JPH06224017A - Manufacture of rare earth element base inter-metallic compound magnet by high pressure sintering in magnetic field - Google Patents
Manufacture of rare earth element base inter-metallic compound magnet by high pressure sintering in magnetic fieldInfo
- Publication number
- JPH06224017A JPH06224017A JP4229846A JP22984692A JPH06224017A JP H06224017 A JPH06224017 A JP H06224017A JP 4229846 A JP4229846 A JP 4229846A JP 22984692 A JP22984692 A JP 22984692A JP H06224017 A JPH06224017 A JP H06224017A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic field
- rare earth
- sintered
- manufacture
- pressure
- 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
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
- H01F1/0596—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2 of rhombic or rhombohedral Th2Zn17 structure or hexagonal Th2Ni17 structure
-
- 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
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
- H01F1/0593—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2 of tetragonal ThMn12-structure
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
【０００１】[0001]
【産業上の利用分野】本発明は、優れた磁気特性を有す
るが高温下で分解するためこれまで焼結による成形が不
可能であった希土類系金属間化合物を、金属あるいは樹
脂等のバインダーを用いることなしに、金属間化合物が
熱分解しない中温度領域下、磁場中で配向させた試料を
高圧焼結することにより磁石とする技術に関するもので
ある。BACKGROUND OF THE INVENTION The present invention uses a rare earth-based intermetallic compound, which has excellent magnetic properties but decomposes at high temperature and cannot be formed by sintering, and a binder such as a metal or a resin. The present invention relates to a technique of forming a magnet by high-pressure sintering of a sample oriented in a magnetic field in an intermediate temperature region where an intermetallic compound is not thermally decomposed without using it.
【０００２】[0002]
【従来の技術】高温下で分解する難焼結性の希土類系金
属間化合物磁石は、亜鉛などの金属あるいはエポキシ樹
脂等をバインダーとして、金属間化合物が熱分解する温
度よりも低い温度領域で成形したボンド磁石として現在
製造されている。2. Description of the Related Art A rare earth-based intermetallic compound magnet which is hard to sinter and decomposes at high temperature is formed in a temperature range lower than the temperature at which the intermetallic compound is thermally decomposed by using a metal such as zinc or an epoxy resin as a binder. It is currently manufactured as a bonded magnet.
【０００３】[0003]
【発明が解決しようという課題】難焼結性の希土類系金
属間化合物の成形体を製造する従来の方法では、磁性に
寄与しない金属あるいは樹脂等をバインダーとして含む
ため、その磁気特性は本来期待されるものと比べ大幅に
低下し、磁性材料としての高性能化の大きな妨げとなっ
ていた。従って、磁性に寄与しないバインダーを使用す
ることなしに、希土類系金属間化合物のみから成る磁石
を製造し、その本来の磁気特性を発現させる必要があ
る。In the conventional method for producing a compact of a rare earth-based intermetallic compound that is difficult to sinter, the magnetic properties originally expected are obtained because a metal or resin that does not contribute to magnetism is included as a binder. It was significantly lower than that of the magnetic material, and it was a great obstacle to improving the performance as a magnetic material. Therefore, it is necessary to produce a magnet composed of only a rare earth-based intermetallic compound without using a binder that does not contribute to magnetism, and to exhibit its original magnetic characteristics.
【０００４】[0004]
【課題を解決するための手段】前記の目的を達成するた
めには、難焼結性の希土類系金属間化合物を単磁区の粒
子粉末とした後磁場中で粒子の結晶方位をそろえ、これ
らを分解させることなしに焼結する製造プロセスの開発
が不可欠である。本発明では、磁場中で粉末粒子の結晶
方位をそろえた後、200℃から800℃の中温度領域下、10
0気圧以上の圧力で加圧焼結し、磁気特性および機械的
強度に優れた希土類系金属間化合物の焼結磁石を製造す
ることを特徴としている。Means for Solving the Problems In order to achieve the above-mentioned object, a rare-earth intermetallic compound which is difficult to sinter is made into a single-domain particle powder, and the crystal orientations of the particles are aligned in a magnetic field. Development of a manufacturing process that sinters without decomposing is essential. In the present invention, after aligning the crystallographic orientation of the powder particles in a magnetic field, under a medium temperature range of 200 ℃ ~ 800 ℃, 10
It is characterized in that pressure-sintering is performed at a pressure of 0 atm or more to produce a sintered magnet of a rare earth-based intermetallic compound excellent in magnetic properties and mechanical strength.
【０００５】[0005]
【作用】本発明では、難焼結性の希土類系金属間化合物
の焼結磁石を、バインダー等を用いることなしに製造す
ることができる。In the present invention, it is possible to manufacture a sintered magnet of a rare earth-based intermetallic compound that is difficult to sinter, without using a binder or the like.
【０００６】製造は、Ln2Fe17Nx、Ln2Fe17CxNy、LnFe11
TiNx等を始めとする難焼結性の希土類系金属間化合物に
適用することができる。特に、３万気圧前後の高圧で焼
結した場合は、非常に良好な機械的強度を有する焼結体
が得られる。Production is carried out by Ln 2 Fe 17 N x , Ln 2 Fe 17 C x N y , LnFe 11
It can be applied to rare-earth intermetallic compounds that are difficult to sinter, such as TiN x . In particular, when sintered at a high pressure of around 30,000 atm, a sintered body having very good mechanical strength can be obtained.
【０００７】また試料は、磁場中で加圧焼結されるか、
あるいは予め磁場中で結晶方位をそろえた後加圧焼結さ
れるため、高い異方性磁場を有する焼結磁石を製造する
ことができる。Further, the sample is pressure-sintered in a magnetic field, or
Alternatively, since the crystal orientations are previously aligned in a magnetic field and pressure sintering is performed, a sintered magnet having a high anisotropic magnetic field can be manufactured.
【０００８】[0008]
【実施例】図１に示す製造工程により、Ln2Fe17Nx、Ln2
Fe17CxNy、LnFe11TiNx等の希土類系金属間化合物の焼結
磁石を製造することができる。[Example] By the manufacturing process shown in FIG. 1, Ln 2 Fe 17 N x , Ln 2
It is possible to manufacture a sintered magnet of a rare earth-based intermetallic compound such as Fe 17 C x N y and LnFe 11 TiN x .
【０００９】製造は、まず上記の希土類系金属間化合物
を振動ボールミルで粒子径が数μｍ以下の単磁区粒子と
なるまで十分に粉砕後、高圧発生装置を用いて磁場中、
200℃から800℃の温度範囲、100気圧以上の圧力下で加
圧焼結するか、あるいは予め磁場中で結晶方位をそろえ
て成形した試料について、同様の条件で加圧焼結するこ
とにより行った。磁石としての安定性と機械的強度は加
圧する圧力と共に向上し、３万気圧で作製した試料では
十分な磁気特性と機械的強度を有する焼結磁石が得られ
た。In the production, first, the above rare earth intermetallic compound is sufficiently pulverized by a vibrating ball mill until it becomes single domain particles having a particle diameter of several μm or less, and then a high pressure generator is used to generate a magnetic field.
Performed by pressure sintering in a temperature range of 200 ° C to 800 ° C under a pressure of 100 atm or more, or by performing pressure sintering under the same conditions on a sample molded in advance by aligning the crystal orientation in a magnetic field. It was The stability and mechanical strength as a magnet increased with the pressure applied, and a sintered magnet having sufficient magnetic characteristics and mechanical strength was obtained in the sample manufactured at 30,000 atm.
【００１０】図２に、Sm2Fe17Nx粉末を3万気圧、550℃
で加圧焼結した試料（曲線ｂ）および同試料を予め磁場
中で加圧成形後、同じ圧力と温度で高圧焼結した試料
（曲線ｃ）のＸ線回折パターンを、未処理試料のそれ
（曲線ａ）と併せて示す。In FIG. 2, Sm 2 Fe 17 N x powder was added at 30,000 atm and 550 ° C.
The X-ray diffraction patterns of the sample (curve b) pressure-sintered in 1) (curve b) and the sample pre-pressurized in a magnetic field, and then high-pressure sintered at the same pressure and temperature (curve c), Shown together with (curve a).
【００１１】ここでまず、550℃で加圧処理した試料で
は、回折パターンには何らの変化も観察されず（曲線ａ
とｂを参照）、SmNとFeへの分解や窒素の解離等は全く
見られなかった。First, no change was observed in the diffraction pattern of the sample subjected to pressure treatment at 550 ° C. (curve a)
And b)), no decomposition into SmN and Fe or dissociation of nitrogen was observed.
【００１２】また、磁場中で粒子の結晶方位をそろえた
後加圧焼結した場合（曲線ｃ）では、磁場に沿ってｃ軸
方向に配向した試料が得られた。（なお、Sm2Fe17Nxの
晶系は本来三方晶系であるが、ここでは六方晶系の単位
格子として表示してある。）個々の結晶粒子は容易磁化
方向であるｃ軸に沿って配向しているため、試料からは
高い異方性磁界が出現し、20MGOe以上の最大エネルギー
積をもつ高性能焼結磁石を容易に作製することができ
た。When pressure-sintering was performed after aligning the crystal orientations of the particles in the magnetic field (curve c), a sample oriented in the c-axis direction along the magnetic field was obtained. (Note that the Sm 2 Fe 17 N x crystal system is originally a trigonal system, but it is shown here as a hexagonal unit cell.) Individual crystal grains are along the c-axis, which is the easy magnetization direction. The high anisotropy field appeared from the sample because it was oriented so that a high-performance sintered magnet with a maximum energy product of 20 MGOe or more could be easily manufactured.
【００１３】[0013]
【発明の効果】本発明は、磁場中、200℃から800℃前後
の中温度領域で加圧焼結を行うため、難焼結性の希土類
系金属間化合物について、十分な機械的強度をもつ焼結
磁石を製造することができる。そのため、磁気特性に寄
与しない金属あるいは樹脂等のバインダーが不要とな
り、単位体積あるいは単位重量当たりの磁束密度が増大
し、高性能永久磁石の製造に効果がある。INDUSTRIAL APPLICABILITY Since the present invention performs pressure sintering in a medium temperature range of about 200 ° C. to 800 ° C. in a magnetic field, it has sufficient mechanical strength for a rare earth intermetallic compound that is difficult to sinter. A sintered magnet can be manufactured. Therefore, a binder such as a metal or a resin that does not contribute to the magnetic characteristics is unnecessary, the magnetic flux density per unit volume or unit weight is increased, and it is effective in manufacturing a high-performance permanent magnet.
【図１】高圧焼結法による希土類系金属間化合物の製造
工程図である。FIG. 1 is a manufacturing process drawing of a rare earth-based intermetallic compound by a high pressure sintering method.
【図２】Sm2Fe17Nxの粉末Ｘ線回折図である。ただし、
(a)は加圧焼結する前の未処理試料、(b)は加圧焼結後の
試料、(c)は一度磁場中で試料粉末の結晶方位をそろえ
た後加圧焼結した試料である。FIG. 2 is a powder X-ray diffraction pattern of Sm 2 Fe 17 N x . However,
(a) is an untreated sample before pressure sintering, (b) is a sample after pressure sintering, and (c) is a sample that has been subjected to pressure sintering after aligning the crystal orientations of the sample powder once in a magnetic field. Is.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｆ 1/053 ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Office reference number FI technical display location H01F 1/053
Claims (1)
Ny、LnFe11TiNx（Ln=希土類）等の難焼結性希土類系金
属間化合物の単磁区粒子粉末を、磁場中で結晶の配向を
そろえると共に200℃から800℃の中温度領域下、100気
圧以上の圧力で加圧焼結することにより、優れた磁気特
性と機械的強度を有する焼結磁石を製造する技術。1. Ln 2 Fe 17 N x , Ln 2 Fe 17 C x that decomposes at high temperature
N y , LnFe 11 TiN x (Ln = rare earth) single-domain particle powder of rare-earth intermetallic compound difficult to sinter, such as crystal orientation aligned in a magnetic field and 200 ℃ to 800 ℃ under medium temperature range, A technology that produces sintered magnets with excellent magnetic properties and mechanical strength by pressure sintering at a pressure of 100 atm or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4229846A JPH06224017A (en) | 1992-08-28 | 1992-08-28 | Manufacture of rare earth element base inter-metallic compound magnet by high pressure sintering in magnetic field |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4229846A JPH06224017A (en) | 1992-08-28 | 1992-08-28 | Manufacture of rare earth element base inter-metallic compound magnet by high pressure sintering in magnetic field |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06224017A true JPH06224017A (en) | 1994-08-12 |
Family
ID=16898606
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4229846A Pending JPH06224017A (en) | 1992-08-28 | 1992-08-28 | Manufacture of rare earth element base inter-metallic compound magnet by high pressure sintering in magnetic field |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06224017A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1241687A1 (en) * | 2001-03-14 | 2002-09-18 | Shin-Etsu Chemical Co., Ltd. | Bulk anisotropic rare earth permanent magnet and preparation method |
-
1992
- 1992-08-28 JP JP4229846A patent/JPH06224017A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1241687A1 (en) * | 2001-03-14 | 2002-09-18 | Shin-Etsu Chemical Co., Ltd. | Bulk anisotropic rare earth permanent magnet and preparation method |
| US6863742B2 (en) | 2001-03-14 | 2005-03-08 | Shin-Etsu Chemical Co., Ltd. | Bulk anisotropic rare earth permanent magnet and preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kirchmayr | Permanent magnets and hard magnetic materials | |
| Nakayama et al. | Microstructures and crystallographic orientation of crystalline grains in anisotropic Nd‐Fe‐Co‐B‐(Ga or Zr) magnet powders produced by the hydrogenation‐decomposition‐desorption‐recombination process | |
| CA1297264C (en) | Isotropic rare earth-iron field magnets for magnetic resonance imaging | |
| JPS62291904A (en) | Mafufacture of permanent magnet | |
| JPH0420975B2 (en) | ||
| KR101345496B1 (en) | Powder for magnet, powder compact, rare earth-iron-boron-based alloy material, method for producing powder for magnet, and method for producing rare earth-iron-boron-based alloy material | |
| US3540945A (en) | Permanent magnets | |
| EP0542529B1 (en) | Method of making alloy powders of the RE-Fe/Co-B-M-type and bonded magnets containing this alloy powder | |
| Horikawa et al. | Recent progress in the development of high-performance bonded magnets using rare earth–Fe compounds | |
| Schultz et al. | Preparation and properties of mechanically alloyed rare earth permanent magnets | |
| CN108962580B (en) | Preparation method of dysprosium-infiltrated/terbium neodymium iron boron magnet | |
| JP2002015907A (en) | Switching spring magnet powder and its manufacturing method | |
| JPH02308512A (en) | R-fe-b permanent magnet having biased anisotropy and manufacture thereof | |
| Makita et al. | Coercivity of Zn evaporation-coated Sm2Fe17Nx fine powder and its bonded magnets | |
| JPH1092617A (en) | Permanent magnet and its manufacture | |
| JPH06224017A (en) | Manufacture of rare earth element base inter-metallic compound magnet by high pressure sintering in magnetic field | |
| JPH08181009A (en) | Permanent magnet and its manufacturing method | |
| Sugimoto et al. | HDDR process for the production of high performance rare-earth magnets | |
| CN113416903B (en) | Application of alloy powder, hard magnetic material and preparation method and application thereof | |
| JP2004363474A (en) | Method for manufacturing particles for permanent magnet | |
| JPH06507676A (en) | Magnetostrictive powder composite material and its manufacturing method | |
| JP3209291B2 (en) | Magnetic material and its manufacturing method | |
| JPH0142338B2 (en) | ||
| JPH07297013A (en) | Manufacture method of magnetic powder | |
| Mao et al. | Synthesis and characterization of hard magnetic materials: PrFe 10.5 V 1.5 N x |