JPS6181604A - Preparation of rare earth magnet - Google Patents

Preparation of rare earth magnet

Info

Publication number
JPS6181604A
JPS6181604A JP59183757A JP18375784A JPS6181604A JP S6181604 A JPS6181604 A JP S6181604A JP 59183757 A JP59183757 A JP 59183757A JP 18375784 A JP18375784 A JP 18375784A JP S6181604 A JPS6181604 A JP S6181604A
Authority
JP
Japan
Prior art keywords
powder
alloy
rare earth
sintering
magnetic
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
JP59183757A
Other languages
Japanese (ja)
Other versions
JPH0344405B2 (en
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 JP59183757A priority Critical patent/JPS6181604A/en
Publication of JPS6181604A publication Critical patent/JPS6181604A/en
Publication of JPH0344405B2 publication Critical patent/JPH0344405B2/ja
Granted 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

Landscapes

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

Abstract

PURPOSE:To improve magnetic characteristics by sintering after the powder of Nd, Fe, B system alloy whose main formation phase is Nd2Fe14B is mixed with the fine powder of Ce, Fe, B system alloy and is molded. CONSTITUTION:Nd2Fe14B system magnetic alloy containing Nd, Fe and B as the main components is manufactured by powder metallurgy. In this process, the powder of Nd, Fe, B system magnetic alloy is mixed with 0-18wt% (0 is not included) of the powder of Ce, Fe, B system magnetic alloy whose main formation phase is Ce2Fe14B and then is molded. This molded substance is sintered and represents improved magnetic characteristics as a product.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 ° 本発明はNd 2 F e 14 B系合金磁石で
代表される希土類金属(R)と遷移金属(T)とからな
るR2T14B系金属間化合物磁石の製造方法、特にN
d、Fe、Bを主成分とする永久磁石の粉末冶金法よる
製造方法に関する。
[Detailed Description of the Invention] [Field of Industrial Application] ° The present invention is directed to an R2T14B intermetallic compound consisting of a rare earth metal (R) and a transition metal (T), typified by Nd 2 Fe 14 B alloy magnets. Magnet manufacturing method, especially N
The present invention relates to a method for producing a permanent magnet containing d, Fe, and B as main components by powder metallurgy.

〔従来技術〕[Prior art]

一般にR,Fe’、B系磁石の製造方法については2つ
の方法に大別される。ひとつは溶解しているR1FeJ
B系合金を急冷しだ後9時効して粉砕した磁石粉末を磁
場中で配向して製造する方法であり、これによって所謂
高分子複合型磁石が得られる。一方はR,Fe、B系磁
石合金を溶解してインが、1・を作り。
In general, methods for manufacturing R, Fe', and B-based magnets are roughly divided into two methods. One is dissolved R1FeJ
This is a method of manufacturing a B-based alloy by quenching it, aging it for 9 hours, and then pulverizing it, and orienting it in a magnetic field, thereby producing a so-called polymer composite magnet. On the other hand, R, Fe, and B-based magnetic alloys are melted to create In and 1.

このインゴットを微粉砕した後、磁場中で成形し。After pulverizing this ingot, it is molded in a magnetic field.

焼結して製造する方法であり、これによって焼結型磁石
が得られる。なお、粉末冶金法によって製造されるR、
Fe’、B系の焼結型磁石に関しては特開昭59−46
008に記載されている。
This is a method of manufacturing by sintering, and a sintered magnet is obtained by this method. In addition, R manufactured by powder metallurgy method,
For Fe', B-based sintered magnets, see JP-A-59-46.
008.

R! Fe r B系磁石の粉末冶金法による製造工程
は溶解、粉砕、磁場中配向、圧縮成形、焼結9時効の順
に進められる。R9Fe、B系磁石合金の)答辞は真空
あるいは不活性雰囲気中で、アーク又は高周波加熱によ
って行われる。粉砕は粗粉砕と微粉砕に分けられ、粗粉
砕はノヨークラッ/ヤー、鉄乳鉢やロールミル等で行わ
れる。微粉砕はボールミル。
R! The manufacturing process of Fer B magnets by powder metallurgy is carried out in the following order: melting, pulverization, orientation in a magnetic field, compression molding, sintering, and 9 aging. (R9Fe, B-based magnet alloy) is heated in a vacuum or inert atmosphere by arc or high-frequency heating. Grinding is divided into coarse grinding and fine grinding, and coarse grinding is carried out in a noyo clay/yer, iron mortar, roll mill, etc. Fine grinding is done using a ball mill.

撮動ミル、ソエットミル等で行われる。磁場中配向及び
圧縮成形は金型を用いて磁場中で同時に行われる。焼結
は不活性雰囲気中で温度1ooo〜1150℃の範囲で
行われる。また時効は必要に応じて温度300〜900
℃程度の温度で行われる。
It is carried out in photographic mills, soet mills, etc. Orientation in a magnetic field and compression molding are performed simultaneously in a magnetic field using a mold. Sintering is carried out in an inert atmosphere at temperatures ranging from 100°C to 1150°C. In addition, aging is performed at a temperature of 300 to 900 as necessary.
It is carried out at a temperature of about ℃.

一般に焼結型磁石では焼結温度を低下させる方向にもっ
ていくことによって減磁特性の角形性及び保磁力(Ho
)が向上する。またR、Fe+B系合金は非常に反応性
に富んでおり、微粉末状態での取り扱ンこノ い及び成形体の焼結過程での酸化などによって、焼M’
lの低下、磁気特性の低下及びバラツキを生ずる原因と
なる。従来、焼結型磁石の特性向上のため、前述のよう
に焼結はヘリウム、アルコゝンなどの不活性雰囲気中で
行われ、さらに不純ガスの影響を軽減するために、粉末
成形体の外部にケ9.ターを設置して焼結する場合もあ
るが+ R+Fe、B系合金においては磁石特性上の顕
著な効果をもたらすて至っていない。
In general, in sintered magnets, by lowering the sintering temperature, the squareness of the demagnetizing characteristic and the coercive force (Ho
) will be improved. In addition, R, Fe+B alloys are highly reactive, and when handled in a fine powder state or oxidized during the sintering process of compacts, sintered M'
This causes a decrease in l, a decrease in magnetic properties, and variations in magnetic properties. Conventionally, in order to improve the characteristics of sintered magnets, sintering was performed in an inert atmosphere such as helium or alcohol, as described above, and in order to further reduce the effects of impurity gases, sintering was performed outside the powder compact. Nike 9. In some cases, sintering is carried out by installing a magnet, but this has not yet produced a significant effect on magnetic properties in +R+Fe and B-based alloys.

口発明の目的〕 本発明の目的はR、F e r B  系磁石合金を用
いて。
OBJECT OF THE INVENTION The object of the present invention is to use an R, Fer B-based magnetic alloy.

磁石特性上の顕著な効果をもたらす希±急磁石を製造す
ることのできる希土類磁石の製造方法を提供することで
ある。
It is an object of the present invention to provide a method for manufacturing a rare earth magnet that can manufacture a rare magnet that has a remarkable effect on magnetic properties.

〔発明の構成〕[Structure of the invention]

本発明ではNd 2 F e 14 Bを主生成相とす
るNd、Fe、Bス巳 系合金粉末にこの合金よシも融点が低くかつ酸秋作用の
大きいCe HF e g B系合金の微粉末を混合し
て成形した後この成形体を焼結する。
In the present invention, a fine powder of a Ce HF e g B alloy, which has a lower melting point than this alloy and has a large acid fall effect, is added to the Nd, Fe, and B alloy powder whose main phase is Nd 2 Fe 14 B. After mixing and molding, this molded body is sintered.

化学的に活性で低融点なCe、Fe、B系合金微粉末が
Nd ! Fe r B系合金微粉末中に分散された成
形体中では、焼結過程で磁気特性の高いNd合金よシも
Ce合金の酸化が選択的に行われ、結晶粒界の整った磁
石特性の高い焼結体となる。
Chemically active and low melting point Ce, Fe, B based alloy fine powder is Nd! In a compact dispersed in Fe r B alloy fine powder, the sintering process selectively oxidizes the Ce alloy as well as the Nd alloy, which has high magnetic properties, resulting in good magnetic properties with well-organized grain boundaries. It becomes a high-quality sintered body.

〔発明の実施例〕[Embodiments of the invention]

(1)実施例1 高純度のNd 、Ce 、Fe 、Bを使用して、アル
コゝン雰囲するイ/コ゛ットをそれぞれ得た。これらN
d合録びCe合金をそれぞれ粗粉砕して、 Ce合金粉
末をNd合金粉末に対して5重量・q−セント混合した
後。
(1) Example 1 High-purity Nd, Ce, Fe, and B were used to obtain an alkone atmosphere atmosphere. These N
After coarsely pulverizing each of the d-combined Ce alloys and mixing 5 weight/q cents of Ce alloy powder with the Nd alloy powder.

ボールミルを用いて平均粒径3μmに湿式粉砕した。Wet milling was performed using a ball mill to give an average particle size of 3 μm.

次にこの微粉末を10 koeの磁界中において1 t
on//cn12の圧力で成形した。さらにこの圧粉体
を温度1060℃で1時間真空中で加熱し2次に同じ温
度で1時間アルゴンガス雰囲気中に保持した。そ澄・?
−セント含む希土類磁石と従来の希土類磁石の特性を表
に示す。
Next, this fine powder was placed in a magnetic field of 10 koe for 1 t.
Molding was carried out at a pressure of on//cn12. Further, this green compact was heated in vacuum at a temperature of 1060° C. for 1 hour, and then held in an argon gas atmosphere at the same temperature for 1 hour. Sosumi?
The table shows the characteristics of rare earth magnets containing cents and conventional rare earth magnets.

表 5重量係  7,412.8  1 38   ’  
10  1上記の表から明らかな通9 、 Ce、Fe
、B系合金粉末を5重量パーセント混合することによっ
て焼結温度が低下し、さらにこのようにして製造された
希土類磁石は高い磁石特性を示している。
Table 5 Weight 7,412.8 1 38'
10 1 From the table above, it is clear that 9, Ce, Fe
By mixing 5% by weight of B-based alloy powder, the sintering temperature is lowered, and the rare earth magnet produced in this way exhibits high magnetic properties.

(11)実施例2 実施例1において製造したNd+s、sF” 78B6
.5及びCe 15.5F878B6.5の組成比を有
するR2Fe14Bを主生成相とするインコゝットをそ
れぞれ粗粉砕して、 Nd合金粉末及びCe合金粉末を
得た。Nd合金粉末に対してCe合金粉末をO〜20重
量iE−セントまで混合して、ボールミルを用いて平均
粒径約3μmに粉砕した。これら混合粉末をl OkO
eの磁界中において1 ton/crn2の圧力で成形
し、これら圧粉体を温度1080’Cで1時間真空中で
加熱し、さらに同じ温度で3時間アルゴンガス雰囲気中
に保持した。その後100℃/時間以下の冷却速度で除
冷した。
(11) Example 2 Nd+s,sF"78B6 manufactured in Example 1
.. Nd alloy powder and Ce alloy powder were obtained by coarsely pulverizing incots whose main phase was R2Fe14B having a composition ratio of 5 and Ce 15.5F878B6.5. Ce alloy powder was mixed with Nd alloy powder to a weight of 0 to 20 iE-cents, and ground to an average particle size of about 3 μm using a ball mill. These mixed powders are l OkO
The compacts were heated in a vacuum at a temperature of 1080'C for 1 hour, and then kept in an argon gas atmosphere at the same temperature for 3 hours. Thereafter, it was gradually cooled at a cooling rate of 100° C./hour or less.

このよう4CLで得られた試料を温度550℃にむ希土
類磁石の特性を調べたところ第1図(a)〜(c)まず
)の間で希土類磁石の特性の向上が認められる。
When the characteristics of the rare earth magnet were investigated by heating the sample obtained by 4CL to a temperature of 550 DEG C., it was found that the characteristics of the rare earth magnet improved between (a) to (c) in FIG. 1).

このように、 Nd2Fe14B系磁石の粉末冶金法に
よる製造において、Na、FetB系合金粉末にCe 
+ F e HB系合金粉末を混合分散させた成形体を
焼結することは著しい磁石特性の増加を実現させること
ができる。
In this way, in the production of Nd2Fe14B magnets by powder metallurgy, Ce is added to Na and FetB alloy powders.
+F e By sintering a compact in which HB-based alloy powder is mixed and dispersed, a significant increase in magnetic properties can be realized.

〔発明の効果〕〔Effect of the invention〕

本発明を以上詳しく説明したが、 Nd、Fe、Bを主
成分とするNd 2 Fe 、4 B系磁石合金を粉末
冶金法によって製造する方法において、 Na、Fe、
B系合金粉末e に対し、伽2Fe14Bを主生成相とするCe 、Fe
 、B系磁石合金粉末を0〜18重量%(0を含まず)
混合した成形体を焼結する方法によシ著しく優れた磁石
材料が得られる。
The present invention has been described in detail above, but in a method for producing a Nd 2 Fe, 4 B-based magnetic alloy containing Nd, Fe, and B as main components by a powder metallurgy method, Na, Fe,
Ce, Fe with Ka2Fe14B as the main phase for B-based alloy powder e
, 0 to 18% by weight of B-based magnet alloy powder (not including 0)
By sintering the mixed compact, a significantly superior magnetic material can be obtained.

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

第1図(a)乃至(c)はそれぞれNd 15.5 ”
 78 B 6.5 の組成をCe 15.5Fe78
 B6.Sの組成合金粉末との混合比と最大エネルギー
積、残留磁束音度及び伯富こ力との関係で示した図であ
る。
Figures 1(a) to (c) are each Nd 15.5''
78 B 6.5 composition as Ce 15.5Fe78
B6. It is a diagram showing the relationship between the mixing ratio of S with the composition alloy powder, maximum energy product, residual magnetic flux sonicity, and Hakutomi force.

Claims (1)

【特許請求の範囲】[Claims] 1、Nd、Fe、Bを主成分とするNd_2Fe_1_
4B系磁石合金を粉末冶金法によって製造する方法にお
いて、Nd、Fe、B系磁石合金粉末に対してCe_2
Fe_1_4Bを主生成相とするCe、Fe、B系磁石
合金粉末を0乃至18重量パーセント(0を含まず)混
合した成形体を焼結することを特徴とする希土類磁石の
製造方法。
1, Nd_2Fe_1_ whose main components are Nd, Fe, and B
In a method for producing a 4B-based magnet alloy by powder metallurgy, Ce_2 is added to Nd, Fe, and B-based magnet alloy powder.
A method for producing a rare earth magnet, which comprises sintering a molded body containing 0 to 18 weight percent (excluding 0) of Ce, Fe, and B-based magnet alloy powder containing Fe_1_4B as the main phase.
JP59183757A 1984-09-04 1984-09-04 Preparation of rare earth magnet Granted JPS6181604A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59183757A JPS6181604A (en) 1984-09-04 1984-09-04 Preparation of rare earth magnet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59183757A JPS6181604A (en) 1984-09-04 1984-09-04 Preparation of rare earth magnet

Publications (2)

Publication Number Publication Date
JPS6181604A true JPS6181604A (en) 1986-04-25
JPH0344405B2 JPH0344405B2 (en) 1991-07-05

Family

ID=16141443

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59183757A Granted JPS6181604A (en) 1984-09-04 1984-09-04 Preparation of rare earth magnet

Country Status (1)

Country Link
JP (1) JPS6181604A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4981513A (en) * 1987-05-11 1991-01-01 Union Oil Company Of California Mixed particulate composition for preparing rare earth-iron-boron sintered magnets
US5015306A (en) * 1987-05-11 1991-05-14 Union Oil Company Of California Method for preparing rare earth-iron-boron sintered magnets
US5015304A (en) * 1987-05-11 1991-05-14 Union Oil Company Of California Rare earth-iron-boron sintered magnets
US5055129A (en) * 1987-05-11 1991-10-08 Union Oil Company Of California Rare earth-iron-boron sintered magnets
CN106920618A (en) * 2017-03-24 2017-07-04 南京理工大学 A kind of ferrocerium boron magnet alloy band for improving coercivity and magnetic energy product

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109972027A (en) * 2018-12-24 2019-07-05 南昌航空大学 A method for preparing anisotropic CeFeB permanent magnet alloy by adding low melting point PrCu intergranular phase

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5964739A (en) * 1982-09-03 1984-04-12 ゼネラルモーターズコーポレーション High energy rare earth metal-transition metal magnetic alloy
JPS5989401A (en) * 1982-11-15 1984-05-23 Sumitomo Special Metals Co Ltd Permanent magnet

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5964739A (en) * 1982-09-03 1984-04-12 ゼネラルモーターズコーポレーション High energy rare earth metal-transition metal magnetic alloy
JPS5989401A (en) * 1982-11-15 1984-05-23 Sumitomo Special Metals Co Ltd Permanent magnet

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4981513A (en) * 1987-05-11 1991-01-01 Union Oil Company Of California Mixed particulate composition for preparing rare earth-iron-boron sintered magnets
US5015306A (en) * 1987-05-11 1991-05-14 Union Oil Company Of California Method for preparing rare earth-iron-boron sintered magnets
US5015304A (en) * 1987-05-11 1991-05-14 Union Oil Company Of California Rare earth-iron-boron sintered magnets
US5055129A (en) * 1987-05-11 1991-10-08 Union Oil Company Of California Rare earth-iron-boron sintered magnets
CN106920618A (en) * 2017-03-24 2017-07-04 南京理工大学 A kind of ferrocerium boron magnet alloy band for improving coercivity and magnetic energy product

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JPH0344405B2 (en) 1991-07-05

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