JPH04124202A - Compacting assist agent of alloy powder for rare earth element series permanent magnet - Google Patents

Compacting assist agent of alloy powder for rare earth element series permanent magnet

Info

Publication number
JPH04124202A
JPH04124202A JP2240098A JP24009890A JPH04124202A JP H04124202 A JPH04124202 A JP H04124202A JP 2240098 A JP2240098 A JP 2240098A JP 24009890 A JP24009890 A JP 24009890A JP H04124202 A JPH04124202 A JP H04124202A
Authority
JP
Japan
Prior art keywords
polyoxyethylene
rare earth
lubricant
alloy powder
compacting
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
JP2240098A
Other languages
Japanese (ja)
Inventor
Yukiko Ozaki
由紀子 尾崎
Michio Shimotomai
道夫 下斗米
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.)
JFE Steel Corp
Original Assignee
Kawasaki Steel Corp
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 Kawasaki Steel Corp filed Critical Kawasaki Steel Corp
Priority to JP2240098A priority Critical patent/JPH04124202A/en
Publication of JPH04124202A publication Critical patent/JPH04124202A/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
    • H01F1/0533Alloys characterised by their composition containing rare earth metals in a bonding agent
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0576Alloys 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 pressed, e.g. hot working

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

Abstract

PURPOSE:To manufacture a rare earth elemental permanent magnet having excellent magnetic characteristic by using the rare earth metal powder as a raw material, by using a mixed material of one kind of polyoxyethylene compound and lubricant as compacting assist agent. CONSTITUTION:This invention is related to the compacting assist agent for the alloy powder for rare earth elemental permanent magnet composed of the mixed material of at least one kind of the poloxyethylene compound selected among polyoxyethylene sorbithan fatty acid ester, polyoxyethylene sorbitor fatty acid ester, polyoxyethylene alkyl amine and polyoxyethylene derivative and the lubricant, and HLB value in the case of testing as nonionic surface active agent to the polyoxyethlene compound is desirable to be <=15.0. Further, as the lubricant, paraffin, camphor, etc., is available. Further, the suitable mixing ratio of the above polyoxyethylene compound to the lubricant is 1:5-1:1 by wt. ratio and particularly near 1:2 the most suitable ratio.

Description

【発明の詳細な説明】 (産業上の利用分野) この発明は、希土類系永久磁石用合金粉末の成型助剤に
関し、とくにREzPe+a[+系、RECoB系ある
いはREzCO+7系(ただしREはYを含むランタノ
イド元素のうちから選ばれる少なくとも1種)等の合金
粉末の成型の際に用いて好適なものである。
DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a forming aid for rare earth alloy powder for permanent magnets, particularly REzPe+a[+ series, RECoB series or REzCO+7 series (where RE is a lanthanoid containing Y). It is suitable for use in molding alloy powders such as at least one selected from among the elements.

(従来の技術) 近年の電気・電子機器に対する小型化、高効率化の要求
に伴い、永久磁石材料についても高性能化が求められて
いる。そこで、かかる要請に応えるものとして、RE 
−Co系永久磁石やRE2Fe+Jt系永久磁石(特公
昭59−64739号公報)、さらにはRECo系にお
いてはCoの一部を、またREJe、、B、系において
はFeの一部をそれぞれ、他の遷移金属元素およびその
他の特性改善元素の一種または二種以上で置換した希土
類永久磁石が提案された。
(Prior Art) With the recent demand for smaller size and higher efficiency of electrical and electronic equipment, permanent magnet materials are also required to have higher performance. Therefore, as a response to such requests, RE
-Co-based permanent magnets and RE2Fe+Jt-based permanent magnets (Japanese Patent Publication No. 59-64739), and furthermore, in the RECo system, part of the Co, and in the REJe, B, system, part of the Fe is Rare earth permanent magnets substituted with one or more transition metal elements and other property-improving elements have been proposed.

かような希土類磁石は一軸磁気異方性を特徴とするもの
で、この性質を利用して、原料合金粉末を磁場中で加圧
成型後、焼結することにより、結晶配向性の良い永久磁
石を製造している。
Such rare earth magnets are characterized by uniaxial magnetic anisotropy, and by taking advantage of this property, raw material alloy powder is press-molded in a magnetic field and then sintered to create permanent magnets with good crystal orientation. is manufactured.

しかしながら成型時において、原料粉のみをそのまま加
圧成型すると、ダイス壁面との11!擦によってダイス
面および成型体表面にきす、むしれおよび割れ等が生じ
易く、品質および生産性の低下を招く重大な原因となっ
ていた。
However, during molding, if only the raw material powder is pressure molded as it is, the die wall surface will be 11! Rubbing tends to cause scratches, chips, cracks, etc. on the die surface and the surface of the molded body, which is a serious cause of deterioration in quality and productivity.

かかる成型時における問題の解決策として、従来はパラ
フィン、ステアリン酸、ビスアミドあるいは金属石けん
等の結合剤類の添加が行われていた。
Conventionally, as a solution to such problems during molding, binders such as paraffin, stearic acid, bisamide, or metal soap have been added.

しかしながら、パラフィンは成型改良効果が小さいだけ
でなく、多量に使用すると後続工程の焼結過程で十分に
除去できず、焼結体中に炭素が残留して磁気特性の劣化
を招く。またステアリン酸、ビスアミドおよび金属石け
んなどは、原料合金粉末中への均一分散が難しいのに加
え、成型体の強度が低下するという欠点があった。
However, not only does paraffin have a small shaping effect, but if a large amount is used, it cannot be removed sufficiently in the subsequent sintering process, and carbon remains in the sintered body, resulting in deterioration of magnetic properties. Furthermore, stearic acid, bisamide, metal soap, and the like have the drawback that it is difficult to uniformly disperse them into the raw material alloy powder, and the strength of the molded product decreases.

これらの問題に対し、特開昭61−34101号公報、
特開昭60−184604号公報および特開昭60−1
84605号公報などにおいて、ポリオキンエチレンア
ルキルエーテル、ポリオキンエチレンモノ脂肪酸エステ
ルおよびポリオキンエチレンアルキルアリルエーテルの
うちから選んだ少なくとも一種、さらにはこれらのポリ
オキンエチレン系化合物とパラフィン、しょうのうおよ
びステアリン酸塩等の既存の潤滑剤とを混合した成型改
良剤が提案された。
For these problems, Japanese Patent Application Laid-Open No. 61-34101,
JP-A-60-184604 and JP-A-60-1
84605, etc., at least one selected from polyoxine ethylene alkyl ether, polyoxine ethylene monofatty acid ester, and polyoxine ethylene alkyl allyl ether, and furthermore, these polyoxine ethylene compounds, paraffin, ginger, and stearin. A molding improver mixed with existing lubricants such as acid salts has been proposed.

しかしながら、かかる成型改良剤の添加は、Brが幾分
同上するとはいえ、結晶配向性から見るとその効果は十
分とはいい難かった。
However, the effect of adding such a molding improver was not sufficient from the viewpoint of crystal orientation, although Br was somewhat the same.

(発明が解決しようとする課題) この発明は、上記の諸問題を有利に解決するもので、合
金粉末中への分散性に優れるのはいうまでもなく、潤滑
効果が高く、従って磁場中での粉体成型時における成型
性および結晶配向性を著しく向上させ、ひいては高い残
留磁束密度を得ることができる、希土類系永久磁石用合
金粉末の成型助剤を提案することを目的とする。
(Problems to be Solved by the Invention) This invention advantageously solves the above-mentioned problems, and it goes without saying that it has excellent dispersibility in alloy powder, and has a high lubricating effect, so it can be used in a magnetic field. The purpose of the present invention is to propose a molding aid for alloy powder for rare earth permanent magnets, which can significantly improve moldability and crystal orientation during powder molding, and can also obtain high residual magnetic flux density.

(課題を解決するための手段) すなわちこの発明は、ポリオキシエチレンソルビタン脂
肪酸エステル、ポリオキシエチレンソルビトール脂肪酸
エステル、ポリオキシエチレンアルキルアミンおよびポ
リオキシエチレン誘導体のうちから選んだ少なくとも一
種のポリオキシエチレン化合物と潤滑剤との混合体から
なる希土類系永久磁石用合金粉末の成型助剤である。
(Means for Solving the Problem) That is, the present invention provides at least one polyoxyethylene compound selected from polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene alkylamine, and polyoxyethylene derivative. This is a forming aid for alloy powder for rare earth permanent magnets, which consists of a mixture of powder and lubricant.

この発明において、上記したポリオキシエチレン化合物
の非イオン性界面活性剤としてみた場合のHLBMは1
5.0以下が望ましい。
In this invention, the HLBM of the above polyoxyethylene compound when viewed as a nonionic surfactant is 1.
5.0 or less is desirable.

また潤滑剤としては、パラフィン、しょうのうなどが有
利に適合する。
Further, as the lubricant, paraffin, ginger, etc. are advantageously suitable.

さらに上記ポリオキシエチレン化合物と潤滑剤との好適
混合割合は、重量比でl:5〜1:1であり、とくに1
:2近傍が最適である。
Further, the preferred mixing ratio of the polyoxyethylene compound and the lubricant is 1:5 to 1:1 by weight, especially 1:1.
:2 neighborhood is optimal.

(作 用) この発明に従う成型助剤を用いて希土類系磁石を製造す
るには、次の要領で行えばよい。
(Function) A rare earth magnet can be manufactured using the molding aid according to the present invention in the following manner.

すなわち所定量の前記ポリオキシエチレン化合物と潤滑
剤とを、有機溶媒(シクロヘキサン、ヘキサン、ベンゼ
ン、トルエン、石油ベンジン等)中で混合し、この溶液
を、原料合金粉末100重量部に対し、溶液中の成型助
剤の割合が0.01〜0.5重量部程度となる量添加、
混合したのち、磁場中で加圧成形する。ついで得られた
成型体を、不活性雰囲気下または真空中にて600℃以
下の温度で脱脂した後、焼結を行う、なお不活性雰囲気
下の脱脂は、10−’Torr以下の不活性ガス流中で
行うことが望ましい。
That is, a predetermined amount of the polyoxyethylene compound and a lubricant are mixed in an organic solvent (cyclohexane, hexane, benzene, toluene, petroleum benzene, etc.), and this solution is added to 100 parts by weight of the raw material alloy powder in the solution. Adding an amount such that the proportion of the molding aid is about 0.01 to 0.5 parts by weight,
After mixing, the mixture is press-molded in a magnetic field. The obtained molded body is then degreased at a temperature of 600° C. or less in an inert atmosphere or in a vacuum, and then sintered. It is desirable to do this in the current.

(実施例) 実施例1 平均粒径:約2.5μsに粉砕したNd1s(Feo、
56Coo、 1oNio、 + 4) ?7Bl1組
成の合金微粉末100重量部と、予め第1表に示す各成
型助剤(試料階1〜6)をそれぞれ溶解させたシクロヘ
キサン20〜35重量部とを混合し、スラリー(合金微
粉末に対する成型助剤の配合割合0.10〜0.30重
量部)とした。
(Example) Example 1 Nd1s (Feo,
56Coo, 1oNio, + 4)? 100 parts by weight of a fine alloy powder having a composition of 7Bl1 is mixed with 20 to 35 parts by weight of cyclohexane in which each molding aid shown in Table 1 (sample grades 1 to 6) has been dissolved in advance, and a slurry (based on the fine alloy powder) is mixed. The blending ratio of the molding aid was 0.10 to 0.30 parts by weight).

ついでこのスラリーを、12 koeの横磁場中にて2
.0t/cm”の圧力で幅15閣、長さ15■、高さ1
0mmの直方体に加圧成型したのち、室温、300℃、
 400’Cおよび600 ’Cで各2時間ずつ10−
 ’ 〜10− ”Torrの^r波流中脱脂し、真空
中にて1060℃、1時間、ついで1気圧のAr中にて
1060°C,1時間焼結し、その後さらに時効処理を
行って焼結磁石を作製した。
This slurry was then heated in a transverse magnetic field of 12 koe for 2
.. Width: 15 cm, length: 15 cm, height: 1 at a pressure of 0t/cm"
After pressure molding into a rectangular parallelepiped of 0mm, room temperature, 300℃,
10-2 hours each at 400'C and 600'C
'~10-'' Degreased in a Torr wave flow, sintered in vacuum at 1060°C for 1 hour, then sintered in 1 atm Ar at 1060°C for 1 hour, and then further aged. A sintered magnet was produced.

かくして得られた焼結磁石の結晶配向度aおよび磁気特
性について調べた結果を第1表に併記する。
Table 1 also shows the results of examining the degree of crystal orientation a and magnetic properties of the sintered magnet thus obtained.

また第1表には、比較例のため、成型助剤を一切添加し
ない場合(試料隘7)、流動パラフィンと従来汎用され
たポリオキシエチレンラウリルエーテルまたはポリエチ
レングリコールモノラウレートとの混合物を添加した場
合(試料No、 8および9)についての調査結果につ
いても併せて示す。
Table 1 also shows, as a comparative example, a case in which no molding aid was added (sample 7), and a mixture of liquid paraffin and conventionally widely used polyoxyethylene lauryl ether or polyethylene glycol monolaurate. The investigation results for the cases (Samples Nos. 8 and 9) are also shown.

ここに結晶配向度aは、着磁方向に垂直な平面でのX線
回折強度I(hkl)から次のようにして求めた。
Here, the degree of crystal orientation a was determined as follows from the X-ray diffraction intensity I (hkl) in a plane perpendicular to the magnetization direction.

ここでPおよびPoはそれぞれ、磁場中配向させた焼結
体および無配向の焼結体において、全回折ピーク中、C
面=(001)面による回折ピークの占める割合を示す
Here, P and Po are respectively included in the total diffraction peak of C
Plane = shows the ratio of diffraction peaks accounted for by the (001) plane.

実施例2 平均粒径:約2.5 a mに粉砕したNd1s(Fe
o、 5bCoo、 1oNio、 + 4) 7Js
組成の合金微粉末100重量部と、予め第2表に示す成
型助剤(試料No、10〜15)をそれぞれ溶解させた
ベンゼン20〜35重量部とを混合し、スラリー(合金
に対する成型助剤の配合割合0.25〜0.30重量部
)とした。
Example 2 Nd1s (Fe
o, 5bCoo, 1oNio, + 4) 7Js
100 parts by weight of alloy fine powder having the composition and 20 to 35 parts by weight of benzene in which molding aids (sample numbers 10 to 15) shown in Table 2 have been dissolved in advance are mixed, and a slurry (molding aid for the alloy) is mixed. The blending ratio was 0.25 to 0.30 parts by weight).

ついでこのスラリーを12kOeの横磁場中ムごて実施
例1と同様に加圧成型したのち、室温、300°Cおよ
び600℃で各2時間ずつ10− ’ 〜10− ”T
orrのA1流中で脱脂し、真空中にて1060℃、1
時間焼結し、その後さらに時効処理を行って焼結磁石を
作製した。
This slurry was then pressure-molded in a transverse magnetic field of 12 kOe in the same manner as in Example 1, and then molded at room temperature, 300°C and 600°C for 2 hours each for 10-' to 10-''T.
Degreased in A1 stream of orr and heated at 1060°C in vacuum for 1
A sintered magnet was produced by sintering for a time and then further aging treatment.

かくして得られた焼結磁石の結晶配向度aおよび磁気特
性について調べた結果を第2表に併記する。
Table 2 also shows the results of examining the degree of crystal orientation a and magnetic properties of the sintered magnet thus obtained.

第1表および第2表から明らかなように、この発明に従
う成型助剤を用いた場合は、内部潤滑効果の向上によっ
て、従来に比べて焼結磁石の結晶配向性が著しく改善さ
れ、ひいては磁気特性とくに残留磁束密度が向上してい
る。
As is clear from Tables 1 and 2, when the molding aid according to the present invention is used, the crystal orientation of the sintered magnet is significantly improved compared to the conventional one due to the improvement of the internal lubrication effect, and the magnetic The characteristics, especially the residual magnetic flux density, are improved.

(発明の効果) この発明の成型助剤は、合金粉末中への分散性に富むだ
けでなく、優れた潤滑作用を有するので、ダイス面およ
び成型体の摩擦を大幅に低減できるだけでなく、結晶配
向性も格段に向上し、ひいては磁気特性の向上が達成で
きる。
(Effects of the Invention) The molding aid of this invention not only has high dispersibility in alloy powder but also has excellent lubricating action, so it can not only significantly reduce the friction between the die surface and the molded body, but also The orientation is also significantly improved, and as a result, the magnetic properties can be improved.

Claims (1)

【特許請求の範囲】[Claims] 1.ポリオキシエチレンソルビタン脂肪酸エステル、ポ
リオキシエチレンソルビトール脂肪酸エステル、ポリオ
キシエチレンアルキルアミンおよびポリオキシエチレン
誘導体のうちから選んだ少なくとも一種のポリオキシエ
チレン化合物と潤滑剤との混合体からなる希土類系永久
磁石用合金粉末の成型助剤。
1. For use in rare earth permanent magnets, comprising a mixture of at least one polyoxyethylene compound selected from polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene alkylamine, and polyoxyethylene derivatives and a lubricant. A molding aid for alloy powder.
JP2240098A 1990-09-12 1990-09-12 Compacting assist agent of alloy powder for rare earth element series permanent magnet Pending JPH04124202A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2240098A JPH04124202A (en) 1990-09-12 1990-09-12 Compacting assist agent of alloy powder for rare earth element series permanent magnet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2240098A JPH04124202A (en) 1990-09-12 1990-09-12 Compacting assist agent of alloy powder for rare earth element series permanent magnet

Publications (1)

Publication Number Publication Date
JPH04124202A true JPH04124202A (en) 1992-04-24

Family

ID=17054465

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2240098A Pending JPH04124202A (en) 1990-09-12 1990-09-12 Compacting assist agent of alloy powder for rare earth element series permanent magnet

Country Status (1)

Country Link
JP (1) JPH04124202A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5486224A (en) * 1993-12-28 1996-01-23 Sumitomo Metal Industries, Ltd. Powder mixture for use in compaction to produce rare earth iron sintered permanent magnets
CN103996478A (en) * 2014-06-11 2014-08-20 廊坊京磁精密材料有限公司 Method for manufacturing neodymium iron boron magnet

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5486224A (en) * 1993-12-28 1996-01-23 Sumitomo Metal Industries, Ltd. Powder mixture for use in compaction to produce rare earth iron sintered permanent magnets
US5527504A (en) * 1993-12-28 1996-06-18 Sumitomo Metal Industries, Ltd. Powder mixture for use in compaction to produce rare earth iron sintered permanent magnets
CN103996478A (en) * 2014-06-11 2014-08-20 廊坊京磁精密材料有限公司 Method for manufacturing neodymium iron boron magnet
CN103996478B (en) * 2014-06-11 2016-10-26 廊坊京磁精密材料有限公司 A kind of preparation method of neodymium iron boron magnetic body

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