JPS6347907A - Manufacture of rare earth magnet - Google Patents

Manufacture of rare earth magnet

Info

Publication number
JPS6347907A
JPS6347907A JP61192595A JP19259586A JPS6347907A JP S6347907 A JPS6347907 A JP S6347907A JP 61192595 A JP61192595 A JP 61192595A JP 19259586 A JP19259586 A JP 19259586A JP S6347907 A JPS6347907 A JP S6347907A
Authority
JP
Japan
Prior art keywords
aging
manufacturing
magnet
ageing
rare earth
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
JP61192595A
Other languages
Japanese (ja)
Inventor
Tadakuni Sato
忠邦 佐藤
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.)
Tokin Corp
Original Assignee
Tohoku Metal Industries 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 Tohoku Metal Industries Ltd filed Critical Tohoku Metal Industries Ltd
Priority to JP61192595A priority Critical patent/JPS6347907A/en
Publication of JPS6347907A publication Critical patent/JPS6347907A/en
Pending legal-status Critical Current

Links

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
    • H01F1/057Alloys 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
    • H01F1/0577Alloys 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

Abstract

PURPOSE:To obtain a high-performance magnet having a high energy product by applying an ageing for a long period of time at a low temperature when manufacturing a R2T14B-system magnet by the use of the powdered metal technique. CONSTITUTION:In a method for manufacturing a R2T14B-system alloy containing Nd.Fe.B as the principal component by means of the powdered metal technique, extremely high magnet characteristics having a (BH)max which is 45MGOe or higher are obtained by applying an ageing for 2-30 hours within a temperature range of 470-600 deg.C after sintering a compressed powder in a magnetic field. Since high magnet characteristics is thus obtained even if the sustained- release hold time is set over a wide range, the work can simply be performed, and the setting ranges of the amount of heat and the heat-up speed needed for the ageing can be made wider, so mass-treatment is available at a time.

Description

【発明の詳細な説明】 本発明は、N d l’;’ e−B系永久磁石を代表
とする希土類金属(R)と遷移金属(T)とホウ素(B
)を主成分としてなるR2T14B系金属間化合物磁石
の中でも、極めて高い磁石特性である最大エネルギー積
(B H) m a X、  45MGOe以上を有す
る高エネルギー積の高性能磁石の製造方法に関するもの
である。
Detailed Description of the Invention The present invention utilizes rare earth metals (R), transition metals (T), and boron (B
) The present invention relates to a method for manufacturing a high-performance magnet with a high energy product, which has a maximum energy product (B H) m a .

R−Fe−B系磁石の製造方法については、二つの方法
に大別される。ひとつは、溶解している合金を超急冷し
た後、粉砕した磁石粉末を磁場中で配向して製造される
高分子複合型磁石である。一方は、溶解して得られた磁
石合金のインゴットを微粉砕し、磁場中で成形した後、
焼結して製造される焼結型磁石である。本発明は、焼結
型磁石に関係している。
Methods for manufacturing R-Fe-B magnets are roughly divided into two methods. One is a polymer composite magnet, which is manufactured by ultra-quenching a molten alloy and then orienting crushed magnetic powder in a magnetic field. On the one hand, a magnetic alloy ingot obtained by melting is pulverized and shaped in a magnetic field, and then
It is a sintered magnet manufactured by sintering. The present invention relates to sintered magnets.

R−Fe−B系磁石の粉末冶金法によって製造される焼
結型磁石に関する文献として、特開昭59−46008
や日本応用磁気学会第35回研究会資料「Nd−Fe−
B系新磁石」 (昭和59年5月)があげられる。これ
らの文献には、溶解して得たインゴットを粉砕、磁場中
成形後Ar雰囲ス中で焼結し、1時間の短時間納処理に
より11(cの向とを計る方法について記述しである。
As a document regarding sintered magnets manufactured by powder metallurgy of R-Fe-B magnets, JP-A-59-46008
``Nd-Fe-
"B Series New Magnets" (May 1981). These documents describe a method for measuring the direction of 11 (c) by crushing an ingot obtained by melting, forming it in a magnetic field, sintering it in an Ar atmosphere, and performing a short delivery process of 1 hour. be.

一般に、水系磁石の粉末冶金法による製造工程は、原料
合金の溶解、粉砕、磁場中配向、圧縮成形、焼結、時効
の順に進められる。溶解は、アーク、高周波等の真空ま
たは不活性雰囲気中で通常行われ、合金原料インゴット
を得ている。粉砕は粗粉砕と微粉砕にわけられ、粗粉砕
はショークラッシャー、鉄乳鉢、ディスクミルやロール
ミル等で行われる。微粉砕は、ボールミル、振動ミル、
ジェットミル等で行われる。磁場配向及び圧縮成形は金
型を用いて磁場中で同時に行われるのが通例である。焼
結は、1000〜1150”Cの範囲で不活性雰囲気中
で行われる。時効は、600”C近傍の温度で約1時間
行われる。この際最適温度及び最適保持時間を設定した
としても、 (BH)m a rはせいぜい43. 5
 MGOe程度である。
Generally, the manufacturing process of water-based magnets by powder metallurgy is carried out in the following order: melting of a raw material alloy, pulverization, orientation in a magnetic field, compression molding, sintering, and aging. Melting is usually performed in a vacuum or inert atmosphere using arc, high frequency, etc., to obtain an alloy raw material ingot. Grinding is divided into coarse grinding and fine grinding, and coarse grinding is performed using a show crusher, iron mortar, disk mill, roll mill, etc. Fine grinding can be done using ball mills, vibrating mills,
This is done using a jet mill, etc. Magnetic field orientation and compression molding are usually performed simultaneously in a magnetic field using a mold. Sintering is carried out in an inert atmosphere in the range of 1000-1150"C. Aging is carried out at a temperature near 600"C for about 1 hour. At this time, even if the optimum temperature and holding time are set, (BH)mar is at most 43. 5
It is about MGOe.

本発明者は、種々実験を重ねた結果、これらの工程中で
時効条件を変化させることにより、著しく高い磁石特性
の得られることを発見した。すなわち、従来の時効と比
較し、低い温度で長時間時効処理を施すことにより、I
Hc、8Hc、減磁曲線の角形性が向上し、著しく高い
(BH)maxが得られることを発見した。本発明によ
れば、時効保持時間を広範囲に設定しても高い磁石特性
が得られるので、作業が簡便に行えること、時効処理の
際に必要な熱量と昇温速度の設定範囲を広くすることが
できることから、一度に大量処理が可能となる等、工業
的な有用性も向上する。
As a result of various experiments, the inventors of the present invention have discovered that by changing the aging conditions during these steps, significantly improved magnetic properties can be obtained. In other words, compared to conventional aging, by aging at a lower temperature for a longer time, the I
It was discovered that the squareness of Hc, 8Hc, and demagnetization curves was improved, and a significantly high (BH)max was obtained. According to the present invention, high magnetic properties can be obtained even if the aging holding time is set over a wide range, so the work can be performed easily, and the setting range of the amount of heat and temperature increase rate required for aging treatment can be widened. Since it is possible to process a large amount at once, it also improves its industrial usefulness.

本発明における時効条件の範囲は、Nd−Fe・B系磁
石の最大の特徴である高エネルギー積を考慮し、 (B
H)max、45MGOe以上としている。この磁石特
性を満たす本発明の時効条件は、時効温度が470℃〜
600℃で、時効保持時間は2〜30時間とした0時効
保持時間を2時間以上としたのは、2時間未満ては(B
H)mayが低いこと、30時間以内としたのは、これ
以上では工業的に極めて不利益となるからである。また
時効保持温度範囲を限定したのは、470℃〜600℃
以外では30時間以下の保持で(BH)max、45M
GOe以上が得られないためである。
The range of aging conditions in the present invention is determined by considering the high energy product, which is the greatest feature of Nd-Fe・B magnets, and (B
H) max, 45 MGOe or more. The aging condition of the present invention that satisfies this magnetic property is that the aging temperature is 470℃~
At 600°C, the aging holding time was 2 to 30 hours, and the zero aging holding time was 2 hours or more (B
The reason why H) may be low and within 30 hours is that anything longer than this would be extremely disadvantageous industrially. In addition, the aging holding temperature range was limited to 470°C to 600°C.
(BH) max, 45M with retention of 30 hours or less
This is because GOe or higher cannot be obtained.

また、後述する実施例に示すように、従来行われていた
1時間程度の時効保持時間では、厳畜に時効温度を設定
したとしても、 (BH)may。
Furthermore, as shown in the examples described below, with the conventional aging holding time of about one hour, (BH) may occur even if the aging temperature is set strictly.

45 MGOe以上を得ることが極めて困難である。し
かしながら、本発明の時効保持時間におけるように、従
来に比べ2倍以上の保持時間とすることにより、広い時
効処理条件範囲で、 (BH)max、45MGOe以
上の極めて高性能な希土類磁石の製造が可能となり、工
業上極めて有用な製法となる。
It is extremely difficult to obtain more than 45 MGOe. However, by making the aging holding time more than twice that of the conventional one, as in the case of the aging holding time of the present invention, it is possible to manufacture extremely high-performance rare earth magnets with (BH)max of 45 MGOe or more over a wide range of aging treatment conditions. This makes it an extremely useful manufacturing method industrially.

以下、実施例について述べる。Examples will be described below.

〔実施例〕〔Example〕

純度97%のNd(残部はCe、Prを主体とする他の
希土類元素)、クリスタルボロン及び電解鉄を使用し、
Ndが31.0wt%、Bが1.ow t%、残部Fe
となる様にアルゴン雰囲気中で、高周波加熱により溶解
し、Cu鋳型に流し込んでFe析出相のRm (3Vo
l、%以下)な合金インゴットを得た。次に、このイン
ゴットを粗粉砕した後ボールミルを用いて平均粒径約3
μmに微粉砕した。この粉末を25 KOeの磁界中、
Iton/em2の圧力で成形した。この成形体を10
70℃で真空中1時間保持した後、Ar雰囲気中で1時
間保持し、焼結した後、50℃/ In以上の冷却速度
で400℃以下まで急冷した。
Using 97% pure Nd (the remainder is other rare earth elements mainly consisting of Ce and Pr), crystal boron, and electrolytic iron,
Nd was 31.0 wt%, B was 1. ow t%, balance Fe
The Fe precipitated phase Rm (3Vo
%) was obtained. Next, after coarsely pulverizing this ingot, it was milled using a ball mill with an average particle size of approximately 3
It was pulverized to micrometers. This powder was placed in a magnetic field of 25 KOe.
It was molded at a pressure of Iton/em2. 10 pieces of this molded body
After being held at 70°C in vacuum for 1 hour, it was held in an Ar atmosphere for 1 hour, sintered, and then rapidly cooled to 400°C or less at a cooling rate of 50°C/In or more.

この焼結体を、470℃、500℃、550℃、600
℃、650℃の各温度で、最短1/4時間から最長32
時間まで保持し急冷した。これら試料の磁気特性を図に
示す。
This sintered body was heated at 470°C, 500°C, 550°C, and 600°C.
℃, 650℃, minimum 1/4 hour to maximum 32 hours
It was held for up to an hour and quenched. The magnetic properties of these samples are shown in the figure.

従来実施されていた1時間程度の時効保持時間では、6
00℃以上の保持温度で(BH)maxは最高43 M
GOe程度が得られているが、600℃以下の保持温度
では、30 MGOeと効果がない。
With the conventional aging holding time of about 1 hour, 6
(BH)max is maximum 43 M at a holding temperature of 00℃ or higher
Although approximately GOe has been obtained, at a holding temperature of 600° C. or lower, the result is 30 MGOe, which is ineffective.

一方時効保持温度を従来の時効条件く1時間程度の短時
間保持)で決定される最適時効温度(600〜650℃
)よりも低くし、時効保持温度を長くした650℃、時
効保持時間8〜16時間の条件では、 (BH)max
、50MGOeの著しく高い磁石特性が得られている。
On the other hand, the optimum aging temperature (600 to 650℃) is determined by keeping the aging temperature under conventional aging conditions for a short period of about 1 hour
) under the conditions of 650°C and a long aging holding temperature of 8 to 16 hours, (BH)max
, 50MGOe, extremely high magnetic properties were obtained.

この高い磁石特性は、+)(cSa)(c、減磁曲線の
角形性の向上によるものである。
This high magnetic property is due to the improvement in the squareness of the demagnetization curve.

上記のことから、N d −F e−B系における通常
の磁石特性値よりも、明らかに高性能であると判断てき
る(BH)max、45MGOe以上の磁石特性は、4
70℃〜600℃の温度範囲で2時間以上の保持での時
効処理により得られていることがわかる。尚、30時間
以上の処理時間は、工業上著しく不利益となると考えら
れるので、時効保持時間は最長30時間に制限した。
From the above, it can be determined that the magnetic properties of (BH) max, 45MGOe or higher, which are clearly higher in performance than the normal magnet property values in the N d -F e-B system, are 4
It can be seen that this was obtained by aging treatment at a temperature range of 70°C to 600°C for 2 hours or more. Incidentally, since a treatment time of 30 hours or more is considered to be extremely disadvantageous industrially, the aging holding time was limited to a maximum of 30 hours.

以上の実施例では、Nd−Fe−B系磁石についてのみ
述べているが、4πl5(Br)の減少が顕著でない元
素で一部@換(例えば、Pr、C。
In the above embodiments, only Nd-Fe-B magnets are described, but some of the elements with which the decrease in 4πl5(Br) is not significant (for example, Pr, C).

等)しても、45 MGOe以上が得られ(理論的には
Brが13.42に6以上であればよい、)本発明を限
定するものではない。
etc.), 45 MGOe or more can be obtained (theoretically, it is sufficient if Br is 13.42 to 6 or more), but does not limit the present invention.

また、従来の経験から、Nd−Fe−Bの一部にCe、
Pr、Dy、Gd、Ha、Tb等の希土類元素及びYや
Co%N1等の遷移金属を含んでいたとしても、同様の
時効効果の得られることは明らかである。また、本発明
の時効温度範囲で、保持温度を変化させても同様の効果
が期待できる。
In addition, from past experience, it has been found that Ce, part of Nd-Fe-B
It is clear that similar aging effects can be obtained even if rare earth elements such as Pr, Dy, Gd, Ha, and Tb and transition metals such as Y and Co%N1 are included. Furthermore, similar effects can be expected even if the holding temperature is varied within the aging temperature range of the present invention.

本発明について、以上詳しく説明したが、Nd・Fe−
Bを主成分として含有するR2T14B系合金を粉末冶
金法によフて製造する方法において、磁場中圧粉体を焼
結した後、470℃〜600℃の温度範囲で、2〜30
時間時効処理することにより、 (BH)max、45
MGOe以上の極めて高い磁石特性が得られるものであ
り、本発明は工業上非常に有益である。
Although the present invention has been explained in detail above, Nd.Fe-
In a method for manufacturing an R2T14B alloy containing B as a main component by a powder metallurgy method, after sintering a powder compact in a magnetic field, it is heated for 2 to 30 minutes in a temperature range of 470°C to 600°C.
By time aging treatment, (BH)max, 45
The present invention is industrially very useful since extremely high magnetic properties exceeding those of MGOe can be obtained.

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

図は、実施例における焼結体の時効保持時間と磁石特性
の関係を示す0図中・印は470℃、O印は500℃、
0印は550℃、Δ印は600℃、X印は650℃の時
効温度で処理された試料の磁石特性を表す。
The figure shows the relationship between the aging holding time of the sintered body and the magnetic properties in the example.
The mark 0 represents the magnetic properties of the sample treated at an aging temperature of 550°C, the mark Δ represents 600°C, and the mark X represents the magnetic properties of the sample treated at an aging temperature of 650°C.

Claims (1)

【特許請求の範囲】[Claims]  Nd、Fe、Bを主成分として含有するR_2T_1
_4B系磁石(ここで、Rはイットリウム(Y)及び希
土類元素、Tは遷移金属をあらわす。)を粉末冶金法に
よって製造する方法において、磁場中圧粉体を焼結した
後、470℃〜600℃の温度範囲で、2〜30時間時
効処理することにより、(BH)max、45MGOe
以上の磁石特性を得ることを特徴とする希土類磁石の製
造方法。
R_2T_1 containing Nd, Fe, and B as main components
In a method for manufacturing _4B magnets (where R represents yttrium (Y) and a rare earth element, and T represents a transition metal) by a powder metallurgy method, after sintering the green compact in a magnetic field, By aging treatment for 2 to 30 hours in the temperature range of ℃, (BH)max, 45MGOe
A method for manufacturing a rare earth magnet characterized by obtaining the above magnetic properties.
JP61192595A 1986-08-18 1986-08-18 Manufacture of rare earth magnet Pending JPS6347907A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP61192595A JPS6347907A (en) 1986-08-18 1986-08-18 Manufacture of rare earth magnet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61192595A JPS6347907A (en) 1986-08-18 1986-08-18 Manufacture of rare earth magnet

Publications (1)

Publication Number Publication Date
JPS6347907A true JPS6347907A (en) 1988-02-29

Family

ID=16293881

Family Applications (1)

Application Number Title Priority Date Filing Date
JP61192595A Pending JPS6347907A (en) 1986-08-18 1986-08-18 Manufacture of rare earth magnet

Country Status (1)

Country Link
JP (1) JPS6347907A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108637249A (en) * 2018-06-06 2018-10-12 山西大缙华磁性材料有限公司 A kind of neodymium iron boron magnetic body sintering process

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6077960A (en) * 1983-10-03 1985-05-02 Sumitomo Special Metals Co Ltd Permanent magnet and its manufacture
JPS6187825A (en) * 1984-10-05 1986-05-06 Hitachi Metals Ltd Manufacture of permanent magnet material
JPS621204A (en) * 1985-03-13 1987-01-07 Hitachi Metals Ltd Manufacture of permanent magnet

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6077960A (en) * 1983-10-03 1985-05-02 Sumitomo Special Metals Co Ltd Permanent magnet and its manufacture
JPS6187825A (en) * 1984-10-05 1986-05-06 Hitachi Metals Ltd Manufacture of permanent magnet material
JPS621204A (en) * 1985-03-13 1987-01-07 Hitachi Metals Ltd Manufacture of permanent magnet

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108637249A (en) * 2018-06-06 2018-10-12 山西大缙华磁性材料有限公司 A kind of neodymium iron boron magnetic body sintering process

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