JPS61252604A - Manufacture of rare earth magnet - Google Patents
Manufacture of rare earth magnetInfo
- Publication number
- JPS61252604A JPS61252604A JP60093808A JP9380885A JPS61252604A JP S61252604 A JPS61252604 A JP S61252604A JP 60093808 A JP60093808 A JP 60093808A JP 9380885 A JP9380885 A JP 9380885A JP S61252604 A JPS61252604 A JP S61252604A
- Authority
- JP
- Japan
- Prior art keywords
- cooled
- magnet
- didymium
- sintering
- 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.)
- Granted
Links
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
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は希土類磁石の製造方法に関し、特にＮｄ ２
Ｆｅ 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Ｒ、Ｔ、４Ｂ系金属間化
合物磁石の製造方法に関するものである。[Detailed Description of the Invention] [Industrial Field of Application] The present invention relates to a method for manufacturing rare earth magnets, particularly Nd 2
Rare earth metals (R
) and a transition metal (T) and a transition metal (T).
Ｒ−Ｆｅ−Ｂ系磁石の製造方法は２つに大別される。ひ
とつは、溶解している合金を急冷した後。Methods for manufacturing R-Fe-B magnets are roughly divided into two. One is after the molten alloy is rapidly cooled.
時効し、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。他のひとつは、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
は後者の焼結型磁石に関係している。This is a polymer composite magnet manufactured by orienting aged and pulverized magnet powder in a magnetic field. The other type is a sintered magnet, which is manufactured by pulverizing an ingot of a magnetic alloy obtained by melting, shaping it in a magnetic field, and then sintering it. The present invention relates to the latter sintered magnet.
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５９４６００８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、溶解して得られたインゴットを粉砕し、得ら
れた微粉末を成形した圧粉体を、 Ａｒ雰囲気中で焼結
した後、急冷する方法について記述しである。そしてこ
れらの合金には高純度のＮｄが使用されている。Documents related to sintered magnets manufactured by powder metallurgy of R-Fe-B magnets include Japanese Patent Application Laid-Open No. 5946008 and Japanese Society of Applied Magnetics Research 35th Research Meeting Materials "Nd-Fe-B
"New Magnet System" (May 1981). These documents describe a method of pulverizing an ingot obtained by melting, molding the obtained fine powder, sintering it in an Ar atmosphere, and then rapidly cooling it. High purity Nd is used in these alloys.
高純度のＮｄは、 ＰｒとＮｄの分離が容易でないため
に、高価となっている。したがって高純度のＮｄを使用
する上記の従来の焼結型磁石の場合においては、磁石の
原料価格が相当高価になった。また性能的にみて必ずし
も満足すべきものではなかった。High purity Nd is expensive because it is difficult to separate Pr and Nd. Therefore, in the case of the above-mentioned conventional sintered magnet using high-purity Nd, the cost of the raw material for the magnet has become considerably high. Furthermore, performance was not necessarily satisfactory.
したがって本発明の目的は安価で而も性能のよりＲ−Ｆ
ｅ−Ｂ系磁石を提供しようとするものである。Therefore, the object of the present invention is to provide a low cost and high performance R-F
The purpose is to provide an e-B magnet.
本発明者は９種々実験を行なった結果、 Ｐｒ・Ｎｄを
主成分とするジジム（Ｃｅ含有量はＩＱｗｔ％でも可で
あるが、望ましくは５ｗｔ％以下）を磁石用合金原料と
して使用することにより、高純度Ｎｄを使用したＮｄＦ
ｅ−、Ｂ系磁石に比べ、安価で而も高性能な磁石が製造
できることを見出した。合わせて、圧粉体の焼結後、冷
却速度や熱処理をある範囲に制御することにより磁石の
より一層の高性能化が実現できることも見出したのであ
る。As a result of nine different experiments, the present inventor found that by using didymium whose main components are Pr and Nd (Ce content can be IQwt%, but preferably 5wt% or less) as an alloy raw material for magnets. , NdF using high purity Nd
It has been found that it is possible to produce a magnet that is cheaper and has higher performance than e- and B-based magnets. In addition, they discovered that by controlling the cooling rate and heat treatment within a certain range after sintering the green compact, it was possible to achieve even higher performance of the magnet.
すなわち本発明によれば、 Ｒ２Ｔ１４Ｂ系磁石（ここ
でＲはイツトリウム及び希土類元素、Ｔは遷！金属をあ
らねす。）を粉末冶金法によって製造する方法において
、 Ｐｒ、Ｎｄを主成分としたジジムを原料とし′た（
Ｐｒ−Ｎｄ）・Ｆｅ−Ｂ系合金の粉末成形体を、焼結後
５００’Ｃ／ｈｒ以下の冷却速度で徐冷することと焼結
徐冷後３５０℃〜６５０℃の温度で熱処理し急冷するこ
とによって製造することを特徴とする希土類磁石の製造
方法が得られる。That is, according to the present invention, in a method for producing an R2T14B magnet (where R stands for yttrium and a rare earth element, and T stands for a metal) by a powder metallurgy method, didymium containing Pr and Nd as main components is used. was used as raw material (
After sintering, a powder compact of Pr-Nd)/Fe-B alloy is slowly cooled at a cooling rate of 500'C/hr or less, and after sintering and slow cooling, it is heat treated at a temperature of 350°C to 650°C and then rapidly cooled. A method for producing a rare earth magnet is obtained, which is characterized in that it is produced by the following steps.
従来の希土類磁石の例としてＳｍＣｏ系磁石では、原料
の低価格化を安価な希土類金属との一部置換で行なうと
、原料価格の低下率よりも。As an example of conventional rare earth magnets, in the case of SmCo magnets, if the cost of raw materials is reduced by partially replacing them with cheaper rare earth metals, the rate of decline in raw material prices will be greater than the rate of decline in raw material prices.
磁石性能（エネルギー積）の減少率が大きくなるという
傾向を示している。したがって２本発明は原料価格の低
下と磁石の高性能化が同時に達成でき、従来の磁石材料
とは全く異なった傾向を示す発明であり、工業上極めて
有益である。This shows a tendency for the rate of decrease in magnet performance (energy product) to increase. Therefore, the present invention can simultaneously reduce the cost of raw materials and improve the performance of the magnet, exhibiting a completely different tendency from conventional magnet materials, and is extremely useful industrially.
はじめにこの種の磁石合金の粉末冶金法（っいて一般的
に説明すると、その製造工程は、原料の溶解、粉砕、磁
場中配向、圧縮成形、焼結の順に進められる。溶解は、
アーク、高周波等の真空または不活性雰囲気中で行なう
。粉砕は。Firstly, the powder metallurgy method (generally speaking, the manufacturing process for this type of magnetic alloy proceeds in the following order: melting of raw materials, pulverization, orientation in a magnetic field, compression molding, and sintering.
Perform in vacuum or inert atmosphere using arc, high frequency, etc. As for the crushing.
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、鉄乳鉢やロールミル等で行なわれる。微粉砕は、ボ
ールミル、振動ミル、ジェットミル等で行なわれる。磁
界中配向及び圧縮成形は、金型を用いて磁界中で同時に
行なわれるのが通例である。焼結は１０００〜１１５０
℃の範囲で。It is divided into coarse pulverization and fine pulverization, and coarse pulverization is performed using a show crusher, iron mortar, roll mill, etc. Fine pulverization is performed using a ball mill, vibration mill, jet mill, or the like. Orientation in a magnetic field and compression molding are usually performed simultaneously in a magnetic field using a mold. Sintering is 1000-1150
In the range of °C.
不活性雰囲気中で行なわれる。焼結後は、焼結体を急冷
していた。It is carried out in an inert atmosphere. After sintering, the sintered body was rapidly cooled.
以下実施例について具体的に述べる。なおはじめの冷却
速度に関する例においては、比較のために従来の高純度
のＮｄを用いた例を併記しである。Examples will be described in detail below. In the first example regarding the cooling rate, an example using conventional high-purity Nd is also shown for comparison.
実施例１゜
従来例として高純度（９９チ以上）のＮｄとＦｅ、Ｂを
使用し、又本発明の実施例、としてＰｒとＮｄ。Example 1 High purity (99% or higher) Nd, Fe, and B were used as a conventional example, and Pr and Nd were used as an example of the present invention.
比が１対９で純度９７％以上のジジムとＦｅ、Ｂを使用
して、アルゴン雰囲気中で、高周波加熱により、それぞ
れ、 Ｎｄ３３ｗｔ％、 Ｂ１．０ｗｔ％、 Ｆｅ
残部からなるＮｄ−Ｆｅ−Ｂ系合金と、 Ｒ３３ｗｔ％
、Ｂ１．０ｗｔ％、 Ｆｅ残部からなる（Ｐｒ−Ｎｄ
）Ｆｅ−Ｂ系合金のインゴットを得た。Using didymium, Fe, and B with a ratio of 1:9 and a purity of 97% or higher, 33 wt% Nd, 1.0 wt% B, and Fe were produced by high-frequency heating in an argon atmosphere.
Nd-Fe-B alloy consisting of the balance and R33wt%
, B1.0wt%, the remainder being Fe (Pr-Nd
) An ingot of Fe-B alloy was obtained.
次にこのインゴットを粗粉砕した後、ボールミルにて平
均粒径約３μｍに粉砕した。 次にこの粉末を３０ Ｋ
Ｏｅの磁界中、 １ｔｏｎ／ ２の圧力でα
成形した。この成形体を１０８０℃で１時間真空保持し
た後、 Ａｒ雰囲気中で１時間保持し焼結した。Next, this ingot was coarsely ground, and then ground to an average particle size of about 3 μm using a ball mill. Then this powder was heated to 30K
α molding was performed at a pressure of 1 ton/2 in a magnetic field of Oe. This molded body was held in vacuum at 1080°C for 1 hour and then held in an Ar atmosphere for 1 hour to sinter.
その後、５０℃〜５００′Ｃ／／ｈｒの冷却速度で約３
００’Ｃまで徐冷した。After that, the cooling rate of 50°C to 500'C//hr is approximately 3
It was slowly cooled down to 00'C.
その焼結体の磁石特性を第１図に示す。従来のＮｄ１ｉ
’ｅ−Ｂ系磁石に比較し１本発明による（Ｐｒ・冷却速
度でミーは高い値を示し、又（ＢＨ）ｒｒｌａｘは著し
く高い値が得られている。（図中、○印は（Ｐｒ−Ｎｄ
）・Ｆｅ−Ｂ系磁石を、Δ印はＮｄ−Ｆｅ−Ｂ系磁石を
表わす。）
以下余日
実施例２゜
ＰｒとＮｄの比が６対７で純度９０％以上のジジムとＦ
ｅとフェロボロンを使用して、実施例１と同様にして、
Ｒ３５ｗｔ％、 Ｂ１．１ｗｔ％、 Ｆｅ残部からな
る（Ｐｒ−Ｎｄ）・Ｆｅ４系合金のインゴットを得た。Figure 1 shows the magnetic properties of the sintered body. Conventional Nd1i
Compared to the 'e-B series magnet, the present invention shows a high value for (Pr/cooling rate) and a significantly high value for (BH)rrlax. (In the figure, the ○ marks indicate (Pr -Nd
)・Fe-B type magnet, and Δ mark represents Nd-Fe-B type magnet. ) Example 2 for the rest of the day: Didym and F with a Pr:Nd ratio of 6:7 and a purity of 90% or more
In the same manner as in Example 1 using e and ferroboron,
An ingot of a (Pr-Nd)/Fe4 alloy consisting of 35 wt% R, 1.1 wt% B, and the balance Fe was obtained.
次にこのインゴットを実施例１と同様にして粉砕、磁場
成形し、成形体を得た。この成形体を１０６０℃で１時
間真空保持した後、 Ａｒ中で１時間保持し、焼結した
。その後、 １００１：／ｈｒの冷却速度で２００℃ま
で徐冷した。この焼結体を３００℃〜７００℃の温度で
各１時間熱処理した後急冷した。Next, this ingot was crushed and magnetically molded in the same manner as in Example 1 to obtain a molded body. This molded body was held in vacuum at 1060° C. for 1 hour, and then held in Ar for 1 hour to sinter it. Thereafter, it was slowly cooled to 200° C. at a cooling rate of 1001:/hr. This sintered body was heat treated at a temperature of 300° C. to 700° C. for 1 hour each and then rapidly cooled.
その試料の磁石特性を第２図に示す。熱処理温度が３５
０℃〜６５０℃の範囲で高い（ＢＨ）ｍａｘが得られて
いる。６５０℃近傍の熱処理でＩＨＣが減少したにもか
かわらずｔ （ＢＨ）ｍａＸが減少していないのは、減
磁曲線の角型性の向上によるものである。Figure 2 shows the magnetic properties of the sample. Heat treatment temperature is 35
High (BH)max has been obtained in the range of 0°C to 650°C. The reason why t (BH)maX did not decrease despite the decrease in IHC due to the heat treatment at around 650° C. is due to the improvement in the squareness of the demagnetization curve.
以上の実施例においては、ジジムの純度としてＰｒとＮ
ｄで表記してきたが、ジジムは精製度の低いＰｒとＮｄ
の混合物である。したがってこれらの不純物とし−Ｃは
、他の希土類元素（例えばＬａ、Ｃｅ、Ｓｍ等）があげ
られる。 この中で最も多く混在するＲ元素はＣｅであ
わ、Ｒ中のＣｅ混入量が１０ｗｔ ％以下であれば９本
発明の効果は期待されるが、 ５ｗ１％以下であること
が望ましい。In the above examples, the purity of didymium is Pr and N.
Although it has been expressed as d, didymium is Pr and Nd with low purity.
It is a mixture of Therefore, these impurities -C may include other rare earth elements (for example, La, Ce, Sm, etc.). Among these, the most common R element is Ce, and the effects of the present invention can be expected if the amount of Ce mixed in R is 10wt% or less, but it is preferably 5w1% or less.
また１合金原料の製造において溶解時に、ＰｒとＮｄを
一緒に溶解しても同様な磁気特性に対する熱処理の効果
が期待できるものである。更に、 Ｐｒ−Ｆｅ−Ｂ系合
金とＮｄ−Ｆｅ−Ｂ系合金の合金粉末成形体を焼結した
ものについても同様な効果が期待できる。すなわち、焼
結体が、 ＰｒとＮｄを主成分としたＲ２Ｆｅ１４Ｂ系
合金であれば、同様な熱処理の効果が実現されるもので
ある。Furthermore, even if Pr and Nd are melted together during melting in the production of a single alloy raw material, similar heat treatment effects on magnetic properties can be expected. Further, similar effects can be expected from sintered alloy powder compacts of Pr-Fe-B alloy and Nd-Fe-B alloy. That is, if the sintered body is an R2Fe14B alloy containing Pr and Nd as main components, similar heat treatment effects can be achieved.
以上の説明から分るように、 Ｒ２Ｆｅ、、Ｂ系磁石の
粉末冶金法による製造において、安価に製造されるジジ
ムを合金の原料として使用することによって、磁石原料
の低価格化ばかりでなく。As can be seen from the above description, in the production of R2Fe, B-based magnets by powder metallurgy, the use of didymium, which is produced at low cost, as an alloy raw material not only reduces the price of the magnet raw material.
焼結後の冷却条件や熱処理温度を制御することにより、
高性能な磁石特性が得られる。By controlling the cooling conditions and heat treatment temperature after sintering,
High performance magnetic properties can be obtained.
第１図は実施例１におけるＮｄ−Ｐｅ−Ｂ系磁石と（Ｐ
ｒ−Ｎｄ）・Ｆｅ−Ｂ系磁石の焼結後の冷却速度と磁気
特性の関係を示す図、第２図は実施例２における（Ｐｒ
−Ｎｄ）・Ｆｅ−Ｂ系磁石の熱処理温度と磁気特性の関
係を示す図である。
気４図
重加速度（’Ｃ／ｈｒ）Figure 1 shows the Nd-Pe-B magnet in Example 1 and (P
Figure 2 is a diagram showing the relationship between the cooling rate and magnetic properties after sintering of a (Pr-Nd)/Fe-B magnet in Example 2.
FIG. 3 is a diagram showing the relationship between heat treatment temperature and magnetic properties of a -Nd)/Fe-B magnet. Ki 4 heavy acceleration ('C/hr)
Claims (1)
ム及び希土類元素、Ｔは遷移金属をあられす。）を粉末
冶金法によって製造する方法において、Ｐｒ、Ｎｄを主
成分としたジジムを原料とした（Ｐｒ・Ｎｄ）・Ｆｅ・
Ｂ系合金の粉末成形体を、焼結後５００℃／＿ｈ＿ｒ以
下の冷却速度で徐冷することと焼結徐冷後３５０℃〜６
５０℃の温度で熱処理し急冷することによって製造する
ことを特徴とする希土類磁石の製造方法。1. In the method of manufacturing R_2T_1_4B magnets (where R stands for yttrium and rare earth elements, and T stands for transition metals) using powder metallurgy, didymium containing Pr and Nd as the main components (Pr. Nd)・Fe・
After sintering, the powder compact of B-based alloy is slowly cooled at a cooling rate of 500°C/_h_r or less, and after sintering and slow cooling, it is cooled at 350°C to 6.
A method for producing a rare earth magnet, characterized in that it is produced by heat treatment at a temperature of 50°C and rapid cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60093808A JPS61252604A (en) | 1985-05-02 | 1985-05-02 | Manufacture of rare earth magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60093808A JPS61252604A (en) | 1985-05-02 | 1985-05-02 | Manufacture of rare earth magnet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61252604A true JPS61252604A (en) | 1986-11-10 |
| JPH0426524B2 JPH0426524B2 (en) | 1992-05-07 |
Family
ID=14092702
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60093808A Granted JPS61252604A (en) | 1985-05-02 | 1985-05-02 | Manufacture of rare earth magnet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61252604A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62120457A (en) * | 1985-11-21 | 1987-06-01 | Tdk Corp | Manufacture of permanent magnet |
| EP1011113A3 (en) * | 1998-12-11 | 2000-11-15 | Shin-Etsu Chemical Co., Ltd. | Method for the preparation of a rare earth permanent magnet |
| CN112750613A (en) * | 2020-03-31 | 2021-05-04 | 河北泛磁聚智电子元件制造有限公司 | Preparation method of ultrahigh maximum magnetic energy product sintered samarium-cobalt magnet |
-
1985
- 1985-05-02 JP JP60093808A patent/JPS61252604A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62120457A (en) * | 1985-11-21 | 1987-06-01 | Tdk Corp | Manufacture of permanent magnet |
| EP1011113A3 (en) * | 1998-12-11 | 2000-11-15 | Shin-Etsu Chemical Co., Ltd. | Method for the preparation of a rare earth permanent magnet |
| CN112750613A (en) * | 2020-03-31 | 2021-05-04 | 河北泛磁聚智电子元件制造有限公司 | Preparation method of ultrahigh maximum magnetic energy product sintered samarium-cobalt magnet |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0426524B2 (en) | 1992-05-07 |
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