃における初期磁束量−大気中180℃
×1000時間加熱後20℃に戻した試料の磁束量)÷
(20℃における初期磁束量)×100(%)。これら
の結果を表1に示した。なお、下記の各実施例、各比較
例における磁気特性、密度、不可逆減磁率(α)は実施
例1と同様にして評価した。
DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below with reference to examples. (Examples 1 to 3) N in atomic% as bonded magnet powder
with d 11.5 Fe 80.7 B 6 MQI composition of Nb 1.8 (magnetic quenching International) made of MQP-O material was ground to an average particle size of 110μm at a bantam mill. The MQP-O material before pulverization is a magnet powder having an average crystal grain size of 0.01 to 0.5 μm having a high coercive force that can withstand practical use after being subjected to a super-quenching method, pulverization and heat treatment. The crushed particle size of the magnet powder by a bantam mill can be appropriately selected in the range of 1 to 1000 μm. To this pulverized powder, a silane coupling material manufactured by Nippon Unicar Co., Ltd. was added in an amount corresponding to 0.25% by weight to perform a surface treatment. Next, a liquid glycidylamine type epoxy resin (E630) manufactured by Yuka Shell Co., Ltd. and DDS (diaminodiphenylsulfone) as an aromatic amine curing agent
(A weight ratio of E630: DDS =
100: 43.2) was weighed so that the total amount was equivalent to 2.6% by weight relative to the surface-treated powder, and the resin mixture was divided into two portions and added to the magnetic powder or the kneaded material. Knead with a shaft kneader. First, in the first kneading, 80% by weight of the total resin part is kneaded with the magnet powder,
The obtained kneaded material was subjected to a primary heat curing treatment under the conditions shown in Table 1. The primary curing and the secondary curing in Table 1 are primary heat curing treatments,
This represents the next heat curing treatment. Subsequently, at the time of the second kneading, the remaining 20% by weight of the total amount of the resin part was added and kneaded.
Next, a heat curing treatment was performed, and then compression molding was performed without a magnetic field in a predetermined molding die. The obtained isotropic bonded magnet molded body is subjected to a main heat-curing treatment (a process of holding at 180 ° C. × 1 hour in the air, holding at 190 ° C. × 4 hours, and cooling to room temperature), and performing the heat-resistant bonded magnet of the present invention. I got The density of the bonded magnet, the magnetic properties at 20 ° C., and the irreversible demagnetization rate (α) were measured after finishing the bonded magnet into a cylindrical sample having a permeance coefficient of 2 (thickness / diameter = 0.7). The irreversible demagnetization rate (α) is determined by measuring the initial magnetic flux measured at 20 ° C. after magnetizing the sample with a pulse magnetic field of 50 kOe at room temperature, and subsequently cooling the sample to 180 ° C. × 1000 hours in the atmosphere and cooling to 20 ° C. It is a magnetic flux amount change rate obtained from the measured magnetic flux amount, and was calculated by the following equation. Irreversible demagnetization rate (α) = (initial magnetic flux at 20 ° C-180 ° C in air)
× The amount of magnetic flux of the sample returned to 20 ° C. after heating for 1000 hours) ÷
(Initial magnetic flux at 20 ° C.) × 100 (%). The results are shown in Table 1. The magnetic properties, density, and irreversible demagnetization rate (α) in each of the following examples and comparative examples were evaluated in the same manner as in Example 1.

【0014】(比較例1〜5)上記実施例と同様の表面
処理磁石粉末を用い、油化シェル(株)製液状グリシジ
ルアミン型エポキシ樹脂(E630)と芳香族アミン硬
化剤であるDDS(ジアミノジフェニルスルフォン)を
総量で磁石粉末対比で2.6重量%相当(重量比でE6
30:DDS=100:43.2)になるよう秤量し、
二軸混練機で一回のみ混練した。混練後表1に示す1次
加熱硬化処理のみを行った。得られた混練物を用いてそ
のまま所定の金型に磁場なしで圧縮成形し等方性のボン
ド磁石成形体を得た。以降は実施例1と同様にして本加
熱硬化処理を行い、各特性を評価した結果を表1に示
す。 (比較例6)2次加熱硬化処理を160℃×1時間とし
た以外は実施例1と同様にして本加熱硬化処理までを行
い等方性のボンド磁石を得た。このものの各特性を評価
した結果を表1に併記した。
Comparative Examples 1 to 5 A liquid glycidylamine type epoxy resin (E630) manufactured by Yuka Shell Co., Ltd. and a DDS (diamino) Diphenylsulfone) in a total amount of 2.6% by weight relative to the magnet powder (E6 in weight ratio).
30: DDS = 100: 43.2)
It was kneaded only once with a twin-screw kneader. After kneading, only the primary heat curing treatment shown in Table 1 was performed. The obtained kneaded product was directly compression-molded into a predetermined mold without a magnetic field to obtain an isotropic bonded magnet molded product. Thereafter, the main heat-curing treatment was performed in the same manner as in Example 1, and the results of evaluating each characteristic are shown in Table 1. (Comparative Example 6) The same process as in Example 1 was performed except that the secondary heat curing treatment was performed at 160 ° C for 1 hour to obtain an isotropic bonded magnet. Table 1 also shows the results of evaluating the properties of this product.

【0015】[0015]

【表1】 [Table 1]

【0016】表1より、2回の混練および1次と2次の
加熱硬化処理を行った実施例1〜3のものではαが5%
以下であり、最大エネルギー積(BH)max も6MG
Oeを越えている。これに対し、比較例1〜3では1次
加熱硬化処理温度が低いため樹脂部の硬化が遅く、密度
およびBrが高くなり最大エネルギー積が8MGOeを
上回っている。しかし、実施例1〜3に比べてiHcが
やや低く、特にαが大きい。これは本加熱硬化時に樹脂
部と磁石粉末が反応したためと考えられる。また、比較
例4、5では高iHcが得られておりαも5%以下にで
きているが、密度が低く最大エネルギー積は5MGOe
を下回っている。また、2次加熱硬化処理温度が150
℃を越えている比較例6の場合は硬化が進行しすぎてボ
ンド磁石に隙間が多く生じ、ボンド磁石の密度が低下し
ていた。
As shown in Table 1, in Examples 1 to 3 in which kneading was performed twice and primary and secondary heat curing treatments were performed, α was 5%.
And the maximum energy product (BH) max is also 6MG
Oe is exceeded. On the other hand, in Comparative Examples 1 to 3, the primary heat curing treatment temperature was low, so that the curing of the resin portion was slow, the density and Br were increased, and the maximum energy product exceeded 8 MGOe. However, iHc is slightly lower than in Examples 1 to 3, and α is particularly large. This is probably because the resin portion and the magnet powder reacted during the main heat curing. Further, in Comparative Examples 4 and 5, high iHc was obtained and α was made 5% or less, but the density was low and the maximum energy product was 5MGOe.
Is below. In addition, the secondary heat curing temperature is 150
In the case of Comparative Example 6 in which the temperature was higher than 0 ° C., the curing was excessively progressed and many gaps were formed in the bonded magnet, and the density of the bonded magnet was lowered.

【0017】液状グリシジルアミン型エポキシ樹脂と芳
香族アミン硬化剤との混合物からなる総樹脂部量の変化
による磁気特性および不可逆減磁率の変化を検討した結
果を次に説明する。 (実施例4〜7、比較例7)表2に示すように樹脂部の
総量を変更するとともに2次加熱硬化処理を115℃×
1時間とした以外は実施例1と同様にしてボンド磁石を
作成し、評価した。
The results of examining the change in magnetic properties and irreversible demagnetization rate due to the change in the total amount of resin composed of a mixture of a liquid glycidylamine type epoxy resin and an aromatic amine curing agent will be described below. (Examples 4 to 7, Comparative Example 7) As shown in Table 2, the total amount of the resin portion was changed and the second heat curing treatment was performed at 115 ° C. ×
A bonded magnet was prepared and evaluated in the same manner as in Example 1 except that the time was changed to 1 hour.

【0018】[0018]

【表2】 [Table 2]

【0019】表2より、実施例4〜7では樹脂部総量の
増加にともないボンド磁石に占める磁石粉末の比率が低
下するため徐々に密度および磁気特性が低下しているが
比較例7に比べて大きく、αは上記実施例1〜3と同様
に良好である。なお、樹脂部総量の下限値は0.1重量
%以上であれば実用に供することが可能である。
From Table 2, it can be seen that in Examples 4 to 7, the density and magnetic properties gradually decreased because the proportion of the magnet powder in the bonded magnet decreased with the increase in the total amount of the resin part. Α is as good as in Examples 1 to 3 above. In addition, if the lower limit of the total amount of the resin part is 0.1% by weight or more, the resin can be practically used.

【0020】次に、本加熱硬化雰囲気による影響を検討
した結果について説明する。 (実施例8〜9、比較例8〜10)本加熱硬化処理直前
までの製造工程は実施例5と同様にして作成したボンド
磁石成形体を準備した。次に、本加熱硬化時の雰囲気の
みを大気中(実施例8)、酸素含有量50ppmのアル
ゴンガス中(実施例9)、酸素含有量10ppm未満の
真空中(比較例8)とアルゴンガス中(比較例9)と窒
素ガス中(比較例10)として各々180℃×1時間、
続いて190℃×4時間の加熱保持後室温まで冷却する
本加熱硬化処理を行った。結果を表3に示した。
Next, the result of examining the effect of the heat-curing atmosphere will be described. (Examples 8 to 9 and Comparative Examples 8 to 10) A bonded magnet molded body prepared in the same manner as in Example 5 except for the manufacturing process immediately before the main heat curing treatment was prepared. Next, only the atmosphere at the time of the main heating and curing was in the air (Example 8), in an argon gas having an oxygen content of 50 ppm (Example 9), in a vacuum having an oxygen content of less than 10 ppm (Comparative Example 8), and in an argon gas. (Comparative Example 9) and 180 ° C. × 1 hour in nitrogen gas (Comparative Example 10)
Subsequently, a main heat curing treatment of cooling to room temperature after heating and holding at 190 ° C. × 4 hours was performed. The results are shown in Table 3.

【0021】[0021]

【表3】 [Table 3]

【0022】表3より、20℃では比較例8〜10のも
のが実施例8、9よりもやや高い磁気特性となってい
る。しかし、αは実施例8、9のものが比較例8〜10
の約半分であり、本発明のボンド磁石が良好な耐熱性を
有していることがわかる。つまり10ppm未満の酸素
を含んだ真空中、アルゴン中、または窒素ガス中で本加
熱硬化処理を行うと室温における磁気特性は高いが、大
気中で長時間高温にさらされるような酸化を強力にうけ
る環境下において酸化されて磁気特性の劣化が早くなる
ことを示している。なお、本加熱硬化雰囲気の酸素含有
量が10ppm以上であれば、実施例8、9のものと略
同様の結果を得ることが可能である。また本発明の耐熱
ボンド磁石は、1次加熱硬化処理と2次加熱硬化処理と
本加熱硬化処理のうちの少なくとも1工程を酸素含有量
の下限が10ppm以上から上限は大気中相当の酸素含
有量雰囲気とすることで得ることが可能である。
From Table 3, at 20 ° C., those of Comparative Examples 8 to 10 have slightly higher magnetic characteristics than those of Examples 8 and 9. However, α was determined in Examples 8 and 9 in Comparative Examples 8 to 10.
This indicates that the bonded magnet of the present invention has good heat resistance. In other words, when the main heat-curing treatment is performed in a vacuum containing less than 10 ppm of oxygen, in argon, or in a nitrogen gas, the magnetic properties at room temperature are high, but oxidization that is exposed to a high temperature for a long time in the air is strongly received. This indicates that the magnetic properties are oxidized under the environment and the magnetic properties are rapidly deteriorated. When the oxygen content of the main heat-curing atmosphere is 10 ppm or more, substantially the same results as those of Examples 8 and 9 can be obtained. In the heat-resistant bonded magnet of the present invention, the lower limit of the oxygen content of at least one of the first heat-curing treatment, the second heat-curing treatment and the main heat-curing treatment is from 10 ppm or more to the upper limit is the oxygen content equivalent to the atmosphere. It can be obtained by setting the atmosphere.

【0023】次に、図1に本発明の耐熱ボンド磁石用の
理想的なコンパウンドの要部断面構造を模式的に示し
た。上記磁石粉末を1層目の樹脂部が結着して内側のコ
ンパウンドを構成しているとともに、外周側を2層目の
樹脂部が覆った略2層構造となっている。この構造を有
したコンパウンドにより、上記の通り、180℃までの
良好な耐熱性と高い磁気特性を有した耐熱ボンド磁石が
得られる。
Next, FIG. 1 schematically shows a cross-sectional structure of a principal part of an ideal compound for a heat-resistant bonded magnet of the present invention. The magnet powder is bonded to a first-layer resin portion to form an inner compound, and has a substantially two-layer structure in which an outer peripheral side is covered by a second-layer resin portion. By using the compound having this structure, a heat-resistant bonded magnet having good heat resistance up to 180 ° C. and high magnetic properties can be obtained as described above.

【0024】上記実施例では等方性のR−T−B−Nb
系磁石粉末を充填した希土類ボンド磁石を記載したが、
等方性または異方性のR−T−B系磁石粉末を充填した
希土類ボンド磁石、異方性のR−T−B−Nb系磁石粉
末を充填した希土類ボンド磁石においても上記と同様の
効果が期待できる。さらにはこれらの磁石粉末は超急冷
法を用いて作製されたもののみならず、HDDR法を用
いて作製された平均の再結晶粒径が0.01〜0.5μ
mでかつ磁石粉末の平均粒径が1〜1000μmのもの
を用い得る。さらには、他の公知の希土類磁石粉末を充
填した希土類ボンド磁石においても上記と同様の効果が
期待される。具体的には、SmCo5磁石粉末、Sm2
17磁石粉末(TM=Co+Fe+Cu+ZrまたはC
o+Fe+Cu+Hf)、ThMn12型化合物の構造を
有したNd(+Pr)−Fe−N系磁石合金粉末、Th
2Zn17型化合物および/またはTbCu7型化合物の構
造を有したSm−Fe−N系磁石合金粉末、交換スプリ
ング磁石粉末等が挙げられる。
In the above embodiment, the isotropic RTB-Nb
Rare earth bonded magnet filled with system magnet powder is described,
The same effect can be obtained in a rare-earth bonded magnet filled with isotropic or anisotropic RTB-based magnet powder and a rare-earth bonded magnet filled with anisotropic RTB-Nb-based magnet powder. Can be expected. Furthermore, these magnet powders are not only manufactured using the super-quenching method, but also have an average recrystallized particle size manufactured using the HDDR method of 0.01 to 0.5 μm.
m and the average particle size of the magnet powder is 1 to 1000 μm. Furthermore, the same effects as described above are expected for rare-earth bonded magnets filled with other known rare-earth magnet powders. Specifically, SmCo 5 magnet powder, Sm 2 T
M 17 magnet powder (TM = Co + Fe + Cu + Zr or C
o + Fe + Cu + Hf), Nd (+ Pr) -Fe-N magnet alloy powder having a structure of ThMn 12 type compound, Th
Examples include Sm-Fe-N-based magnet alloy powder and exchange spring magnet powder having a structure of 2 Zn 17 type compound and / or TbCu 7 type compound.

【0025】[0025]

【発明の効果】本発明によれば、希土類ボンド磁石の成
形原料であるコンパウンドを略2層構造にすることによ
り、希土類ボンド磁石の密度を低下させることなく酸化
進行を抑え、180℃までの良好な耐熱性と高い磁気特
性を有した耐熱型の希土類ボンド磁石およびその製造方
法を実現することができる。
According to the present invention, the compound, which is a raw material for forming a rare-earth bonded magnet, has a substantially two-layer structure, so that the oxidation can be suppressed without lowering the density of the rare-earth bonded magnet, and the temperature up to 180.degree. A heat resistant rare earth bonded magnet having excellent heat resistance and high magnetic properties and a method for manufacturing the same can be realized.

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

【図1】本発明の耐熱ボンド磁石の成形原料であるコン
パウンドの要部断面模式図である。
FIG. 1 is a schematic cross-sectional view of a main part of a compound which is a raw material for forming a heat-resistant bonded magnet of the present invention.

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 FI // C22C 38/00 303 H01F 1/08 A ──────────────────────────────────────────────────の Continued on front page (51) Int.Cl. 6 Identification code FI // C22C 38/00 303 H01F 1/08 A

Claims (7)

【特許請求の範囲】[Claims] 【請求項1】 希土類磁石粉末を熱硬化性樹脂を主体と
した樹脂部で結着してなる耐熱ボンド磁石の製造方法に
おいて、 前記の磁石粉末と樹脂部とを混練後1次加熱硬化処理を
施し、次にこの混練物を粗粉砕したものに再度前記樹脂
部を追添加して混練後、この混練物に2次加熱硬化処理
を施して得られた略2層構造のコンパウンドを用いて成
形、本加熱硬化処理を行うことを特徴とする耐熱ボンド
磁石の製造方法。
1. A method for manufacturing a heat-resistant bonded magnet comprising a rare-earth magnet powder bound by a resin portion mainly composed of a thermosetting resin, comprising: kneading the magnet powder and a resin portion; The kneaded product is then roughly pulverized, and the above resin portion is again added thereto and kneaded. Then, the kneaded product is subjected to a second heat-curing treatment, and molded using a compound having a substantially two-layer structure. And a method for producing a heat-resistant bonded magnet, which comprises performing a main heat curing treatment.
【請求項2】 請求項1において、1次加熱硬化処理、
2次加熱硬化処理、本加熱硬化処理のうちの少なくとも
1工程を10ppm〜大気中相当の酸素を含む雰囲気中
で行う耐熱ボンド磁石の製造方法。
2. The method according to claim 1, wherein the first heat curing treatment is performed.
A method for producing a heat-resistant bonded magnet, wherein at least one of the secondary heat-curing treatment and the main heat-curing treatment is performed in an atmosphere containing 10 ppm to a substantial amount of oxygen in the atmosphere.
【請求項3】 請求項1または2において、1次加熱硬
化処理を100〜160℃、2次加熱硬化処理温度を8
0〜150℃で行う耐熱ボンド磁石の製造方法。
3. The method according to claim 1, wherein the first heat-curing treatment is performed at 100 to 160 ° C., and the second heat-curing treatment is performed at a temperature of 8 ° C.
A method for producing a heat-resistant bonded magnet performed at 0 to 150 ° C.
【請求項4】 希土類磁石粉末を実質的に液状グリシジ
ルアミン型エポキシ樹脂と芳香族アミン硬化剤との混合
物からなる樹脂部で結着するとともに、その樹脂部の総
量が前記磁石粉末に対して0.1〜8重量%であること
を特徴とする耐熱ボンド磁石。
4. The rare earth magnet powder is bound by a resin portion substantially composed of a mixture of a liquid glycidylamine type epoxy resin and an aromatic amine curing agent, and the total amount of the resin portion is 0 to the magnet powder. 0.1 to 8% by weight.
【請求項5】 R214Bを主相とするR−T−B系合
金(RはYを含めた希土類元素のうちの1種または2種
以上、TはFeまたはFeとCo、Bはホウ素)からな
る磁石粉末を、実質的に液状グリシジルアミン型エポキ
シ樹脂と芳香族アミン硬化剤との混合物からなる樹脂部
で結着するとともに、その樹脂部の総量が前記磁石粉末
に対して0.1〜8重量%であることを特徴とする耐熱
ボンド磁石。
5. An RTB-based alloy having R 2 T 14 B as a main phase (R is one or more of rare earth elements including Y, T is Fe or Fe and Co, B Is bonded with a resin part substantially consisting of a mixture of a liquid glycidylamine type epoxy resin and an aromatic amine curing agent, and the total amount of the resin part is 0 to the magnet powder. 0.1 to 8% by weight.
【請求項6】 原子%表示でRX100-X-y-zyNb
z(RはYを含めた希土類元素のうちの1種または2種
以上、TはFeまたはFeとCo、Bはホウ素、Nbは
ニオブである)で表され、x=8〜15、y=4〜8、
z=0.1〜2の範囲にあるR−T−B−Nb系磁石粉
末を、実質的に液状グリシジルアミン型エポキシ樹脂と
芳香族アミン硬化剤との混合物からなる樹脂部で結着す
るとともに、その樹脂部の総量が前記磁石粉末に対して
0.1〜8重量%であることを特徴とする耐熱ボンド磁
石。
In 6. atomic percentages R X T 100-Xyz B y Nb
z (R is one or more of the rare earth elements including Y, T is Fe or Fe and Co, B is boron, Nb is niobium), x = 8 to 15, y = 4-8,
The RTB-Nb-based magnet powder in the range of z = 0.1 to 2 is bound with a resin part substantially consisting of a mixture of a liquid glycidylamine type epoxy resin and an aromatic amine curing agent. A heat-resistant bonded magnet, wherein the total amount of the resin part is 0.1 to 8% by weight based on the magnet powder.
【請求項7】 希土類磁石粉末を熱硬化性樹脂を主体と
した樹脂部で結着してなる耐熱ボンド磁石であって、2
0℃における最大エネルギー積が5MGOe以上、密度
が5.0g/cc以上であるとともに、パーミアンス係
数2に形成した前記耐熱ボンド磁石を50kOeのパル
ス磁場で着磁後、続いて大気中において180℃で10
00時間保持後20℃に戻した場合の不可逆減磁率が5
%以下であることを特徴とする耐熱ボンド磁石。
7. A heat-resistant bonded magnet comprising a rare earth magnet powder bound by a resin portion mainly composed of a thermosetting resin,
The maximum energy product at 0 ° C. is 5 MGOe or more, the density is 5.0 g / cc or more, and the heat-resistant bonded magnet formed to have a permeance coefficient of 2 is magnetized with a pulse magnetic field of 50 kOe. 10
Irreversible demagnetization rate when returning to 20 ° C after holding for 00 hours is 5
% Or less.
JP10016211A 1997-03-18 1998-01-28 Heat resistant bonded magnet and manufacturing method thereof Pending JPH10321452A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10016211A JPH10321452A (en) 1997-03-18 1998-01-28 Heat resistant bonded magnet and manufacturing method thereof

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP6476397 1997-03-18
JP9-64763 1997-03-18
JP10016211A JPH10321452A (en) 1997-03-18 1998-01-28 Heat resistant bonded magnet and manufacturing method thereof

Publications (1)

Publication Number Publication Date
JPH10321452A true JPH10321452A (en) 1998-12-04

Family

ID=26352484

Family Applications (1)

Application Number Title Priority Date Filing Date
JP10016211A Pending JPH10321452A (en) 1997-03-18 1998-01-28 Heat resistant bonded magnet and manufacturing method thereof

Country Status (1)

Country Link
JP (1) JPH10321452A (en)

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WO2020003692A1 (en) * 2018-06-26 2020-01-02 信越化学工業株式会社 Method of manufacturing negative electrode active material for nonaqueous electrolyte secondary battery
US11944946B2 (en) 2013-06-28 2024-04-02 Saint-Gobain Performance Plastics Corporation Mixing assemblies including magnetic impellers

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016523704A (en) * 2013-06-28 2016-08-12 サン−ゴバン パフォーマンス プラスティックス コーポレイション Mixing assembly including magnetic impeller
US9815035B2 (en) 2013-06-28 2017-11-14 Saint-Gobain Performance Plastics Corporation Mixing assemblies including magnetic impellers
US10471401B2 (en) 2013-06-28 2019-11-12 Saint-Gobain Performance Plastics Corporation Mixing assemblies including magnetic impellers
US11944946B2 (en) 2013-06-28 2024-04-02 Saint-Gobain Performance Plastics Corporation Mixing assemblies including magnetic impellers
WO2020003692A1 (en) * 2018-06-26 2020-01-02 信越化学工業株式会社 Method of manufacturing negative electrode active material for nonaqueous electrolyte secondary battery
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