JPH01162302A - Manufacture of alloy powder for bonded magnet - Google Patents
Manufacture of alloy powder for bonded magnetInfo
- Publication number
- JPH01162302A JPH01162302A JP62321686A JP32168687A JPH01162302A JP H01162302 A JPH01162302 A JP H01162302A JP 62321686 A JP62321686 A JP 62321686A JP 32168687 A JP32168687 A JP 32168687A JP H01162302 A JPH01162302 A JP H01162302A
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- powder
- coercive force
- boron
- alloy powder
- 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
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 47
- 239000000956 alloy Substances 0.000 title claims abstract description 47
- 239000000843 powder Substances 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000010298 pulverizing process Methods 0.000 claims abstract description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052796 boron Inorganic materials 0.000 claims abstract description 14
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 8
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 abstract description 9
- 238000000137 annealing Methods 0.000 abstract description 7
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- 239000001257 hydrogen Substances 0.000 abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 5
- 239000011261 inert gas Substances 0.000 abstract description 2
- 150000002431 hydrogen Chemical class 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 12
- 239000003822 epoxy resin Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 229920000647 polyepoxide Polymers 0.000 description 6
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 5
- 238000003466 welding Methods 0.000 description 4
- QIVUCLWGARAQIO-OLIXTKCUSA-N (3s)-n-[(3s,5s,6r)-6-methyl-2-oxo-1-(2,2,2-trifluoroethyl)-5-(2,3,6-trifluorophenyl)piperidin-3-yl]-2-oxospiro[1h-pyrrolo[2,3-b]pyridine-3,6'-5,7-dihydrocyclopenta[b]pyridine]-3'-carboxamide Chemical compound C1([C@H]2[C@H](N(C(=O)[C@@H](NC(=O)C=3C=C4C[C@]5(CC4=NC=3)C3=CC=CN=C3NC5=O)C2)CC(F)(F)F)C)=C(F)C=CC(F)=C1F QIVUCLWGARAQIO-OLIXTKCUSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- -1 Rare earth transition metal Chemical class 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910000828 alnico Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- AYOOGWWGECJQPI-NSHDSACASA-N n-[(1s)-1-(5-fluoropyrimidin-2-yl)ethyl]-3-(3-propan-2-yloxy-1h-pyrazol-5-yl)imidazo[4,5-b]pyridin-5-amine Chemical compound N1C(OC(C)C)=CC(N2C3=NC(N[C@@H](C)C=4N=CC(F)=CN=4)=CC=C3N=C2)=N1 AYOOGWWGECJQPI-NSHDSACASA-N 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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
- H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
Ｓｍ−Ｃｏ系に代表される希土類遷移金属系ボンド永久
磁石は、従来のフェライト磁石やアルニコ磁石に比べて
はるかに大きな磁気エネルギーを有することから、その
需要は急激に伸びている。[Detailed Description of the Invention] [Industrial Application Field] Rare earth transition metal-based bonded permanent magnets, represented by Sm-Co-based permanent magnets, have much greater magnetic energy than conventional ferrite magnets and alnico magnets. , and its demand is growing rapidly.
前記の希土類遷移金属系ボンド磁石は、当初原料費が高
価なため音響用ピックアップ、ウォッチ。The above-mentioned rare earth transition metal bonded magnets are initially used in audio pickups and watches due to their high raw material costs.
クロックなど超小型製品に使用範囲が限定されていたが
、近年各種産業及び民生用電気、電子機器の主要材料と
して重要な役割を示すようにな９た。Its use was limited to ultra-small products such as clocks, but in recent years it has come to play an important role as a main material in various industries and consumer electrical and electronic devices9.
具体的には音響関係を初めとする電子機器の小型化、高
性能化、省エネルギー化等のニーズにより、小型モータ
ー、小型スピーカー、ヘッドホン、ステップモーター等
へ応用分野を広げており、今後もＯＡ、ＦＡ、自動車電
装品、医療機器へと需要が拡大していくものと考えられ
ている。Specifically, due to the need for miniaturization, higher performance, and energy savings in audio-related and other electronic equipment, we are expanding the field of application to small motors, small speakers, headphones, step motors, etc., and will continue to use OA, Demand is expected to expand to include FA, automotive electrical components, and medical equipment.
本発明はＲ，ボロン、鉄系ボンド磁石用合金粉末を製造
するにあたり、Ｙを含む１０〜３０ａｔ％のＲ，４〜１
０ａ ｔ％のボロン、６０〜８６ａｔ％の鉄、及び製造
上不可避な不純物からなる合金を粉砕する工程の少なく
とも１つ以上の工程で合金に１〜５０ｋｇ／ｃｄの圧力
下で水素ガスを吸蔵させ所定の粒径に粉砕した後、真空
中又はアルゴンガス雰囲気中で３００℃〜６００℃に加
熱し脱水素及びアニールすることにより、粉砕による合
金粉末の残留歪の発生を極力少なくするとともに、粉末
表面にＲ−ｒｉｃｈ相を析出させ、従来避けられなかっ
た粉砕による保磁力の低下を防止し、高性能希土類。In producing R, boron, iron-based bonded magnet alloy powder, the present invention uses 10 to 30 at% of R, 4 to 1 containing Y.
In at least one step of pulverizing an alloy consisting of 0 at% boron, 60 to 86 at% iron, and impurities unavoidable in manufacturing, the alloy is made to absorb hydrogen gas under a pressure of 1 to 50 kg/cd. After pulverizing to a predetermined particle size, the alloy powder is heated to 300°C to 600°C in vacuum or in an argon gas atmosphere to dehydrogenate and anneal, thereby minimizing residual strain in the alloy powder due to pulverization and improving the powder surface. The R-rich phase is precipitated to prevent the coercive force from decreasing due to pulverization, which was previously unavoidable, making it a high-performance rare earth.
ボロン、鉄系異方性ボンド磁石用合金粉末を製造するこ
とにある。Our purpose is to produce boron and iron-based anisotropic bonded alloy powder for magnets.
Ｒ，ポロン、鉄系ボンド磁石用合金は従来溶湯超急冷法
で製造したＮｄ−Ｆｅ−Ｂ系磁石用合金のみが実用化さ
れていた。しかし、この方法で得られるボンド磁石では
非晶質相中に析出する主相（Ｎｄｚ Ｆｅｚ Ｂ）
の結晶粒径が２０〜１１００ｎと、粉末粒径（約０．１
ｍ）に比べて非常に小さく、かつそれぞれの容易磁化方
向がランダムである。そのため、磁場配向ができず等方
性であり、最大エネルギー積で８〜９ Ｍ Ｇ Ｏｅと
ＳｍＣｏ系異方性ボンド磁石の最大エネルギー積１２〜
１６ＭＧＯｅに比べて低い。Conventionally, only Nd-Fe-B alloys for R, Poron, and iron-based bonded magnets manufactured by a molten metal super-quenching method have been put into practical use. However, in the bonded magnet obtained by this method, the main phase (Ndz Fez B) precipitated in the amorphous phase
The crystal grain size is 20 to 1100n, and the powder grain size (approximately 0.1
m), and each easy magnetization direction is random. Therefore, magnetic field orientation is not possible and it is isotropic, with a maximum energy product of 8-9 M G Oe and a maximum energy product of 12-9 M G Oe for SmCo-based anisotropic bonded magnets.
It is lower than 16MGOe.
上記の理由で複雑な着磁方向を要求されるような等方性
磁石でなければならないもの以外は利用価値が低い。For the above-mentioned reasons, the utility value is low unless it is an isotropic magnet that requires a complicated magnetization direction.
又、Ｎｄ、Ｐｒなどの軽希土類、ボロン、鉄系の合金を
従来のＳｍＣｏ系ボンド磁石用合金粉末と同様の方法で
溶解粉砕したものは、磁場配向は可能で異方性磁石とな
るが、保磁力が１ｏｏｏｏ ｅ以下であり高性能磁石と
して使用できない。これは、前記軽希土類、ポロン、鉄
系合金の保磁力発生の主要因である結晶粒界のＲ−ｒｉ
ｃｈ相が粉砕のス１ヘレスにより、破壊されるためであ
ることが知られている。又、粉砕のストレスによる結晶
歪を除去するため６００〜７００℃でアニールするとあ
る程度保磁力は回復するが粒同士が溶着するため磁場配
向が困難になる。In addition, light rare earth elements such as Nd and Pr, boron, and iron-based alloys melted and ground in the same manner as conventional SmCo-based bonded magnet alloy powders can be oriented in a magnetic field and become anisotropic magnets, but Since the coercive force is less than 1ooooe, it cannot be used as a high-performance magnet. This is due to the R-ri of grain boundaries, which is the main factor in the generation of coercive force in light rare earth, poron, and iron alloys.
It is known that this is because the ch phase is destroyed by the crushing process. Further, when annealing is performed at 600 to 700° C. to remove crystal distortion caused by crushing stress, the coercive force is recovered to some extent, but the grains are welded together, making magnetic field orientation difficult.
ただし、軽希土類をＤｙなど重希土類に置き換えた合金
を従来のＳｍＣｏ系ボンド磁石と同様の方法で溶解粉砕
したものは、歪取りアニールをしなくとも保磁力が１０
００００ ｅを超え粒同士の溶着も発生しない場合もあ
る。しかし、Ｂｒが非常に低く、これも高性能磁石とし
て使用できない。However, alloys in which light rare earths are replaced with heavy rare earths such as Dy, which are melted and crushed in the same manner as conventional SmCo bonded magnets, have a coercive force of 10% even without strain relief annealing.
0000 e and no welding of grains occurs in some cases. However, Br is very low, and this also cannot be used as a high-performance magnet.
前記、従来の技術で説明したように、溶湯急冷法で製造
した合金は磁場配向ができず、ＳｍＣ。As explained above in the prior art section, alloys manufactured by the molten metal quenching method cannot be oriented in a magnetic field, and SmC.
系ボンド磁石と同様の方法で製造した合金は保磁力が低
いことから、両者とも異方性ボンド磁石用合金粉末とな
り得ない。本発明ではＳｍＣｏ系ボンド磁石と同様の方
法で製造した磁石合金について、粉砕のための結晶粒の
歪による保磁力の低下を防ぎ、さらに歪除去のためのア
ニールにより発生する粉末の溶着を防止することで、高
性能異方性ボンド磁石用合金を得ようとするものである
。Since alloys manufactured in the same manner as the bonded magnets have low coercive force, neither of them can be used as alloy powder for anisotropic bonded magnets. In the present invention, for magnet alloys manufactured in the same manner as SmCo-based bonded magnets, reduction in coercive force due to distortion of crystal grains due to crushing is prevented, and furthermore, powder welding caused by annealing to remove distortion is prevented. This is an attempt to obtain a high-performance anisotropic bonded magnet alloy.
Ｒ，ポロン、鉄系磁石は１−５系ＳｍＣｏ磁石と同様な
ニュークリエイジョンタイプの磁石であり保磁力発生機
構は、主相であるＮｄｚ −Ｆｅ１２−Ｂ及び主相を取
り囲むように析出しているＲ−ｒｉｃｈ相に、歪、欠陥
などのない完全性に起因している。R, Poron, and iron-based magnets are nucleation type magnets similar to 1-5-based SmCo magnets, and the coercive force generation mechanism consists of the main phase Ndz-Fe12-B and precipitation surrounding the main phase. This is due to the completeness of the R-rich phase, which has no distortion or defects.
本発明では、高周波溶解、アーク溶解などで製造したＲ
、ボロン、鉄系合金インゴットを粉砕する際合金に水素
ガスを吸蔵させ、１０〜１００μｍに自然粉化した後、
ボールミルなどで２〜１０μｍに微粉砕することにより
、機械的粉砕では不可避な粉砕による結晶粒の歪を極力
少なくすることを第１の手段とした。この状態では粉末
は殆ど単結晶の状態まで粉砕されており、粒内に結晶粒
界は存在せず粉末保磁力は１０００’Ｏｅ以下となるこ
とが分かった。そこで、第２の手段として微粉砕で得ら
れた２〜１０μｍの粉末を真空中又はアルゴンガスなど
の不活性ガス中３００〜６００℃の雰囲気で脱水素を行
うと共に従来考えられていた温度より低い温度でのアニ
ールを行うことにより、磁場配向に不都合な粒同士の溶
着が起きない状態で結晶粒に僅かに残留する内部歪を完
全に除去し粒表面にＲ−ｒｉ ｃｈ相を析出させ、粉砕
による保磁力の低下を極力少なくした高性能異方性ボン
ド磁石用合金粉末を得ようとするものである。In the present invention, R manufactured by high frequency melting, arc melting, etc.
, boron, When grinding an iron-based alloy ingot, hydrogen gas is absorbed into the alloy, and after natural powdering of 10 to 100 μm,
The first method was to reduce as much as possible distortion of crystal grains due to pulverization, which is inevitable in mechanical pulverization, by pulverizing the crystal grains to a size of 2 to 10 μm using a ball mill or the like. It was found that in this state, the powder was pulverized to almost a single crystal state, there were no grain boundaries within the grains, and the powder coercive force was 1000'Oe or less. Therefore, as a second method, the powder of 2 to 10 μm obtained by pulverization is dehydrogenated in a vacuum or an inert gas such as argon gas at a temperature of 300 to 600°C, and the temperature is lower than previously thought. By performing annealing at high temperature, the internal strain that remains slightly in the crystal grains is completely removed without welding of grains that is unfavorable to magnetic field orientation, and the R-rich phase is precipitated on the grain surface, resulting in pulverization. The objective is to obtain a high-performance alloy powder for anisotropic bonded magnets that minimizes the decrease in coercive force due to
本発明によれば前記、問題を解決する手段に記した通り
水素吸蔵で自然粉化した合金を微粉砕することにより、
粉砕による歪が小さい粉末が得られること及び粒同士の
溶着が起きないような低温下での保磁力回復のためのア
ニールが可能となる。According to the present invention, as described in the above-mentioned means for solving the problem, by finely pulverizing an alloy that has been naturally powdered by hydrogen absorption,
It is possible to obtain powder with small distortion due to pulverization, and to perform annealing to recover coercive force at a low temperature where welding of particles does not occur.
〔実施例−１〕
ｆｌｌＮｄ＋ｓ Ｆｅｑｑ Ｂ６及びＮｄ１ｇ−Ｆ
ｅ７Ｓ−Ｂ６となるように配合しアルゴンガス中でアー
ク溶解した合金を出発合金とした。この時Ｎｄは、９５
％以上の純度のもの、Ｂはクリスタルボロン、Ｆｅは９
９．９％以上の電解鉄を使用した。[Example-1] fllNd+s Feqq B6 and Nd1g-F
The starting alloy was prepared by blending e7S-B6 and arc melting it in argon gas. At this time, Nd is 95
% purity or higher, B is crystal boron, Fe is 9
Electrolytic iron of 9.9% or more was used.
（２）アーク溶解した合金はタラソシャーミル、ディス
クミルなどで３２メンシユスルーに粗粉砕し、さらにボ
ールミルで平均粒径４μｍに微粉砕した。(2) The arc-melted alloy was coarsely pulverized to 32-mesh through using a Thalasso shear mill, a disk mill, etc., and further finely pulverized to an average particle size of 4 μm using a ball mill.
（３）得られた合金粉末に体積比で２０％のエポキシ樹
脂を混合し、２ｔｏｎ／ｃｆｆｌの圧力で成形固化した
。このサンプルの磁気特性を表１に示す。(3) Epoxy resin of 20% by volume was mixed with the obtained alloy powder, and the mixture was molded and solidified at a pressure of 2 tons/cffl. Table 1 shows the magnetic properties of this sample.
表−１
〔実施例−２〕
（１１Ｎｄ＋ｓ Ｆｅ、ｑ Ｂｂ及びＮｄ、ｇ −
Ｆｅ７５−Ｂ６となるように配合しアルゴンガス中でア
ーク溶解した合金を出発合金とした。この時Ｎｄは、９
５％以上の純度のもの、Ｂはクリスタルボロン、Ｆｅは
９９．９％以上の電解鉄を使用した。Table-1 [Example-2] (11Nd+s Fe, q Bb and Nd, g −
An alloy blended to give Fe75-B6 and arc melted in argon gas was used as a starting alloy. At this time, Nd is 9
Crystal boron with a purity of 5% or more was used for B, and electrolytic iron with a purity of 99.9% or more was used for Fe.
（２）アーク溶解した合金はクラッシャーミル、ディス
クミルなどで３２メンシユスルーに粗粉砕し、さらにボ
ールミルで平均粒径４μｍに微粉砕した。(2) The arc-melted alloy was coarsely pulverized to 32-mesh through using a crusher mill, a disk mill, etc., and further finely pulverized to an average particle size of 4 μm using a ball mill.
（３）粉砕した合金を石英管にいれ２ ｘｔｏ−ｓ ｔ
ｏ ｒｒの真空度で５５０℃、２０時間の熱処理をほ
どこした。(3) Put the crushed alloy into a quartz tube 2xto-st
Heat treatment was performed at 550° C. for 20 hours at a vacuum degree of o rr.
（４）得られた合金粉末に体積比で２０％のエポキシ樹
脂を混合し２ｔｏｎ／ｃｎ＋の圧力で成形固化した。(4) Epoxy resin of 20% by volume was mixed with the obtained alloy powder and molded and solidified at a pressure of 2 ton/cn+.
このサンプルの磁気特性を表２に示す。Table 2 shows the magnetic properties of this sample.
〔実施例−３〕
（１）Ｎ ｄ １５ Ｆ ｅ ７ｇ Ｂ ｂ及びＮ
ｄ１９ Ｆｅ７５−Ｂ６となるように配合しアルゴン
ガス中でアーク溶解した合金を出発合金とした。この時
Ｎｄは、９５％以上の純度のもの、Ｂはクリスタルボロ
ン、Ｆｅは９９．９％以上の電解鉄を使用した。[Example-3] (1) N d 15 Fe 7g B b and N
An alloy blended to give d19 Fe75-B6 and arc melted in argon gas was used as a starting alloy. At this time, Nd was used with a purity of 95% or more, B was crystal boron, and Fe was electrolytic iron with a purity of 99.9% or more.
（２）アーク溶解した合金はタラソシャーミルで１〜５
顛に粗粉砕し密閉容器に納め、真空中で３００℃３０分
間活性化処理した後、５０ｋｇ／ｃＪの圧力で１時間水
素ガスを吸収させ真空中３００℃で３０分脱水素を行い
５０〜５００μｍに粉末化し、さらにボールミルで平均
粒径４μｍに微粉砕した。(2) The arc-melted alloy is 1 to 5 in a Thalasso shear mill.
After that, it is coarsely ground, placed in a sealed container, and activated in a vacuum at 300°C for 30 minutes, then absorbed hydrogen gas at a pressure of 50 kg/cJ for 1 hour, and dehydrogenated in a vacuum at 300°C for 30 minutes to a size of 50 to 500 μm. The mixture was pulverized into powder and further finely ground to an average particle size of 4 μm using a ball mill.
（３）得られた合金粉末に体積比で２０％のエポキシ樹
脂を混合し２ｔｏｎ／＋ｆｆｌの圧力で成形固化した。(3) The obtained alloy powder was mixed with 20% by volume epoxy resin and molded and solidified under a pressure of 2 tons/+ffl.
このサンプルの磁気特性を表３に示す。Table 3 shows the magnetic properties of this sample.
表−３
〔実施例−４〕
（１）Ｎｄ＋ｓ Ｆｅｔ、 Ｂｂ及びＮｄ＋ｑ Ｆ
ｅ７ｓ−Ｂ６となるように配合しアルゴンガス中でアー
ク溶解した合金を出発合金とした。この時Ｎｄは、９５
％以上の純度のもの、Ｂはクリスタルボロン、Ｆｅは９
９．９％以上の電解鉄を使用した。Table-3 [Example-4] (1) Nd+s Fet, Bb and Nd+q F
The starting alloy was prepared by blending e7s-B6 and arc melting it in argon gas. At this time, Nd is 95
% purity or higher, B is crystal boron, Fe is 9
Electrolytic iron of 9.9% or more was used.
（２）アーク溶解した合金はタラソシャーミルで１〜５
１ｍに粗粉砕し密閉容器に納め、真空中で３００℃で３
０分脱水素を行い５０〜５００μｍに粉末化し、ボール
ミルで平均粒径４μｍに微粉砕した。(2) The arc-melted alloy is 1 to 5 in a Thalasso shear mill.
Coarsely pulverize to 1 m, store in a sealed container, and heat at 300°C in vacuum for 30 minutes.
It was dehydrogenated for 0 minutes and powdered to 50 to 500 μm, and finely pulverized to an average particle size of 4 μm using a ball mill.
（３）粉砕した合金を石英管にいれ２ ｘｉｏ−５ｔ
ｏ ｒｒの真空度で５５０℃、３０時間の熱処理をほど
こし（４）得られた合金粉末に体積比で２０％のエポキ
シ樹脂を混合し２ｔｏｎ／ｃＪの圧力で成形固化した。(3) Put the crushed alloy into a quartz tube 2 xio-5t
A heat treatment was performed at 550° C. for 30 hours at a vacuum degree of o rr. (4) The obtained alloy powder was mixed with 20% by volume epoxy resin and molded and solidified at a pressure of 2 ton/cJ.
このサンプルの磁気特性を表４に示す。Table 4 shows the magnetic properties of this sample.
表−４
〔実施例−５〕
実施例−４により本発明の効果が顕著であることが判明
したので、さらに磁気特性の向上を図るべく検討した結
果、粉砕後の熱処理条件により磁気特性がさらに向上す
ることを見出した。そこで、Ｎｄ１６ Ｆｅｑｅ
Ｂｂとなるように配合した合金を実施例−４に従って水
素吸蔵〜微粉砕した粉末について熱処理温度を４５０℃
〜６５０℃、熱処理時間を２０〜４０時間の間の条件で
熱処理し、体積比で２０％のエポキシ樹脂を混合し２ｔ
ｏｎ／ａＪの圧力で１０ｋＯｅの磁場中成形固化したサ
ンプルの磁気特性（（Ｂ Ｈ） ｍ’ａ ｘ）を図１に
示す。Table 4 [Example 5] As it was found in Example 4 that the effect of the present invention was remarkable, we conducted a study to further improve the magnetic properties. I found that it can be improved. Therefore, Nd16 Feque
A heat treatment temperature of 450°C was applied to a powder obtained by hydrogen storage and pulverization of an alloy blended to become Bb according to Example-4.
Heat-treated at ~650℃ for 20-40 hours, mixed with 20% epoxy resin by volume, and made 2 tons.
FIG. 1 shows the magnetic properties ((B H) m'a x) of a sample molded and solidified in a magnetic field of 10 kOe at a pressure of on/aJ.
〔実施例−６〕
Ｎｄを１５ａ ｔ％〜１９ａｔ％になるように配合した
合金を実施例−４に従って水素吸蔵〜微粉砕し実施例−
５での最適条件である６００℃４０時間で熱処理した粉
末に体積比で２０％のエポキシ樹脂を混合し、２ｔｏｎ
／ｃＩｉｌの圧力で１０ｋＯｅの磁場中成形固化したサ
ンプルの磁気特性（（ＢＨ）ｍａＸ）を図２に示す。[Example-6] An alloy containing 15 at% to 19 at% of Nd was hydrogen-absorbed and pulverized according to Example-4.
The powder was heat-treated at 600°C for 40 hours, which is the optimum condition in step 5, and 20% by volume of epoxy resin was mixed with it, and 2 tons of
FIG. 2 shows the magnetic properties ((BH) ma
実施例−５及び６により明らかなようにＮｄ−Ｆｅ−Ｂ
を水素吸蔵粉砕後熱処理することにより磁気特性が著し
く改善されることが分かった。又、６００℃以上の熱処
理では、保磁力は向上するものの（ＢＨ）ｍａ ｘはや
や低下することが分かった。As is clear from Examples 5 and 6, Nd-Fe-B
It was found that the magnetic properties were significantly improved by heat treatment after hydrogen storage pulverization. It was also found that when heat treated at 600° C. or higher, although the coercive force was improved, (BH)max was slightly lowered.
その理由として、
■水素吸蔵粉砕により、結晶粒の粉砕による歪が少なく
なる。The reason for this is: (1) Hydrogen storage pulverization reduces distortion caused by pulverization of crystal grains.
■低温熱処理により粉砕による残留歪が、完全に除去さ
れるとともに、粒表面にＲ−ｒｉｃｈ相を析出させ保磁
力の低下を防止する。(2) Residual strain caused by pulverization is completely removed by low-temperature heat treatment, and an R-rich phase is precipitated on the grain surface to prevent a decrease in coercive force.
■熱処理温度が６００℃を超えると粒表面に析出したＲ
−ｒｆｃ）１相同士が溶着するため磁場配向が困難にな
り磁気特性が低下する。ということが分かった。■When the heat treatment temperature exceeds 600℃, R precipitates on the grain surface.
-rfc) Since one phase is welded together, magnetic field orientation becomes difficult and magnetic properties deteriorate. That's what I found out.
前記、発明の詳細な説明で分かる通り本発明によれば、
従来不可能だった希土類、ボロン、鉄系異方性ボンド磁
石を製造することができ、従来Ｓｍｃｏ、系の焼結磁石
でしか達成できなかった。As can be seen from the above detailed description of the invention, according to the present invention,
It is now possible to produce rare earth, boron, and iron-based anisotropic bonded magnets, which was previously impossible, and could only be achieved with Smco-based sintered magnets.
（ＢＨ）ｍａ ｘ１６〜２０ＭＧｏｅの性能をボンド磁
石で達成できる。(BH) A performance of max 16 to 20 MGoe can be achieved with a bonded magnet.
一般に知られているように、焼結磁石は焼結による収縮
が太き（、希土類磁石の主な市場である精密部品に使用
する場合は研削、ラッピング等の仕上げ加工が必要であ
り、製造コストが増加する。As is generally known, sintered magnets have a large shrinkage due to sintering (and when used in precision parts, which is the main market for rare earth magnets, finishing processes such as grinding and lapping are required, which increases manufacturing costs. increases.
ボンド磁石は成形後殆ど収縮しないため、仕上げ加工を
不用とすることも可能となり、製造コストが大幅に削減
できる。更に実施例に示したように、希土類にＮｄを使
用した場合、資源含存量がＳｍの１０倍以上あり、鉄は
ｃｏに比べれば、無限に存在すると言って良く、原料供
給が長期的に安価で安定して得られることが期待できる
。Since bonded magnets hardly shrink after molding, it is possible to eliminate the need for finishing processing, which can significantly reduce manufacturing costs. Furthermore, as shown in the example, when Nd is used as a rare earth, the resource content is more than 10 times that of Sm, and compared to cobalt, it can be said that iron exists infinitely, making the raw material supply cheap in the long term. It is expected that stable results will be obtained.
第１図はＮｄ＋ｂ−Ｆｅｑ８ Ｂｂの合金粉末を各種温
度及び時間でアニールした時の磁気特性図（実施例５）
、
第２図はＮｄｘ−Ｆｅ、４−ｘ−Ｂｂの合金のＸを１５
〜１９ａｔ％の間で変化させた時の磁気特性図（実施例
６）である。
以上
出願人 セイコー電子部品株式会社
代理人 セイコー電子工業株式会社Figure 1 shows the magnetic characteristics of Nd+b-Feq8Bb alloy powder annealed at various temperatures and times (Example 5).
, Figure 2 shows that X of Ndx-Fe, 4-x-Bb alloy is 15
It is a magnetic characteristic diagram (Example 6) when changing between ~19at%. Applicant: Seiko Electronic Components Co., Ltd. Agent: Seiko Electronics Industries Co., Ltd.
Claims (1)
で、Ｙを含む１０〜３０ａｔ％の希土類、４〜１０ａｔ
％のボロン、６０〜８６ａｔ％の鉄からなる合金を粉砕
する工程の少なくとも１つ以上の工程で、合金に１〜５
０ｋｇ／ｃｍ＾２の圧力下で水素ガスを吸蔵させ、所定
の粒径に粉砕した後、真空中又はアルゴンガス雰囲気中
で、３００℃〜６００℃に加熱し粉末表面に希土類（以
下Ｒと記す）−ｒｉｃｈ相を析出しすることを特徴とす
る、Ｒ，ボロン，鉄系のボンド磁石用合金粉末の製造方
法。In the production of alloy powder for rare earth, boron, and iron-based bonded magnets, 10 to 30 at% of rare earth including Y, 4 to 10 at.
In at least one step of grinding an alloy consisting of 60 to 86 at% boron and 60 to 86 at% iron, the alloy contains 1 to 5 at%
After absorbing hydrogen gas under a pressure of 0 kg/cm^2 and pulverizing it to a predetermined particle size, it is heated to 300°C to 600°C in vacuum or in an argon gas atmosphere to coat the powder surface with rare earth elements (hereinafter referred to as R). )-Rich phase is precipitated, a method for producing R, boron, iron-based alloy powder for bonded magnets.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62321686A JPH01162302A (en) | 1987-12-18 | 1987-12-18 | Manufacture of alloy powder for bonded magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62321686A JPH01162302A (en) | 1987-12-18 | 1987-12-18 | Manufacture of alloy powder for bonded magnet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01162302A true JPH01162302A (en) | 1989-06-26 |
Family
ID=18135290
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62321686A Pending JPH01162302A (en) | 1987-12-18 | 1987-12-18 | Manufacture of alloy powder for bonded magnet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01162302A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0626703A2 (en) * | 1993-05-28 | 1994-11-30 | Rhone-Poulenc Specialty Chemicals Co. | Magnetically anisotropic spherical powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62101004A (en) * | 1985-10-28 | 1987-05-11 | Seiko Epson Corp | Rare earth-iron group permanent magnet |
| JPS62137808A (en) * | 1985-12-12 | 1987-06-20 | Mitsubishi Metal Corp | Manufacture of rare earth bonding magnet |
-
1987
- 1987-12-18 JP JP62321686A patent/JPH01162302A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62101004A (en) * | 1985-10-28 | 1987-05-11 | Seiko Epson Corp | Rare earth-iron group permanent magnet |
| JPS62137808A (en) * | 1985-12-12 | 1987-06-20 | Mitsubishi Metal Corp | Manufacture of rare earth bonding magnet |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0626703A2 (en) * | 1993-05-28 | 1994-11-30 | Rhone-Poulenc Specialty Chemicals Co. | Magnetically anisotropic spherical powder |
| EP0626703A3 (en) * | 1993-05-28 | 1995-01-25 | Rhone Poulenc Spec Chim | Magnetically anisotropic spherical powder. |
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