JPH0320001A - Rare earth element-b-fe system sintered magnet superior in corrosion resistance and magnetic characteristic - Google Patents

Rare earth element-b-fe system sintered magnet superior in corrosion resistance and magnetic characteristic

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Publication number
JPH0320001A
JPH0320001A JP1119991A JP11999189A JPH0320001A JP H0320001 A JPH0320001 A JP H0320001A JP 1119991 A JP1119991 A JP 1119991A JP 11999189 A JP11999189 A JP 11999189A JP H0320001 A JPH0320001 A JP H0320001A
Authority
JP
Japan
Prior art keywords
grain boundary
phase
corrosion resistance
sintered magnet
boundary phase
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.)
Granted
Application number
JP1119991A
Other languages
Japanese (ja)
Other versions
JP2663626B2 (en
Inventor
Muneaki Watanabe
宗明 渡辺
Takuo Takeshita
武下　拓夫
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.)
Mitsubishi Materials Corp
Original Assignee
Mitsubishi Materials Corp
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Filing date
Publication date
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Priority to JP1119991A priority Critical patent/JP2663626B2/en
Publication of JPH0320001A publication Critical patent/JPH0320001A/en
Application granted granted Critical
Publication of JP2663626B2 publication Critical patent/JP2663626B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 この発明は、耐食性および磁気特性にすぐれた希土類−
Ｂ−Ｆｅ系焼結磁石に関するものである．〔従来の技術
〕 近年、従来のＳｍ−Ｃｏ系磁石に比べて、より高い磁気
特性を有し、かつ資源的にも高価なＳｍやＣｏを必ずし
も含まない、Ｙを含む希土類元素のうち少なくとも１種
（以上、Ｒで示す）、ＢおよびＦｅを必須戒分とするＲ
−Ｂ−Ｆｅ系永久磁石が発明された．このＲ−Ｂ−Ｆｅ
系永久磁石は、その優れた磁気特性を有する一方で、非
常に腐食され易く、それに伴う磁気特性の劣化が著しい
という欠点を合わせ持っている． このＲ−Ｂ−Ｆｅ系永久磁石は、所定のＲ−Ｂ−Ｆｅ系
合金粉末を圧縮成．形し、焼結することにより製造され
るものであるが、このＲ−Ｂ−Ｆｅ系永久磁石の組成は
、第１図に示されているように、Ｒ２Ｆｅ１４Ｂ相：ａ
、上記Ｒ２Ｆｅ１４Ｂ相の粒界部分に存在するＲリッチ
相（Ｒ９５Ｆｅ５相、Ｒ７５Ｆｅ２５相などから楕戒さ
れていると言われている）：ｂ、およびＲ２Ｆｅ１４Ｂ
４相からなるＢリッチ相：Ｃから主として横或されてお
、り、上記腐食の原因は、主として粒界部分に存在ずる
Ｒリッチ相：ｂが腐食されやすい相であるために、Ｒり
・ソチ相＝ｂを介して粒界腐食が内部に進行することに
よるものと言われている． これらの対策として、特開昭６１−１８５９１０号公報
では、Ｒ−Ｂ−Ｆｅ系永久磁石の表面にＺｎの薄膜を拡
散形成する方法、特開昭６１−２７０３０８号公報では
、Ｒ−Ｂ−Ｆｅ系永久磁石の表面層を除去したのち、Ａ
１の薄膜を被着させる方法、さらに特開昭６３−７７１
０４号公報では、Ｒ−Ｂ−Ｆｅ系永久磁石−の表面にエ
ボキシ樹脂、熱硬化型アクリル樹脂、アルキド樹脂、メ
ラミン樹脂、シリコン樹脂等の塗装用合成樹脂等の耐酸
化性樹脂を塗布する方法が開示されている． 〔発明が解決しようとする課題〕 ところが、上記従来の技術で述べられているＲ−Ｂ−Ｆ
ｅ系永久磁石の防食方法は、いずれも上記永久磁石の表
面にＺｎ，Ａｊ、または合成樹脂等の耐食性のある保護
膜を被着させるもので、磁石の製造工程とは別の工程が
必要となり、工程が複雑化する上にコスト高となり、さ
らに、上記合成樹脂保護膜は厚さがあるために特に小型
磁石製品の寸法精度を悪くする．いずれにしても上記防
食方法は上記永久磁石の外部を腐食等に対して保護する
にすぎず、上記保護膜がはく離したりまたは亀裂が生じ
たりした場合には、それらの個所から内部に腐食が浸透
し、内部的な腐食は防止できず、それに伴って磁気特性
も劣化するという問題点があった． 〔課題を解決するための手段〕 そこで、本発明者等は、耐食性にすぐれ、がっ磁気特性
にもすぐれたＲ−Ｂ−Ｆｅ系焼結磁石を製造すべく研究
を行った結果、 Ｒ２Ｆｅ１４Ｂ相（以下、主相という）と上記主相の−
まわりに存在する粒界相とからなる＃ＩＩＩＩＩｌを有
するＲ−Ｂ−Ｆｅ系焼結磁石であって、（ａ）、粒界相
に、Ｎｌ，Ｃｏ．Ｍｎ，Ｃｒ，Ｔｉ，Ｖ，Ａｊ　，Ｇａ
，Ｉ　ｎ，Ｚｒ，Ｈｆ　，Ｔａ，ＮｂＭｏ．Ｓｉ，Ｒｅ
およびＷのうち少なくとも１種。（以下、Ｍという）が
２０〜９０原子％を含有した粒界相を有するＲ−Ｂ−Ｆ
ｅ系焼結磁石は、すぐれた耐食性を有する． （ｂ）　　粒界相に、Ｍおよび／またはＲ：２σ〜９０
原子％を含有し、さらに酸素：３０〜７０原子％を含有
した粒界相を有するＲ−Ｂ−Ｆｅ系焼結磁石は、一層す
ぐれた耐食性を有する． という知見を得たのである． この発明は、かかる知見にもとづいてなされたものであ
って、 （１）主相と粒界相からなるＲ−Ｂ−Ｆｅ系焼結磁石に
おいて、上記粒界相は、 Ｍ：２０〜９０原子％ を含む粒界相である耐食性および磁気特性にすぐれた希
土類−Ｂ−Ｆｅ系焼結磁石、 （２）主相と粒界相からなるＲ−Ｂ−Ｆｅ系焼結磁石に
おいて、上記粒界相は、 Ｍ：２Ｇ〜９０原子％、 酸素＝３０〜７０原子％、を含む粒界相である耐食性お
よび磁気特性にすぐれた希土類−Ｂ−Ｆｅ系焼結磁石、 （３）主相と粒界相からなるＲ−Ｂ−Ｆｅ系焼結磁石に
おいて、上記粒界相は、 Ｍ　：２０〜９０原子％、 酸素＝３０〜７０原子％、 を含む粒界相である耐食性および磁気特性にすぐれた希
土類一Ｂ−Ｆｅ系焼結磁石、 （４）主相と粒界相からなるＲ−Ｂ−Ｆｅ系焼結磁石に
おいて、上記粒界相は、 Ｍ＋Ｒ：２０〜９０原子％、 酸素　：３０〜７０原子％、 を含む粒界相である耐食性および磁気特性にすぐれた希
土類一Ｂ−Ｆｅ系焼結磁石、 に特徴を有するものである． 上記Ｍが粒界相に２０原子％未満含まれていても十分な
耐食性が得られず、一方、粒界相にＭが９０原子％を越
えて含有させようとすると、製造中に上記Ｍは主相にも
拡ｒ？Ｉｉｌｔ人するために耐食性は向上するが磁気特
性が大幅に低下するので好ましくない． さらに、粒界相に、Ｍおよび／またはＲとともに酸素を
３０〜７０原子％を含有せしめると磁気特性が低下する
ことなく耐食性が一層向上する．粒界相の上記酸素含有
量が３０原子％未満では耐食性の一層の向上はなく、一
方、７０原子％をこえて含有させると主相にも酸素が拡
散し磁気特性を大幅に低下させるので好ましくない． 上記Ｍを含有した粒界相、並びにＭおよび／またはＲと
ともにｉ！！素を含有した粒界相は、第１図に示される
Ｒリッチ相よりも腐食しにくい相であり、この腐食しに
くい粒界相は焼結過程での結晶粒の成長を抑制し高密度
化させる作用を有するために耐食性および磁気特性が共
に優れたＲ−Ｂ−Ｆｅ系焼結磁石が得られるものと考え
られる．この発明の粒界相にＭ：２０〜９０原子％を含
む希土類−Ｂ−Ｆｅ系焼結磁石は、所定の組威を有する
Ｒ−Ｂ−Ｆｅ系合金粉末にＭの超微粉末またはＭの水素
化物粉末を０．　０００５〜３重量％配合し、混合して
得られた混合粉末を、成形し、非酸化性雰囲気中、温度
＝９００〜１２００℃で焼結することにより製造される
．上記Ｒ−Ｂ−Ｆｅ系合金粉末に混合する粉末は、Ｍの
超微粉末よりもＭの水素化物粉末の方が好ましい．Ｍの
超微粉末は焼結中にＲ２Ｆｅ１４Ｂ相に拡散するが、Ｍ
の水素化物粉末はＲ２Ｆｅ，４Ｂ相に拡散する量が少な
く、焼結中にＭの水素化物の水素は放出され、Ｍのみが
粒界Ｒ：２０〜９０原子％とともに酸素＝３０〜７０原
子％を含む希土類−Ｂ−Ｆｅ系焼結磁石は、所定の組成
を有するＲ−Ｂ−Ｆｅ系合金粉末に、Ｍおよび／または
Ｒの酸化物粉末を０．　０００５〜２．５重量％配合し
、混合して得られた混合粉末を、成形し、非酸化性雰囲
気中、温度＝９００〜１２００℃で焼結することにより
製造される． このようにして製造された希土類一Ｂ−Ｆｅ系焼結磁石
は、必要に応じて非酸化性雰囲気中、温度＝４００〜７
００℃で熱処理してもよい．〔実施例〕 つぎに、この発明の実施例について説明する．実施例１
〜１７ まず、１５％Ｎｄ−８％Ｂ一残Ｆｅ（但し％は原子％）
となるように溶解し、合金インゴットを作製した．この
合金インゴットをアルゴン雰囲気中で温度：　１Ｇ５０
℃、２０時間保持の熱処理を行ったあと、粉砕し、平均
粒径：３５μｍのＲ−Ｂ−Ｆｅ系合金粉末を用意した． 一方、添加粉末として、ＮｉＯ粉末（平均粒径：１．０
　μｍ）　、ＣＯ２　０３　　（平均粒径：　１．２　
μｍ）　．Ｍ　ｎ　０　２粉末（平均粒径：　１．０　
μｍ　）、Ｃｒ２０３粉末（平均粒径：１．２μｍ），
ＴＩＯ２粉末（平均粒径：　１．５　μｍ　）　，Ｖ２
０５粉末（平均粒径：１．４μｍ），Ａ　ｊ　２　０　
３粉末（平均粒径：１．２μｍ）．Ｇａ２　０３粉末（
平均粒径：Ｌ２μｍ），Ｉｎ２０３粉末《平均粒径：　
１．４　μｍ　）、Ｚ　ｒ　Ｏ　２粉末（平均粒径：１
．２，ｃｚｍ）、ＨｆＯ２　（平均粒径：１．２ｕｍ）
、Ｎ　ｂ　２　０　ａ粉末《平均粒径：１．３μｍ＞、
Ｄｙ２０３粉末（平均粒径：１．２ｕｍ）、Ｙ　２　０
　３粉末（平均粒径：１．０μｍ）を用意した．上記Ｒ
−Ｂ−Ｆｅ系合金粉末と上記酸化物添加粉末のうち１種
または２種以上をｏ．　ｏｏｏｓ〜２．５重圭％の範囲
内で配合し、混合し、この混合粉末を成形圧＝２ｔ／一
で磁場中（１４ＫＯｅ）にて威形し、たて：２０噛×横
：２０ａｍｘ高さ＝１５−の成形体を作製した．これら
成形体を真空中（　１Ｇ−５Ｔｏｒｒ）で１０’Ｃ／ｌ
ｌｉｎの昇温速度にて加熱し、温度．　１０８０℃、２
時間保持の条件で焼結し、１００℃／ｌｉｎの冷却速度
で冷却した． この焼結体を加熱速度＝１００℃／ｌＩｉｎで加熱し、
温度＝６２０℃、２時間保持したのち、１００℃／ｗｉ
ｎの冷却速度で冷却し熱処理した． この熱処理した焼結体の組織を調べたところ、Ｒ２Ｆｅ
１４Ｂ相および粒界相からなり、第１図とほぼ同一の組
織を有しており、上記粒界相の組成を、ＳＴＥＭにより
測定してその結果を第１表に示した．さらに、上記焼結
体の磁気特性を測定し、この焼結体を温度＝６０℃、湿
度＝９０％の大気中に１０００時間放置して耐食試験を
行なった後、再度、磁気特性を測定するとともに錆の発
生状況を目視により［ｌＩ察し、これらの結果を第１表
に示した．第１表において、耐食試験前に測定した磁気
特性の測定値を「耐食試験前Ｊの欄に、耐食試験後に測
定した磁気特性の測定値を「耐食試験後」の欄に示した
． 実施例１８〜２８ 添加粉末として、Ｚ　ｒ　Ｈ　２粉末（平均粒径：（平
均粒径：　１．３　μｍ）　、ＶＨ粉末（平均粒径：１
．５　μｍ　）　，　Ｈ　ｆ　Ｈ２粉末（平均粒径１．
３μｍ）およびＹＨ３粉末《平均粒径：１．１μｍ》を
用意し、これら粉末を上記実施例１〜１７で用意した１
５％Ｎｄ−８％Ｂ一残Ｆｅ（但し、％は、原子％）のＲ
−Ｂ−Ｆｅ系合金粉末と０．０００５〜３重量％の範囲
内の所定割合となるように配合し、混合して混合粉末と
し、これら混合粉末を上記実膳例１〜１７と全く同一条
件で焼結体を作製し、同様に粒界相の金属元素をＳＴＥ
Ｍにより測定し、磁気特性を測定したのち耐食試験を行
ない、錆の発生状況を目視により［察したのち、再度磁
気特性を測定して、それらの値を第２表に示した． 第１表および第２表の結果から、粒界相に金属元素およ
び酸素の含まれない従来例と比べて、粒界相に金属元素
、または金属元素と酸素とが同時に含まれているこの発
明の希土類一Ｂ−Ｆｅ系焼結磁石は磁気特性に優れてい
るとともに耐食性にもすぐれていることがわかる． 〔発明の効果〕 この発明のＲ−Ｂ−Ｆｅ系焼結磁石には表面処理する必
要がなく、また焼結磁石の磁気特性の劣化が少ないので
、この磁石を組み込んだ装置の性能の低下が防止される
という産業上すぐれた効果を奏するものである．[Detailed Description of the Invention] [Industrial Application Field] The present invention uses rare earth metals with excellent corrosion resistance and magnetic properties.
This relates to B-Fe sintered magnets. [Prior Art] In recent years, at least one rare earth element containing Y, which has higher magnetic properties than conventional Sm-Co magnets and does not necessarily contain Sm or Co, which are expensive in terms of resources, has been developed. R with species (denoted as R above), B and Fe as essential precepts
-B-Fe permanent magnets were invented. This R-B-Fe
While permanent magnets have excellent magnetic properties, they also have the disadvantage of being highly susceptible to corrosion and resulting in significant deterioration of magnetic properties. This R-B-Fe permanent magnet is made by compressing a predetermined R-B-Fe alloy powder. This R-B-Fe permanent magnet is manufactured by shaping and sintering, and the composition of this R-B-Fe permanent magnet is as shown in FIG.
, R-rich phase (said to be elliptical from R95Fe5 phase, R75Fe25 phase, etc.) existing in the grain boundary part of the R2Fe14B phase: b, and R2Fe14B
B-rich phase consisting of 4 phases: It is mainly lateralized from C, and the cause of the above corrosion is mainly the R-rich phase that exists in the grain boundary area.Since b is a phase that is easily corroded, R-rich phase This is said to be due to intergranular corrosion progressing internally via the Sochi phase (b). As a countermeasure to these problems, JP-A-61-185910 discloses a method of diffusing and forming a Zn thin film on the surface of an R-B-Fe permanent magnet, and JP-A-61-270308 discloses a method of diffusing and forming a Zn thin film on the surface of an R-B-Fe permanent magnet. After removing the surface layer of the system permanent magnet,
The method of depositing a thin film of No. 1, and also Japanese Patent Application Laid-open No. 63-771
No. 04 discloses a method of applying an oxidation-resistant resin such as a synthetic resin for painting such as epoxy resin, thermosetting acrylic resin, alkyd resin, melamine resin, silicone resin, etc. to the surface of an R-B-Fe-based permanent magnet. is disclosed. [Problem to be solved by the invention] However, the R-B-F described in the above-mentioned conventional technology
All methods for preventing corrosion of e-based permanent magnets involve coating the surface of the permanent magnet with a corrosion-resistant protective film made of Zn, Aj, or synthetic resin, which requires a process different from the magnet manufacturing process. This complicates the process and increases costs.Furthermore, the thickness of the synthetic resin protective film deteriorates the dimensional accuracy of small magnet products in particular. In any case, the above corrosion prevention method only protects the outside of the permanent magnet from corrosion, etc., and if the above protective film peels off or cracks occur, corrosion will occur inside from those points. There was a problem that penetration and internal corrosion could not be prevented, and the magnetic properties deteriorated accordingly. [Means for Solving the Problems] Therefore, the present inventors conducted research to produce an R-B-Fe-based sintered magnet that has excellent corrosion resistance and magnetic properties, and as a result, the R2Fe14B phase (hereinafter referred to as the main phase) and - of the above main phase
An R-B-Fe based sintered magnet having #IIIIl consisting of a grain boundary phase existing around the grain boundary phase, (a) Nl, Co. Mn, Cr, Ti, V, Aj, Ga
, In, Zr, Hf, Ta, NbMo. Si, Re
and at least one of W. (hereinafter referred to as M) having a grain boundary phase containing 20 to 90 at%
E-based sintered magnets have excellent corrosion resistance. (b) M and/or R: 2σ~90 in the grain boundary phase
An R-B-Fe based sintered magnet having a grain boundary phase containing 30 to 70 atomic % of oxygen has even better corrosion resistance. We obtained this knowledge. The present invention was made based on this knowledge, and includes: (1) In an R-B-Fe sintered magnet consisting of a main phase and a grain boundary phase, the grain boundary phase has M: 20 to 90 atoms. (2) In the R-B-Fe sintered magnet consisting of a main phase and a grain boundary phase, the grain boundary phase The phase is a rare earth-B-Fe based sintered magnet with excellent corrosion resistance and magnetic properties, which is a grain boundary phase containing M: 2G to 90 at% and oxygen = 30 to 70 at%, (3) Main phase and grains. In the R-B-Fe-based sintered magnet consisting of an interfacial phase, the grain boundary phase is a grain boundary phase containing M: 20 to 90 at%, oxygen = 30 to 70 at%, and has excellent corrosion resistance and magnetic properties. (4) In the R-B-Fe sintered magnet consisting of a main phase and a grain boundary phase, the grain boundary phase is as follows: M+R: 20 to 90 at%, oxygen: 30 A rare earth B-Fe based sintered magnet with excellent corrosion resistance and magnetic properties, which has a grain boundary phase containing ~70 at%. Even if the grain boundary phase contains less than 20 atomic percent of M, sufficient corrosion resistance cannot be obtained. On the other hand, if the grain boundary phase contains more than 90 atomic percent of M, the above M is Expands to the main phase? Corrosion resistance improves due to the corrosion resistance, but the magnetic properties are significantly reduced, which is not desirable. Furthermore, when the grain boundary phase contains 30 to 70 at % of oxygen together with M and/or R, the corrosion resistance is further improved without deteriorating the magnetic properties. If the oxygen content in the grain boundary phase is less than 30 atomic %, there is no further improvement in corrosion resistance, whereas if it exceeds 70 atomic %, oxygen will diffuse into the main phase, resulting in a significant decrease in magnetic properties, which is preferable. do not have. The above grain boundary phase containing M, together with M and/or R, i! ! The grain boundary phase containing R-rich is a phase that is less likely to corrode than the R-rich phase shown in Figure 1, and this less corrosive grain boundary phase suppresses the growth of crystal grains during the sintering process, resulting in higher density. It is believed that this sintered R-B-Fe-based magnet has excellent corrosion resistance and magnetic properties due to the action of oxidation. The rare earth-B-Fe based sintered magnet containing 20 to 90 atomic % of M in the grain boundary phase of the present invention is produced by adding ultrafine M powder or M to an R-B-Fe alloy powder having a predetermined composition strength. 0.0% hydride powder. 0005 to 3% by weight, and the resulting mixed powder is molded and sintered at a temperature of 900 to 1200°C in a non-oxidizing atmosphere. The powder to be mixed with the R-B-Fe alloy powder is preferably M hydride powder rather than M ultrafine powder. The ultrafine powder of M diffuses into the R2Fe14B phase during sintering, but the M
The amount of hydride powder diffused into the R2Fe,4B phase is small, and the hydrogen of the hydride of M is released during sintering, and only M has grain boundaries R: 20-90 at% and oxygen = 30-70 at%. A rare earth-B-Fe based sintered magnet containing M and/or R oxide powder is added to an R-B-Fe based alloy powder having a predetermined composition. 0005 to 2.5% by weight, and the resulting mixed powder is molded and sintered at a temperature of 900 to 1200°C in a non-oxidizing atmosphere. The rare earth-B-Fe sintered magnet produced in this way may be sintered in a non-oxidizing atmosphere at a temperature of 400 to 7
It may be heat treated at 00℃. [Example] Next, an example of the present invention will be described. Example 1
~17 First, 15%Nd-8%B, balance Fe (however, % is atomic%)
An alloy ingot was prepared by melting the alloy to give the following properties. This alloy ingot was heated to 1G50 in an argon atmosphere.
After being heat-treated at ℃ for 20 hours, it was pulverized to prepare R-B-Fe alloy powder with an average particle size of 35 μm. On the other hand, NiO powder (average particle size: 1.0
μm), CO2 03 (average particle size: 1.2
μm). M n 0 2 powder (average particle size: 1.0
μm), Cr203 powder (average particle size: 1.2 μm),
TIO2 powder (average particle size: 1.5 μm), V2
05 powder (average particle size: 1.4 μm), A j 2 0
3 powder (average particle size: 1.2 μm). Ga2 03 powder (
Average particle size: L2μm), In203 powder《Average particle size:
1.4 μm), ZrO2 powder (average particle size: 1
．． 2, czm), HfO2 (average particle size: 1.2um)
, Nb20a powder <<average particle size: 1.3 μm>>,
Dy203 powder (average particle size: 1.2um), Y20
3 powders (average particle size: 1.0 μm) were prepared. Above R
-B-Fe alloy powder and one or more of the above oxide-added powders are mixed in an o. The mixed powder was blended within the range of ooos~2.5% by weight, mixed, and compacted in a magnetic field (14KOe) with a molding pressure of 2t/1. A molded body with a diameter of 15- was produced. These molded bodies were heated at 10'C/l in vacuum (1G-5Torr).
Heating was carried out at a heating rate of lin to bring the temperature to . 1080℃, 2
It was sintered under conditions of time holding and cooled at a cooling rate of 100°C/lin. This sintered body is heated at a heating rate of 100°C/lIin,
Temperature = 620℃, after holding for 2 hours, 100℃/wi
It was cooled and heat treated at a cooling rate of n. When the structure of this heat-treated sintered body was investigated, it was found that R2Fe
It consists of a 14B phase and a grain boundary phase, and has almost the same structure as shown in Figure 1.The composition of the grain boundary phase was measured by STEM, and the results are shown in Table 1. Furthermore, the magnetic properties of the sintered body are measured, and the sintered body is left in the atmosphere at a temperature of 60°C and humidity of 90% for 1000 hours to perform a corrosion resistance test, and then the magnetic properties are measured again. At the same time, the occurrence of rust was visually observed and the results are shown in Table 1. In Table 1, the measured values of magnetic properties measured before the corrosion resistance test are shown in the column ``Before corrosion resistance test J'', and the measured values of magnetic properties measured after the corrosion resistance test are shown in the column ``After corrosion resistance test''. Examples 18 to 28 As additive powders, Z r H 2 powder (average particle size: (average particle size: 1.3 μm), VH powder (average particle size: 1
．． 5 μm), H f H2 powder (average particle size 1.
3 μm) and YH3 powder (average particle size: 1.1 μm) were prepared, and these powders were mixed with 1 prepared in Examples 1 to 17 above.
R of 5%Nd-8%B, balance Fe (however, % is atomic%)
- B-Fe-based alloy powder and blended at a predetermined ratio within the range of 0.0005 to 3% by weight, mixed to form a mixed powder, and these mixed powders were prepared under exactly the same conditions as in Examples 1 to 17 above. A sintered body was prepared using STE, and the metal elements in the grain boundary phase were similarly
After measuring the magnetic properties, a corrosion resistance test was conducted, and the state of rust formation was visually observed.The magnetic properties were then measured again, and the values are shown in Table 2. From the results in Tables 1 and 2, it can be seen that this invention in which the grain boundary phase contains a metal element or a metal element and oxygen at the same time, compared to the conventional example in which the grain boundary phase does not contain a metal element or oxygen. It can be seen that the rare earth B-Fe sintered magnet has excellent magnetic properties and corrosion resistance. [Effects of the Invention] The R-B-Fe sintered magnet of the present invention does not require surface treatment, and there is little deterioration in the magnetic properties of the sintered magnet, so there is no reduction in the performance of devices incorporating this magnet. This has an excellent industrial effect of preventing this.

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

第１図は、Ｒ−Ｂ−Ｆｅ系焼結磁石の組ｍ図である． Figure 1 is a diagram of a set of R-B-Fe sintered magnets.

Claims (4)

【特許請求の範囲】[Claims] （１）Ｒ＿２Ｆｅ＿１＿４Ｂ相（Ｒは、Ｙを含む希土類
元素のうち１種または２種以上）および上記 Ｒ＿２Ｆｅ＿１＿４Ｂ相のまわりに存在する粒界相とか
らなる組織を有するＲ−Ｂ−Ｆｅ系焼結磁石であつて、 上記粒界相は、Ｎｉ，Ｃｏ，Ｍｎ，Ｃｒ，Ｔｉ，Ｖ，Ａ
ｌ，Ｇａ，Ｉｎ，Ｚｒ，Ｈｆ，Ｔａ，Ｎｂ，Ｍｏ，Ｓｉ
，ＲｅおよびＷのうち少なくとも１種（以下、Ｍという
）：２０〜９０原子％を含む粒界相であることを特徴と
する耐食性および磁気特性に優れた希土類−Ｂ−Ｆｅ系
焼結磁石。(1) R-B-Fe-based sintered magnet having a structure consisting of an R_2Fe_1_4B phase (R is one or more rare earth elements including Y) and a grain boundary phase existing around the R_2Fe_1_4B phase. The grain boundary phase is Ni, Co, Mn, Cr, Ti, V, A
l, Ga, In, Zr, Hf, Ta, Nb, Mo, Si
, Re, and W (hereinafter referred to as M): a grain boundary phase containing 20 to 90 atomic % of a rare earth-B-Fe based sintered magnet having excellent corrosion resistance and magnetic properties. （２）Ｒ＿２Ｆｅ＿１＿４Ｂ相および上記Ｒ＿２Ｆｅ＿
１＿４Ｂ相のまわりに存在する粒界相とからなる組織を
有するＲ−Ｂ−Ｆｅ系焼結磁石であって、上記粒界相は
、Ｍ：２０〜９０原子％、 酸素：３０〜７０原子％、 を含む粒界相であることを特徴とする耐食性および磁気
特性に優れた希土類Ｂ−Ｆｅ系焼結磁石。(2) R_2Fe_1_4B phase and the above R_2Fe_
An R-B-Fe-based sintered magnet having a structure consisting of a grain boundary phase existing around the 1_4B phase, the grain boundary phase comprising M: 20 to 90 at%, and oxygen: 30 to 70 at%. , A rare earth B-Fe-based sintered magnet with excellent corrosion resistance and magnetic properties, characterized by a grain boundary phase containing. （３）Ｒ＿２Ｆｅ＿１＿４Ｂ相および上記Ｒ＿２Ｆｅ＿
１＿４Ｂ相のまわりに存在する粒界相とからなる組織を
有するＲ−Ｂ−Ｆｅ系焼結磁石であって、上記粒界相は
、Ｒ：２０〜９０原子％、 酸素：３０〜７０原子％、 を含む粒界相であることを特徴とする耐食性および磁気
特性に優れた希土類−Ｂ−Ｆｅ系焼結磁石。(3) R_2Fe_1_4B phase and the above R_2Fe_
An R-B-Fe based sintered magnet having a structure consisting of a grain boundary phase existing around the 1_4B phase, the grain boundary phase comprising: R: 20 to 90 at%, oxygen: 30 to 70 at% A rare earth-B-Fe based sintered magnet with excellent corrosion resistance and magnetic properties, characterized by a grain boundary phase containing , . （４）Ｒ＿２Ｆｅ＿１＿４Ｂ相および上記Ｒ＿２Ｆｅ＿
１＿４Ｂ相のまわりに存在する粒界相とからなる組織を
有するＲ−Ｂ−Ｆｅ系焼結磁石であって、上記粒界相は
、Ｍ＋Ｒ：２０〜９０原子％、 酸素：３０〜７０原子％、 を含む粒界相であることを特徴とする耐食性および磁気
特性に優れた希土類−Ｂ−Ｆｅ系焼結磁石。(4) R_2Fe_1_4B phase and the above R_2Fe_
An R-B-Fe based sintered magnet having a structure consisting of a grain boundary phase existing around the 1_4B phase, the grain boundary phase being M+R: 20 to 90 at%, oxygen: 30 to 70 at% A rare earth-B-Fe based sintered magnet with excellent corrosion resistance and magnetic properties, characterized by a grain boundary phase containing , .
JP1119991A 1989-05-12 1989-05-12 Rare earth-B-Fe based sintered magnet with excellent corrosion resistance and magnetic properties Expired - Fee Related JP2663626B2 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7048808B2 (en) * 2000-10-04 2006-05-23 Neomax Co., Ltd. Rare-earth sintered magnet and method of producing the same
KR100760453B1 (en) * 2002-11-14 2007-09-20 신에쓰 가가꾸 고교 가부시끼가이샤 R-Fe-B Sintered Magnet
JP2013045844A (en) * 2011-08-23 2013-03-04 Toyota Motor Corp Manufacturing method of rare earth magnet, and rare earth magnet

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111326306B (en) * 2020-02-29 2021-08-27 厦门钨业股份有限公司 R-T-B series permanent magnetic material and preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61207545A (en) * 1985-03-09 1986-09-13 Sumitomo Special Metals Co Ltd Manufacture of permanent magnet material
JPS6250437A (en) * 1985-08-28 1987-03-05 Sumitomo Special Metals Co Ltd Permanent magnet material superior in corrosion resistance
JPS6274054A (en) * 1985-09-27 1987-04-04 Hitachi Metals Ltd Permanent magnet alloy

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61207545A (en) * 1985-03-09 1986-09-13 Sumitomo Special Metals Co Ltd Manufacture of permanent magnet material
JPS6250437A (en) * 1985-08-28 1987-03-05 Sumitomo Special Metals Co Ltd Permanent magnet material superior in corrosion resistance
JPS6274054A (en) * 1985-09-27 1987-04-04 Hitachi Metals Ltd Permanent magnet alloy

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7048808B2 (en) * 2000-10-04 2006-05-23 Neomax Co., Ltd. Rare-earth sintered magnet and method of producing the same
KR100760453B1 (en) * 2002-11-14 2007-09-20 신에쓰 가가꾸 고교 가부시끼가이샤 R-Fe-B Sintered Magnet
JP2013045844A (en) * 2011-08-23 2013-03-04 Toyota Motor Corp Manufacturing method of rare earth magnet, and rare earth magnet
US9761358B2 (en) 2011-08-23 2017-09-12 Toyota Jidosha Kabushiki Kaisha Method for producing rare earth magnets, and rare earth magnets

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