JPS62167842A - Production of rare earth magnet - Google Patents
Production of rare earth magnetInfo
- Publication number
- JPS62167842A JPS62167842A JP61007206A JP720686A JPS62167842A JP S62167842 A JPS62167842 A JP S62167842A JP 61007206 A JP61007206 A JP 61007206A JP 720686 A JP720686 A JP 720686A JP S62167842 A JPS62167842 A JP S62167842A
- Authority
- JP
- Japan
- Prior art keywords
- stage
- temp
- sintering
- rare earth
- sintered body
- 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
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
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
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、 Ｎｄ−Ｆｅｆ系永久磁石を代表とする希土
類金属（Ｒ）と遷移金属（Ｔ）とからなるＲ２Ｔ１４Ｂ
系金属間化合物の製造方法でろって、特にＮｄ−Ｆｅ−
Ｂを主成分とする永久磁石を粉末冶金法によって製造す
る場合の磁石特性の改善に関するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention provides R2T14B made of rare earth metal (R) and transition metal (T), typified by Nd-Fef permanent magnets.
In particular, Nd-Fe-
The present invention relates to improvement of magnetic properties when a permanent magnet containing B as a main component is manufactured by a powder metallurgy method.
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。一方は、溶解している合金を超急冷した
薄帯を使用して製造される液体急冷法である。他方は、
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。Methods for manufacturing R-Fe-B magnets are roughly divided into two methods. One is the liquid quenching method, which uses a thin ribbon of super-quenched molten alloy. On the other hand,
This is a sintered magnet manufactured by pulverizing an ingot of a magnetic alloy obtained by melting, molding it in a magnetic field, and then sintering it.
Ｒ−Ｆａｉ系磁面磁石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は特開昭５９−４６００８号
公報や日本応用磁気学会第３５回研究会資料「Ｎｄ−Ｆ
ｅ−Ｂ面断磁石」（昭和５９年５月）がある。Documents related to sintered magnets manufactured by the R-Fai magnetic surface magnet powder metallurgy method include Japanese Patent Application Laid-open No. 59-46008 and Japanese Society of Applied Magnetics 35th Research Meeting Materials “Nd-F
e-B section magnet" (May 1981).
前者には、成形体を焼結後、放冷すると記載されている
のみであり、焼結後の熱処理条件の規定はなされていな
い。また後者には成形体を焼結した後、６００℃近傍の
熱処理でＩＨＣの増加することが記載されている。一方
１日本金属学会春期大会一般講演概要（１９８５，４，
Ｐ、 ３４６ ） Ｐ−Ｆｅ−Ｂ系永久磁石合金の熱処
もにおいては、１０００℃以下での熱処理について記述
しである。しかしながら、これらの熱処理は、１〜２段
の時効処理に関するものでアシ、本発明とは全く異なる
ものである。The former only states that the molded body is left to cool after sintering, but does not specify the conditions for heat treatment after sintering. The latter also describes that after sintering a molded body, heat treatment at around 600° C. increases IHC. On the other hand, 1 Summary of General Lectures at the Spring Conference of the Japan Institute of Metals (1985, April,
P, 346) Regarding heat treatment of P-Fe-B permanent magnet alloy, heat treatment at 1000°C or lower is described. However, these heat treatments relate to one or two stages of aging treatment and are completely different from the present invention.
本発明者は２種々実験を行なった結果、Ｎｄ−Ｆｅ−Ｂ
を主成分としたＲ２Ｔ１４Ｂ系磁石焼結体を多段時効す
ることにより、更に高い磁石特性の得られることを発見
した。As a result of two different experiments, the inventor found that Nd-Fe-B
It has been discovered that even higher magnetic properties can be obtained by subjecting an R2T14B magnet sintered body containing R2T14B as a main component to multi-stage aging.
一般に１本系磁石の粉末冶金法による製造工程は、溶解
、粉砕、磁界中配向、圧縮成形、焼結。Generally, the manufacturing process of single magnets using powder metallurgy includes melting, crushing, orientation in a magnetic field, compression molding, and sintering.
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１通常行なわれる。They proceed in the order of the statute of limitations. Melting is usually carried out in a vacuum or inert atmosphere, such as with a high frequency arc.
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
なわれる。微粉砕は、ゴールミル。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 is done using a goal mill.
振動ミル、ジェットミル等で行なわれる。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なわれるの
が通例である。焼結は１０００〜１１５０℃の範囲で、
不活性雰囲気中で行われる。This is done using a vibration mill, jet mill, etc. Magnetic field orientation and compression molding are usually performed simultaneously in a magnetic field using a mold. Sintering is in the range of 1000 to 1150°C,
It is carried out in an inert atmosphere.
時効は６００℃近傍の温度で行なわれる。Aging is performed at a temperature around 600°C.
本発明者等は、磁石焼結体の時効条件を適正に制御する
ことにより、高い磁石特性を得るものであること本発明
者は発見した。The present inventors have discovered that high magnetic properties can be obtained by appropriately controlling the aging conditions of the magnet sintered body.
本発明はＮｄ−Ｆｅ−Ｂを主成分とするＲ２Ｔ１４Ｂ系
磁石（但しＲはイツトリウムおよび希土類元素、Ｔは遷
移金属）において原料を溶解、粉砕機で粉砕し。In the present invention, raw materials are melted in an R2T14B magnet whose main component is Nd-Fe-B (where R is yttrium and a rare earth element, and T is a transition metal), and then pulverized using a pulverizer.
ついでこれを磁界中成形後時効処理を少くとも３段以上
行う多段時効処理を行うもので、この時効処゛埋の初段
の開始温度を１０００℃以上（焼結温度以下）、最終段
を４００℃から６５０℃で行い保持力ＩＨＣが９ ＫＯ
ｅ以上、エネルギー積（ＯＨ）ｍａｘが３７ ＭＧａｕ
ｓｓ Ｏｅ以上を得た。This is then subjected to a multi-stage aging treatment in which aging treatment is performed in at least three stages after forming in a magnetic field, with the starting temperature of the first stage of aging treatment being 1000°C or higher (below the sintering temperature) and the final stage being 400°C. The holding power IHC was 9 KO.
e or more, energy product (OH) max is 37 MGau
Obtained ss Oe or higher.
１、 純度９８％のＮｄと、高純度のＦｅ４″ｅ便用し
。1. Uses 98% pure Nd and high purity Fe4''e.
Ｎｄが３４ｗｔ％、Ｂが１．１ ｗｊ％、残部Ｆｅとな
るように、Ａｒ雰囲気中で高周波加熱によりインゴット
を作製した。An ingot was produced by high-frequency heating in an Ar atmosphere so that Nd was 34 wt%, B was 1.1 wj%, and the balance was Fe.
次にこの合金を粗粉砕した後、ボールミルにて平均粒径
約３μｍに粉砕した。この粉末を１０ ＫＯｅの磁界中
１ｔｏｎ／Ｊの圧力で成形した。この成形体を焼結温度
１０８０℃で真空中１時間保持した後。Next, this alloy was coarsely ground, and then ground to an average particle size of about 3 μm using a ball mill. This powder was compacted at a pressure of 1 ton/J in a magnetic field of 10 KOe. After holding this molded body in vacuum at a sintering temperature of 1080°C for 1 hour.
Ａｒ中１時間保持し、焼結し、急冷した。It was held in Ar for 1 hour, sintered, and quenched.
次にこの焼結体を、９００℃、９５０℃、 ｉｏｏ。Next, this sintered body was heated at 900°C and 950°C.
℃、１０５０℃、１０８０℃の各温度を時効開始温度と
して夫々１時間保持した後、約１００℃ずつ温度を降下
させながら、各温度で１時間ずつ保持し、５００℃まで
多段時効処理を行なった。その結果を第１図に示す。ま
た第３図に本実施例の時効開始温度１０８０℃の多段時
効処理の加熱冷却・ぞター／を示す。また、比較のため
に、同様の方法で作製した焼結体を、良好とされている
６００℃で１時間時効を行なった時の特性は、第１図に
示すようにＢｒ １２．８ＫＧ 、 ＩＨＣ７，ＯＫＯ
ｅ 、 （ＢＨ）ｍａｘ。℃, 1050℃, and 1080℃ as aging starting temperatures for 1 hour, and then decreasing the temperature by about 100℃ and holding each temperature for 1 hour to perform multi-stage aging treatment up to 500℃. . The results are shown in FIG. Further, FIG. 3 shows the heating, cooling and drying of the multi-stage aging treatment at an aging start temperature of 1080° C. in this example. For comparison, a sintered body produced by the same method was aged for 1 hour at 600°C, which is considered to be good. As shown in Figure 1, the properties were Br 12.8KG, IHC7 ,OKO
e, (BH)max.
３５、０ Ｍ−Ｇ・Ｏｅでｈつだ。35, 0 M-G・Oe and h.
多段時効開始温度を１０００℃から焼結温度の範囲に設
定することにより、磁石特性は著しく向上している。By setting the multi-stage aging start temperature in the range from 1000° C. to the sintering temperature, the magnetic properties are significantly improved.
２、実施例１で作製した焼結体を使用し、焼結温度であ
る１０８０℃から多段時効を開始し、約１００℃ずつ温
度を降下させながら、各温度で１時間ずつ保持し、最終
多段時効処理温度を４００℃から８００℃までの範囲で
変化させて多段時効を行なりた。その時の最終多段時効
処理温度と磁石特性の関係を第２図に示す。2. Using the sintered body produced in Example 1, start multi-stage aging from the sintering temperature of 1080°C, lower the temperature by approximately 100°C, hold each temperature for 1 hour, and complete the final multi-stage aging. Multi-stage aging was performed by changing the aging treatment temperature in the range from 400°C to 800°C. The relationship between the final multi-stage aging treatment temperature and the magnet properties is shown in FIG. 2.
最終多段時効温度が４００℃から６００℃の範囲で、磁
石特性が著しく向上している。When the final multi-stage aging temperature ranges from 400°C to 600°C, the magnetic properties are significantly improved.
以上の実施例はＮｄ−Ｆｅ−Ｂ系と多段時効の効果につ
いて述べたものであるが、これらの結果はＮｄ−Ｆｅ４
を主成分とするＲ２Ｔ１４Ｂ系合金であれば十分に期待
できるものであることは容易に推察できる。The above examples describe the effects of the Nd-Fe-B system and multi-stage aging, but these results do not apply to Nd-Fe4
It can be easily inferred that an R2T14B alloy containing as a main component is highly promising.
また多段時効の保持温度間隔、保持時間についてはこの
実施例では約１００℃、１時間を実施したが、他の温度
間隔、保持時間でもよく、また一定の温度間隔、一定の
保持時間でなく時効処−１過程で温度の昇降等を行った
としても、処理温度が前記した本発明の範囲内であれば
本発明の効果が充分に期待できることは容易に推察でき
る。In addition, regarding the holding temperature interval and holding time of multi-stage aging, in this example, it was carried out at about 100°C for 1 hour, but other temperature intervals and holding times may be used. It can be easily inferred that even if the temperature is raised or lowered in the process-1, the effects of the present invention can be fully expected as long as the treatment temperature is within the range of the present invention described above.
さらに本実施例では段階的に温度を降下させて行ったが
１回の時効の度に急加熱急冷を繰り返しても同様の効果
が現れた。また多段時効の回数については好ましくは３
段以上が効果的であった。Further, in this example, the temperature was lowered stepwise, but the same effect was obtained even if rapid heating and cooling were repeated for each aging. Also, the number of multi-stage aging is preferably 3.
Levels above were effective.
本発明については以上詳細に説明したが。 The present invention has been described in detail above.
Ｎｄ−Ｆｅ−Ｂを主成分とするＲ２Ｔ１４Ｂ系磁石を粉
末冶金法において製造するに当り焼結体を焼結温度から
１０００℃の温度範囲で時効を開始し１４００℃When manufacturing R2T14B magnets containing Nd-Fe-B as the main component by powder metallurgy, the sintered body is aged at a temperature range of 1000°C from the sintering temperature and then heated to 1400°C.
第１図は、実施例１におけるＮｄ−Ｆｅ４系磁石焼結体
の多段時効開始温度と磁石特性の関係を示す。
第２図は、実施例２におけるＮｄ−Ｆｅ−Ｂ系磁石焼結
体の最終多段時効処理温度と磁石特性の関係を示すＯ
第３図は実施例１における開始温度を１０８０℃とした
時の多段時効処理の加熱冷却・リーンを示す。
第１図
多８詩９ｊ′Ｊ開始温度（・Ｃ）
第３図FIG. 1 shows the relationship between the multi-stage aging start temperature and magnetic properties of the Nd-Fe4 magnet sintered body in Example 1. Figure 2 shows the relationship between the final multi-stage aging treatment temperature and magnet properties of the Nd-Fe-B magnet sintered body in Example 2. Figure 3 shows the relationship between the starting temperature in Example 1 and 1080°C. Showing heating/cooling/lean in multi-stage aging treatment. Figure 1: 9j'J starting temperature (・C) Figure 3
Claims (1)
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
時効処理を少くとも３段以上行い、初段は焼結体を焼結
温度から１０００℃の温度範囲で開始し、最終段は４０
０℃から６５０℃の温度範囲で行うことを特徴とする希
土類磁石の製造方法 （但しＲ＿２Ｔ＿１＿４ＢのＲはイットリウムおよび希
土類元素、Ｔは遷移金属を表わす）[Claims] R_2T_1_4B containing 1, Nd, Fe, and B as main components
In the method of manufacturing magnet alloys by powder metallurgy, aging treatment is performed in at least three stages, with the first stage starting the sintered body at a temperature range of 1000°C from the sintering temperature, and the final stage at 40°C.
A method for producing a rare earth magnet, characterized in that it is carried out at a temperature range of 0°C to 650°C (wherein R in R_2T_1_4B represents yttrium and a rare earth element, and T represents a transition metal).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61007206A JPS62167842A (en) | 1986-01-18 | 1986-01-18 | Production of rare earth magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61007206A JPS62167842A (en) | 1986-01-18 | 1986-01-18 | Production of rare earth magnet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62167842A true JPS62167842A (en) | 1987-07-24 |
Family
ID=11659539
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61007206A Pending JPS62167842A (en) | 1986-01-18 | 1986-01-18 | Production of rare earth magnet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62167842A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294401A (en) * | 1989-05-09 | 1990-12-05 | Fuji Elelctrochem Co Ltd | Production of magnet powder |
| JP2019220689A (en) * | 2018-06-15 | 2019-12-26 | スターグループ インダストリアル カンパニー リミテッド | MANUFACTURING METHOD OF HEAVY RARE EARTH GRAIN BOUNDARY DIFFUSION TYPE RE-Fe-B BASED RARE EARTH MAGNET AND HEAVY RARE EARTH GRAIN BOUNDARY DIFFUSION TYPE RE-Fe-B BASED RARE EARTH MAGNET MANUFACTURED BY THE SAME |
-
1986
- 1986-01-18 JP JP61007206A patent/JPS62167842A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294401A (en) * | 1989-05-09 | 1990-12-05 | Fuji Elelctrochem Co Ltd | Production of magnet powder |
| JP2019220689A (en) * | 2018-06-15 | 2019-12-26 | スターグループ インダストリアル カンパニー リミテッド | MANUFACTURING METHOD OF HEAVY RARE EARTH GRAIN BOUNDARY DIFFUSION TYPE RE-Fe-B BASED RARE EARTH MAGNET AND HEAVY RARE EARTH GRAIN BOUNDARY DIFFUSION TYPE RE-Fe-B BASED RARE EARTH MAGNET MANUFACTURED BY THE SAME |
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