JPH11135312A - Permanent magnet powder - Google Patents
Permanent magnet powderInfo
- Publication number
- JPH11135312A JPH11135312A JP9309871A JP30987197A JPH11135312A JP H11135312 A JPH11135312 A JP H11135312A JP 9309871 A JP9309871 A JP 9309871A JP 30987197 A JP30987197 A JP 30987197A JP H11135312 A JPH11135312 A JP H11135312A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic
- magnet powder
- permanent magnet
- coercive force
- thin film
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 88
- 239000010409 thin film Substances 0.000 claims abstract description 51
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 20
- 230000005381 magnetic domain Effects 0.000 claims abstract description 16
- 239000006247 magnetic powder Substances 0.000 claims abstract description 12
- 230000008878 coupling Effects 0.000 claims abstract description 11
- 238000010168 coupling process Methods 0.000 claims abstract description 11
- 238000005859 coupling reaction Methods 0.000 claims abstract description 11
- 230000006911 nucleation Effects 0.000 claims description 12
- 238000010899 nucleation Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 9
- 150000003624 transition metals Chemical class 0.000 claims description 9
- 150000002910 rare earth metals Chemical class 0.000 claims description 7
- 229910000808 amorphous metal alloy Inorganic materials 0.000 claims description 6
- 230000005415 magnetization Effects 0.000 abstract description 26
- 239000010408 film Substances 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 11
- 230000007423 decrease Effects 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 abstract description 5
- 239000006249 magnetic particle Substances 0.000 abstract 3
- 238000009501 film coating Methods 0.000 abstract 2
- 238000004544 sputter deposition Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 11
- 238000005259 measurement Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 229910001172 neodymium magnet Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 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
- H01F1/0551—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0552—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
-
- 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
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]
【発明の属する技術分野】本発明は、永久磁石粉末に係
り、特に、保磁力の温度特性に優れた逆磁区核発生型永
久磁石粉末の改良に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a permanent magnet powder, and more particularly to an improvement of a reversed magnetic domain nucleation type permanent magnet powder having excellent temperature characteristics of coercive force.
【０００２】[0002]
【従来の技術】例えば、希土類−遷移金属系永久磁石は
高性能な永久磁石として知られているが、この希土類−
遷移金属系永久磁石の中でもＳｍＣｏ系やＳｍＦｅＮ
系、ＮｄＦｅＢ系等の急冷粉は粉末としても磁石特性を
発現するため、この粉末をエポキシ系、ナイロン系等の
合成樹脂や金属亜鉛等をバインダーとして成形し磁石と
する結合型磁石の用途に広く用いられている。2. Description of the Related Art Rare earth-transition metal permanent magnets are known as high-performance permanent magnets.
Among transition metal permanent magnets, SmCo-based and SmFeN
Quenched powders such as NdFeB-based and NdFeB-based powders also exhibit magnet properties even as powders. Used.
【０００３】[0003]
【発明が解決しようとする課題】ところで、これ等希土
類−遷移金属系の永久磁石は概してその温度特性が悪
く、特に、その保磁力が高温になるほど低下して磁力が
弱まるといった欠点を有していた。このため、これ等永
久磁石の室温での保磁力を高める等の手法を採ること
で、高温で保磁力が低下しても相対的に磁力が低下しな
いようにする試みがなされている。しかし、このような
方法では室温での保磁力が高くなり過ぎてしまい、これ
に起因して着磁が完全に行えなくなることから室温での
磁力が十分でない等の問題点を有していた。However, these rare earth-transition metal permanent magnets generally have poor temperature characteristics, and in particular, have the disadvantage that the coercive force decreases as the temperature increases and the magnetic force decreases. Was. For this reason, attempts have been made to increase the coercive force of these permanent magnets at room temperature so that the magnetic force does not relatively decrease even if the coercive force decreases at high temperatures. However, such a method has a problem in that the coercive force at room temperature becomes too high and magnetization cannot be completely performed due to this, so that the magnetic force at room temperature is not sufficient.
【０００４】本発明はこの様な問題点に着目してなされ
たもので、その課題とするところは、室温での保磁力を
適正に保ったまま（すなわち、室温での保磁力を高める
等の上記手法を採ることなく）、高温での保磁力の低下
が少ない温度特性に優れた永久磁石粉末を提供すること
にある。The present invention has been made in view of such a problem, and an object thereof is to maintain the coercive force at room temperature properly (ie, to increase the coercive force at room temperature, etc.). An object of the present invention is to provide a permanent magnet powder having excellent temperature characteristics with little decrease in coercive force at a high temperature without employing the above method).
【０００５】[0005]
【課題を解決するための手段】そこで、本発明者はこの
課題を解決するため鋭意研究を重ねた結果、希土類−遷
移金属系等の永久磁石粉末の表面を、この粉末とは別の
磁気特性を有する磁性薄膜で被覆し、かつ、永久磁石粉
末と上記磁性薄膜との間に交換結合力を作用させること
で、永久磁石粉末における保磁力の温度特性をある程度
任意に制御できることを見出すに至った。The inventor of the present invention has conducted intensive studies in order to solve this problem, and as a result, the surface of a permanent magnet powder such as a rare earth-transition metal system has been changed to a magnetic property different from that of this powder. It has been found that the temperature characteristics of the coercive force of the permanent magnet powder can be controlled to some extent by coating with a magnetic thin film having the above, and by applying an exchange coupling force between the permanent magnet powder and the magnetic thin film. .
【０００６】例えば、希土類−遷移金属系の永久磁石、
この中でもＳｍ1Ｃｏ5系、若しくはＳｍ2Ｆｅ17Ｎ3系、
あるいはＮｄＦｅＢ系磁石等逆磁区核発生型の保磁力発
生機構を持つ、いわゆるニュークリエーション型磁石で
は、保磁力の大きさはその逆磁区が発生する磁石表面の
状態に影響される。このため、磁石の表面を何らかの手
法で制御し、逆磁区発生の活性化エネルギーを制御でき
れば上記保磁力を制御することが可能となる。For example, rare earth-transition metal based permanent magnets,
Among them, Sm 1 Co 5 system or Sm 2 Fe 17 N 3 system,
Alternatively, in a so-called nucleation type magnet having a reverse magnetic domain nucleus generating type coercive force generating mechanism such as an NdFeB magnet, the magnitude of the coercive force is affected by the state of the magnet surface where the reverse magnetic domain is generated. For this reason, if the surface of the magnet can be controlled by some method and the activation energy for generating the reverse magnetic domain can be controlled, the coercive force can be controlled.
【０００７】一方、磁性相と軟磁性相をナノスケールで
微細に混在させることで、磁性相に近い保磁力と軟磁性
相の高い磁化を持つ磁石（交換スプリング磁石と呼ばれ
ている）ができることが知られている。これは、磁性相
と軟磁性相が交換結合により結合されることで、磁性相
の保磁力に引きずられて混合相全体の保磁力が高まるこ
とによるものである。On the other hand, by finely mixing the magnetic phase and the soft magnetic phase on a nano scale, a magnet having a coercive force close to the magnetic phase and a high magnetization of the soft magnetic phase (called an exchange spring magnet) can be obtained. It has been known. This is because the magnetic phase and the soft magnetic phase are coupled by exchange coupling, and are dragged by the coercive force of the magnetic phase to increase the coercive force of the entire mixed phase.
【０００８】そこで、この交換スプリング磁石の特徴を
応用して、逆磁区核発生型の永久磁石に対しその表面を
例えば保磁力の大きい別の磁性相で被覆し、かつ、この
磁性相と永久磁石との間に交換結合力を作用させた場
合、永久磁石の保磁力とその温度特性が改善されるとの
予測の下、鋭意実験を繰り返したところ、上述したよう
に希土類−遷移金属系等の永久磁石粉末における保磁力
の温度特性をある程度任意に制御できることを見出すに
至った。更に、逆磁区核発生型の永久磁石においてはご
く薄い表面の状態が保磁力に大きく作用するため、保磁
力の大きい上記磁性相はその膜厚が薄くても永久磁石に
おける保磁力制御の効果を発揮させることが可能とな
る。このことは、通常、特性が低くて磁石材料として使
えないような磁化の低い材料でも、保磁力さえ大きけれ
ば上記永久磁石の表面を被覆する磁性相として採用でき
ることを意味しておりその技術的意義は大きい。つま
り、上記永久磁石の保磁力制御のためにその表面を被覆
する磁性相は、その磁化が低くてもこの磁性相の膜厚を
薄く設定できることから、全体としての磁化は元の永久
磁石の特性をほぼ保持させることができ、永久磁石の保
磁力のみを表面の磁性相で制御できることを意味してい
るからである。本発明はこの様な技術的検討を経て完成
されたものである。Therefore, by applying the characteristics of the exchange spring magnet, the surface of the permanent magnet of the reverse magnetic domain nucleation type is coated with another magnetic phase having a large coercive force, for example. When an exchange coupling force was applied between the two, the coercive force of the permanent magnet and its temperature characteristics were predicted to be improved. It has been found that the temperature characteristics of the coercive force of the permanent magnet powder can be controlled to some extent arbitrarily. Further, in a reversed domain nucleation type permanent magnet, the extremely thin surface state has a large effect on the coercive force. It is possible to demonstrate. This means that a material having a low magnetization, which usually cannot be used as a magnet material because of its low properties, can be used as a magnetic phase covering the surface of the permanent magnet as long as the coercive force is large. Is big. In other words, the magnetic phase covering the surface for controlling the coercive force of the permanent magnet can be set to a thin film thickness even if its magnetization is low, so that the overall magnetization is the characteristic of the original permanent magnet. This means that only the coercive force of the permanent magnet can be controlled by the surface magnetic phase. The present invention has been completed through such technical studies.
【０００９】すなわち、請求項１に係る発明は、逆磁区
核発生型の保磁力発生機構を有する磁石粉末から成る永
久磁石粉末を前提とし、逆磁区核発生型の磁石粉末とこ
の磁石粉末の表面を被覆する保磁力の大きい磁性薄膜と
で構成され、かつ、磁石粉末と磁性薄膜との間に交換結
合力が作用していることを特徴とし、請求項２に係る発
明は、請求項１記載の永久磁石粉末を前提とし、上記逆
磁区核発生型の磁石粉末が、Ｓｍ1Ｃｏ5系、Ｓｍ2Ｆｅ
17Ｎ3系、及び、Ｎｄ2Ｆｅ14Ｂ1系から選択されたいず
れかの希土類−遷移金属系磁石粉末で構成されているこ
とを特徴とするものである。That is, the invention according to claim 1 is based on the premise that a permanent magnet powder made of a magnet powder having a reverse domain nucleus generation type coercive force generating mechanism is used. And a magnetic thin film having a large coercive force covering the magnetic powder, and an exchange coupling force acts between the magnet powder and the magnetic thin film. Assuming that the permanent magnet powder is of the type described above, the magnet powder of the reverse domain nucleation type is Sm 1 Co 5 system, Sm 2 Fe
17 N 3 based, and, any of the rare earth selected from Nd 2 Fe 14 B 1 type - is characterized in that it is constituted by a transition metal-based magnetic powder.
【００１０】次に、請求項３に係る発明は、請求項１ま
たは２記載の永久磁石粉末を前提とし、上記磁性薄膜が
希土類と遷移金属から成るアモルファス合金にて構成さ
れていることを特徴とし、請求項４に係る発明は、請求
項１、２または３記載の永久磁石粉末を前提とし、上記
磁性薄膜における保磁力の温度係数が室温で正であるこ
とを特徴とするものである。Next, a third aspect of the present invention is based on the permanent magnet powder of the first or second aspect, wherein the magnetic thin film is made of an amorphous alloy comprising a rare earth and a transition metal. The invention according to a fourth aspect is based on the permanent magnet powder according to the first, second or third aspect, wherein the temperature coefficient of coercive force in the magnetic thin film is positive at room temperature.
【００１１】[0011]
【発明の実施の形態】以下、本発明の実施の形態につい
て詳細に説明する。Embodiments of the present invention will be described below in detail.
【００１２】まず、本発明に係る永久磁石粉末は、上述
したように逆磁区核発生型の磁石粉末とこの磁石粉末の
表面を被覆する保磁力の大きい磁性薄膜とで構成され、
かつ、磁石粉末と磁性薄膜との間に交換結合力が作用し
ていることを特徴とするものである。First, the permanent magnet powder according to the present invention is composed of a magnetic domain nucleation type magnet powder as described above and a magnetic thin film having a large coercive force covering the surface of the magnet powder,
In addition, an exchange coupling force acts between the magnet powder and the magnetic thin film.
【００１３】そして、上記逆磁区核発生型の磁石粉末と
して、特に、Ｓｍ1Ｃｏ5系、若しくはＳｍ2Ｆｅ17Ｎ
3系、あるいはＮｄ2Ｆｅ14Ｂ1系から選択された希土類
−遷移金属系磁石粉末が適用された場合（請求項２）、
本発明の効果をより一層得ることができる。[0013] As the above-mentioned magnet powder of the reverse domain nucleus generation type, particularly, Sm 1 Co 5 -based or Sm 2 Fe 17 N
3 system, or Nd 2 Fe 14 B 1 type selected from rare earth - if a transition metal based magnet powder is applied (claim 2),
The effect of the present invention can be further obtained.
【００１４】また、上記磁石粉末の表面を被覆する磁性
薄膜としては、保磁力が大きく、好ましくは磁気異方性
が大きい材料で、例えば、希土類と遷移金属から成るア
モルファス合金が適用でき（請求項３）、具体的には、
Ｔｂ、Ｄｙ、Ｓｍ、Ｇｄの中から選択された少なくとも
一種の希土類と、Ｆｅ、Ｃｏの中から選択された少なく
とも一種の遷移金属からアモルファス合金が挙げられ、
特に希土類の原子割合が１５〜４０at％のアモルファス
合金が適している。また、高温下での保磁力の低下を抑
制する観点から、保磁力の温度係数が室温で正である磁
性薄膜の適用が好ましい（請求項４）。また、磁性薄膜
に適用されるこれ等合金には、上述した希土類や遷移金
属の元素以外に磁石粉末の耐食性等を改善する目的で、
Ｃｒ、Ｖ、Ｍｏ、Ｔｉ等の元素を１〜５at％程度添加し
てもよい。As the magnetic thin film covering the surface of the magnet powder, a material having a large coercive force and preferably a large magnetic anisotropy, for example, an amorphous alloy comprising a rare earth and a transition metal can be applied. 3) Specifically,
At least one rare earth element selected from Tb, Dy, Sm, and Gd, and an amorphous alloy from at least one transition metal selected from Fe and Co,
In particular, an amorphous alloy having an atomic ratio of rare earth of 15 to 40 at% is suitable. From the viewpoint of suppressing a decrease in coercive force at a high temperature, it is preferable to use a magnetic thin film whose temperature coefficient of coercive force is positive at room temperature (claim 4). In addition, these alloys applied to the magnetic thin film include, for the purpose of improving the corrosion resistance and the like of the magnet powder in addition to the rare earth and transition metal elements described above,
Elements such as Cr, V, Mo, and Ti may be added at about 1 to 5 at%.
【００１５】次に、希土類−遷移金属系等の上記磁石粉
末の表面に磁性薄膜を被覆する方法は任意であり、例え
ば、図２に示すように製膜室（容器）１内にモータ２０
で駆動される撹拌羽２を設置し、この攪拌羽２で磁石粉
末１００を撹拌させながら製膜を行うスパッタリングや
蒸着法等の物理的気相成長（ＰＶＤ）法、あるいは、熱
ＣＶＤ、プラズマＣＶＤ等の化学的気相成長（ＣＶＤ）
法等で磁性薄膜を被覆することができる。尚、上記撹拌
羽２に変えて図３に示すように製膜室（容器）１の底面
側に偏芯モータ３を設置し、この偏芯モータ３により製
膜室（容器）１内の磁石粉末１００を振動させながらＰ
ＶＤ法やＣＶＤ法で磁性薄膜を被覆することも可能であ
る。尚、希土類−遷移金属系等の磁石粉末と磁性薄膜と
の間に交換結合力が確実に作用するようにするため、磁
性薄膜が製膜される前の磁石粉末についてはその表面を
エッチング処理する等、希土類−遷移金属系等の磁石粉
末表面に酸化層等の異物が存在しないようにすることが
望ましい。Next, the method of coating the surface of the magnet powder of a rare earth-transition metal or the like with a magnetic thin film is optional. For example, as shown in FIG.
A physical vapor deposition (PVD) method such as a sputtering or vapor deposition method in which a film is formed while stirring the magnetic powder 100 with the stirring blade 2, or a thermal CVD or a plasma CVD. Chemical vapor deposition (CVD)
The magnetic thin film can be coated by a method or the like. As shown in FIG. 3, an eccentric motor 3 is installed on the bottom surface side of the film forming chamber (container) 1 instead of the stirring blade 2, and the eccentric motor 3 controls the magnet in the film forming chamber (container) 1. P while vibrating powder 100
The magnetic thin film can be coated by a VD method or a CVD method. In order to ensure that the exchange coupling force acts between the rare earth-transition metal based magnet powder and the magnetic thin film, the surface of the magnet powder before the magnetic thin film is formed is subjected to an etching treatment. It is desirable that there be no foreign matter such as an oxide layer on the surface of the rare earth-transition metal based magnet powder.
【００１６】また、希土類−遷移金属系等の磁石粉末の
表面に被覆する磁性薄膜の膜厚については磁石粉末にお
ける保磁力の改善が図れる範囲において任意に設定され
るが、上述した希土類と遷移金属から成るアモルファス
合金を適用する場合、上記磁性薄膜の膜厚は３０Å（オ
ングストローム）以上に設定することが好ましい。３０
Å（オングストローム）未満の場合、例えば希土類−遷
移金属系の磁石粉末における保磁力制御の効果が十分に
現れないことがあるからである。他方、上記膜厚の上限
は特にないが、２０００Å（オングストローム）を越え
る厚さに設定しても保磁力制御の効果はあまり変わら
ず、かえって生産性が低下したり保磁力以外の磁気特
性、特に磁化が低下する場合があるため２０００Å（オ
ングストローム）以下に設定することが好ましい。The thickness of the magnetic thin film that covers the surface of the rare earth-transition metal based magnetic powder is arbitrarily set within a range where the coercive force of the magnet powder can be improved. When an amorphous alloy consisting of: is used, the thickness of the magnetic thin film is preferably set to 30 ° (angstrom) or more. 30
If it is less than Å (angstrom), for example, the effect of controlling the coercive force of rare earth-transition metal based magnet powder may not be sufficiently exhibited. On the other hand, although there is no particular upper limit of the film thickness, the effect of the coercive force control does not change so much even if the film thickness is set to more than 2000 ° (angstrom). On the contrary, the productivity is reduced and the magnetic properties other than the coercive force, especially Since the magnetization may decrease, it is preferable to set the angle to 2000 ° (angstrom) or less.
【００１７】[0017]
【実施例】以下、本発明の実施例について具体的に説明
する。Embodiments of the present invention will be specifically described below.
【００１８】尚、図２と図３は本実施例で使用されたス
パッタリング装置の概略構成を示す説明図である。すな
わち、図２で示されるスパッタリング装置は、上方側に
真空排気系５とアルゴンガス（Ａｒ）導入系６が設けら
れかつアースされた製膜室（容器）１と、この製膜室
（容器）１内に配置されたカソード７と、このカソード
７に接続されたスパッタ用電源７０と、上記カソード７
に取付けられたスパッタターゲット９と、上記製膜室
（容器）１内に設置された撹拌羽２と、この撹拌羽２を
回転駆動するモータ２０とでその主要部が構成されてい
る。FIGS. 2 and 3 are explanatory views showing the schematic arrangement of the sputtering apparatus used in this embodiment. That is, the sputtering apparatus shown in FIG. 2 is provided with a vacuum evacuation system 5 and an argon gas (Ar) introduction system 6 on the upper side and is grounded and a film forming chamber (container) 1 and this film forming chamber (container) 1, a cathode power supply 70 connected to the cathode 7,
The main parts are constituted by a sputter target 9 attached to the above, a stirring blade 2 installed in the film forming chamber (container) 1, and a motor 20 for rotating the stirring blade 2.
【００１９】他方、図３で示されるスパッタリング装置
は、図２のスパッタリング装置で用いられた撹拌羽２と
モータ２０に代えて偏芯モータ３が適用され、かつ、製
膜室（容器）１の底面側に取付けられたスプリング状支
持部１０により製膜室（容器）１が振動可能に支持され
ている点を除いて図２のスパッタリング装置と略同一で
ある。On the other hand, the sputtering apparatus shown in FIG. 3 employs an eccentric motor 3 instead of the stirring blade 2 and the motor 20 used in the sputtering apparatus shown in FIG. It is substantially the same as the sputtering apparatus of FIG. 2 except that the film forming chamber (container) 1 is supported so as to be able to vibrate by a spring-like supporting portion 10 attached to the bottom surface side.
【００２０】［実施例１］予め表面がエッチングされた
平均粒径６μｍのＳｍＦｅＮ系（Ｓｍ：24.0重量％、Ｆ
ｅ：72.5重量％、Ｎ：3.5重量％）永久磁石粉末５００
ｇを図２に示されたスパッタリング装置の製膜室（容
器）１内に収容した。尚、スパッタリング装置のカソー
ド７にはスパッタターゲット９としてＴｂが２５at％、
Ｆｅが７５at％の合金ターゲットが取付けられている。Example 1 An SmFeN-based material having an average particle diameter of 6 μm (Sm: 24.0% by weight, F
e: 72.5% by weight, N: 3.5% by weight) Permanent magnet powder 500
g was housed in the film forming chamber (vessel) 1 of the sputtering apparatus shown in FIG. The cathode 7 of the sputtering apparatus had Tb of 25 at% as a sputtering target 9.
An alloy target with 75 at% Fe is mounted.
【００２１】次に、製膜室（容器）１内を真空に引いた
後、上記製膜室（容器）１内が１×１０-2torrとなるよ
うにアルゴンガスを導入した。Next, after the inside of the film forming chamber (container) 1 was evacuated, argon gas was introduced so that the inside of the film forming chamber (container) 1 became 1 × 10 -2 torr.
【００２２】次に、上記撹拌羽２を回転させて磁石粉末
１００を撹拌しながらカソード７に−５００Ｖの電圧を
かけ、スパッタリングを３時間行って磁石粉末１００の
表面に上記合金ターゲットと同一組成の磁性薄膜を製膜
した。尚、磁性薄膜の膜厚は１０００Å（オングストロ
ーム）であった。Next, a voltage of -500 V is applied to the cathode 7 while rotating the stirring blades 2 to stir the magnet powder 100, and sputtering is performed for 3 hours, so that the surface of the magnet powder 100 has the same composition as the alloy target. A magnetic thin film was formed. The thickness of the magnetic thin film was 1000 ° (angstrom).
【００２３】そして、磁性薄膜により表面が覆われた実
施例１に係る永久磁石粉末について２５℃と１００℃条
件下における磁気特性（残留磁化と保磁力）をそれぞれ
測定した。測定結果を以下の表１に示す。The magnetic properties (residual magnetization and coercive force) of the permanent magnet powder according to Example 1 whose surface was covered with the magnetic thin film were measured at 25 ° C. and 100 ° C., respectively. The measurement results are shown in Table 1 below.
【００２４】また、実施例１に係る永久磁石粉末の磁化
曲線も合わせて求めた。Further, the magnetization curve of the permanent magnet powder according to Example 1 was also determined.
【００２５】尚、図１は磁化曲線の模式図であり、実施
例１に係る永久磁石粉末の磁化曲線を実線ａで示す。ま
た、一点鎖線ｂは上記磁性薄膜を被覆する前の永久磁石
粉末の磁化曲線、二点鎖線ｃは上記磁性薄膜の磁化曲線
をそれぞれ示す。FIG. 1 is a schematic diagram of a magnetization curve, and the magnetization curve of the permanent magnet powder according to Example 1 is indicated by a solid line a. The dashed line b indicates the magnetization curve of the permanent magnet powder before coating the magnetic thin film, and the dashed line c indicates the magnetization curve of the magnetic thin film.
【００２６】そして、実線ａ、一点鎖線ｂ、二点鎖線ｃ
から明らかなように、実施例１に係る永久磁石粉末の磁
化曲線上は、磁性薄膜を被覆する前の永久磁石粉末、上
記磁性薄膜を単独で測定したものの単純な加算ではな
く、一つの段のないループを示していて磁石粉末と磁性
薄膜との間に交換結合力が十分作用していることが確認
される。The solid line a, the one-dot chain line b, and the two-dot chain line c
As is apparent from the graph, the magnetization curve of the permanent magnet powder according to the example 1 is not a simple addition of the permanent magnet powder before coating the magnetic thin film and the magnetic thin film alone, but one step. It shows no loop, confirming that the exchange coupling force is sufficiently acting between the magnet powder and the magnetic thin film.
【００２７】［実施例２］スパッタリング時間が８分間
で、製膜された上記磁性薄膜の膜厚が５０Å（オングス
トローム）であった点を除き実施例１と略同一の工程に
従い、磁石粉末とその表面を被覆する磁性薄膜とで構成
された実施例２に係る永久磁石粉末を製造した。Example 2 A magnet powder and a magnetic powder were formed according to substantially the same steps as in Example 1 except that the sputtering time was 8 minutes and the thickness of the formed magnetic thin film was 50 ° (angstrom). A permanent magnet powder according to Example 2 comprising a magnetic thin film covering the surface was manufactured.
【００２８】そして、実施例２に係る永久磁石粉末につ
いても２５℃と１００℃条件下における磁気特性（残留
磁化と保磁力）をそれぞれ測定した。測定結果を以下の
表１に示す。The magnetic properties (residual magnetization and coercive force) of the permanent magnet powder according to Example 2 were measured at 25 ° C. and 100 ° C., respectively. The measurement results are shown in Table 1 below.
【００２９】［実施例３］スパッタリング時間が３分間
で、製膜された上記磁性薄膜の膜厚が１５Å（オングス
トローム）であった点を除き実施例１と略同一の工程に
従い、磁石粉末とその表面を被覆する磁性薄膜とで構成
された実施例３に係る永久磁石粉末を製造した。Example 3 A magnet powder and a magnetic powder were prepared according to substantially the same steps as in Example 1 except that the sputtering time was 3 minutes and the thickness of the formed magnetic thin film was 15 ° (angstrom). A permanent magnet powder according to Example 3 constituted by a magnetic thin film covering the surface was manufactured.
【００３０】そして、実施例３に係る永久磁石粉末につ
いても２５℃と１００℃条件下における磁気特性（残留
磁化と保磁力）をそれぞれ測定した。測定結果を以下の
表１に示す。The magnetic properties (residual magnetization and coercive force) of the permanent magnet powder according to Example 3 were measured at 25 ° C. and 100 ° C., respectively. The measurement results are shown in Table 1 below.
【００３１】［実施例４］スパッタリング時間が１０時
間で、製膜された上記磁性薄膜の膜厚が３５００Å（オ
ングストローム）であった点を除き実施例１と略同一の
工程に従い、磁石粉末とその表面を被覆する磁性薄膜と
で構成された実施例４に係る永久磁石粉末を製造した。Example 4 The procedure of Example 1 was repeated except that the sputtering time was 10 hours and the thickness of the formed magnetic thin film was 3500 ° (angstrom). A permanent magnet powder according to Example 4 including a magnetic thin film covering the surface was manufactured.
【００３２】そして、実施例４に係る永久磁石粉末につ
いても２５℃と１００℃条件下における磁気特性（残留
磁化と保磁力）をそれぞれ測定した。測定結果を以下の
表１に示す。The magnetic properties (residual magnetization and coercive force) of the permanent magnet powder according to Example 4 were measured at 25 ° C. and 100 ° C., respectively. The measurement results are shown in Table 1 below.
【００３３】［実施例５］図３に示されたスパッタリン
グ装置が用いられている点を除き実施例１と略同一の工
程に従い、磁石粉末とその表面を被覆する磁性薄膜とで
構成された実施例５に係る永久磁石粉末を製造した。[Embodiment 5] An embodiment comprising a magnet powder and a magnetic thin film covering the surface thereof according to substantially the same steps as in Embodiment 1 except that the sputtering apparatus shown in FIG. 3 is used. A permanent magnet powder according to Example 5 was produced.
【００３４】そして、実施例５に係る永久磁石粉末につ
いても２５℃と１００℃条件下における磁気特性（残留
磁化と保磁力）をそれぞれ測定した。測定結果を以下の
表１に示す。The magnetic properties (residual magnetization and coercive force) of the permanent magnet powder according to Example 5 were measured at 25 ° C. and 100 ° C., respectively. The measurement results are shown in Table 1 below.
【００３５】［実施例６］平均粒径６μｍのＳｍＦｅＮ
系（Ｓｍ：24.0重量％、Ｆｅ：72.5重量％、Ｎ：3.5重
量％）永久磁石粉末に変えて平均粒径２０μｍのＳｍＣ
ｏ系（Ｓｍ：25.5重量％、Ｃｏ：66.9重量％、Ｐｒ：7.
6重量％）永久磁石粉末を適用している点と、スパッタ
リング時間が１時間である点を除き実施例１と略同一の
工程に従い、磁石粉末とその表面を被覆する磁性薄膜と
で構成された実施例６に係る永久磁石粉末を製造した。Example 6 SmFeN having an average particle size of 6 μm
System (Sm: 24.0% by weight, Fe: 72.5% by weight, N: 3.5% by weight) SmC with an average particle size of 20 μm instead of permanent magnet powder
o system (Sm: 25.5% by weight, Co: 66.9% by weight, Pr: 7.
6% by weight) The magnet powder and the magnetic thin film covering the surface were formed according to substantially the same steps as in Example 1 except that the permanent magnet powder was applied and the sputtering time was 1 hour. Example 6 A permanent magnet powder according to Example 6 was manufactured.
【００３６】そして、実施例６に係る永久磁石粉末につ
いても２５℃と１００℃条件下における磁気特性（残留
磁化と保磁力）をそれぞれ測定した。測定結果を以下の
表１に示す。The magnetic properties (residual magnetization and coercive force) of the permanent magnet powder of Example 6 were measured at 25 ° C. and 100 ° C., respectively. The measurement results are shown in Table 1 below.
【００３７】［比較例１］磁性薄膜が被覆されていない
平均粒径６μｍのＳｍＦｅＮ系（Ｓｍ：24.0重量％、Ｆ
ｅ：72.5重量％、Ｎ：3.5重量％）永久磁石粉末自体を
比較例１に係る永久磁石粉末とする。Comparative Example 1 An SmFeN-based material having an average particle size of 6 μm (Sm: 24.0 wt%, F
e: 72.5% by weight, N: 3.5% by weight) The permanent magnet powder itself is used as the permanent magnet powder according to Comparative Example 1.
【００３８】そして、比較例１に係る永久磁石粉末につ
いても２５℃と１００℃条件下における磁気特性（残留
磁化と保磁力）をそれぞれ測定した。測定結果を以下の
表１に示す。The magnetic properties (residual magnetization and coercive force) of the permanent magnet powder according to Comparative Example 1 were measured at 25 ° C. and 100 ° C., respectively. The measurement results are shown in Table 1 below.
【００３９】［比較例２］磁性薄膜が被覆されていない
平均粒径２０μｍのＳｍＣｏ系（Ｓｍ：25.5重量％、Ｃ
ｏ：66.9重量％、Ｐｒ：7.6重量％）永久磁石粉末自体
を比較例２に係る永久磁石粉末とする。Comparative Example 2 An SmCo-based material having an average particle size of 20 μm (Sm: 25.5% by weight, C
o: 66.9% by weight, Pr: 7.6% by weight) The permanent magnet powder itself is used as the permanent magnet powder according to Comparative Example 2.
【００４０】そして、比較例２に係る永久磁石粉末につ
いても２５℃と１００℃条件下における磁気特性（残留
磁化と保磁力）をそれぞれ測定した。測定結果を以下の
表１に示す。The magnetic properties (residual magnetization and coercive force) of the permanent magnet powder according to Comparative Example 2 were measured at 25 ° C. and 100 ° C., respectively. The measurement results are shown in Table 1 below.
【００４１】[0041]
【表１】 [Table 1]
【００４２】（評 価） （１）実施例１〜５と比較例１との比較、並びに、実施
例６と比較例２との比較から、測定温度２５℃下での残
留磁化と保磁力の値は実施例と比較例とで大きな差異は
認められないが、測定温度１００℃下での残留磁化と保
磁力の値は実施例と比較例とで大きな差異が認められ
る。このことから、各比較例に係る永久磁石粉末に較べ
て各実施例に係る永久磁石粉末は保磁力の温度変化が少
なく、優れた温度特性を具備していることが評価され
る。(Evaluation) (1) From the comparison between Examples 1 to 5 and Comparative Example 1 and the comparison between Example 6 and Comparative Example 2, the residual magnetization and coercive force at a measurement temperature of 25 ° C. Although there is no significant difference between the values of the embodiment and the comparative example, the values of the residual magnetization and the coercive force at the measurement temperature of 100 ° C. are significantly different between the example and the comparative example. From this, it is evaluated that the permanent magnet powder according to each of the examples has less temperature change of coercive force and has excellent temperature characteristics as compared with the permanent magnet powder according to each of the comparative examples.
【００４３】（２）また、実施例３と実施例１〜２との
比較から、磁石粉末表面を被覆する上記磁性薄膜の膜厚
が１５Å（オングストローム）と極端に薄い場合には、
磁性薄膜を設けたことによる保磁力の改善効果が若干弱
いことも確認される。(2) From the comparison between Example 3 and Examples 1 and 2, when the thickness of the magnetic thin film covering the surface of the magnet powder is extremely thin, 15 ° (angstrom),
It is also confirmed that the effect of improving the coercive force by providing the magnetic thin film is slightly weak.
【００４４】（３）他方、実施例４と実施例１〜２との
比較から、磁石粉末表面を被覆する上記磁性薄膜の膜厚
が３５００Å（オングストローム）と必要以上に厚く設
定されている場合、磁性薄膜を設けたことによる保磁力
の改善効果は認められるが、適正膜厚の実施例１〜２よ
り優れた結果とはなっておらず、かえって残留磁化が他
の実施例より若干劣ってしまう傾向が確認される。(3) On the other hand, from the comparison between Example 4 and Examples 1 and 2, when the thickness of the magnetic thin film covering the surface of the magnet powder is set to 3500 ° (angstrom), which is unnecessarily large, Although the effect of improving the coercive force due to the provision of the magnetic thin film is recognized, the results are not superior to those of Examples 1 and 2 having an appropriate film thickness, and the residual magnetization is slightly inferior to the other examples. A trend is confirmed.
【００４５】[0045]
【発明の効果】請求項１〜３記載の発明に係る永久磁石
粉末によれば、逆磁区核発生型の磁石粉末表面が別の磁
性薄膜で被覆されていることから上記表面での逆磁区核
の発生が抑制され、かつ、磁石粉末と保磁力の大きい上
記磁性薄膜との間に交換結合力が作用しているため永久
磁石粉末における保磁力を制御することが可能となる。According to the permanent magnet powder according to the first to third aspects of the present invention, since the surface of the reverse magnetic domain nucleation type magnet powder is coated with another magnetic thin film, the reverse magnetic domain nuclei on the surface are provided. Is suppressed, and an exchange coupling force acts between the magnet powder and the magnetic thin film having a large coercive force, so that the coercive force of the permanent magnet powder can be controlled.
【００４６】更に、逆磁区核発生型の磁石粉末表面を被
覆する磁性膜は薄膜であることから上記磁石粉末の保磁
力以外の磁気特性は保持される。Further, since the magnetic film covering the surface of the reverse magnetic domain nucleation type magnet powder is a thin film, magnetic properties other than the coercive force of the magnet powder are maintained.
【００４７】従って、逆磁区核発生型の磁石粉末におけ
る磁化等の磁気特性を保持したまま保磁力の温度特性が
改善される効果を有している。Therefore, there is an effect that the temperature characteristics of the coercive force are improved while maintaining the magnetic characteristics such as magnetization in the reverse magnetic domain nucleation type magnet powder.
【００４８】特に、請求項４記載の発明に係る永久磁石
粉末によれば、逆磁区核発生型の磁石粉末表面を被覆す
る上記磁性薄膜における保磁力の温度係数が室温で正で
あるため、希土類−遷移金属系等の永久磁石における保
磁力の温度特性を更に改善できる効果を有している。In particular, according to the permanent magnet powder according to the fourth aspect of the present invention, since the temperature coefficient of coercive force of the magnetic thin film covering the surface of the reverse magnetic domain nucleation type magnet powder is positive at room temperature, -Has the effect of further improving the temperature characteristics of the coercive force of a permanent magnet such as a transition metal.
【図１】実施例１に係る永久磁石粉末の磁化曲線の模式
図。FIG. 1 is a schematic diagram of a magnetization curve of a permanent magnet powder according to Example 1.
【図２】実施例で用いられたスパッタリング装置の概略
構成説明図。FIG. 2 is a schematic structural explanatory view of a sputtering apparatus used in an example.
【図３】実施例で用いられた他のスパッタリング装置の
概略構成説明図。FIG. 3 is a schematic structural explanatory view of another sputtering apparatus used in the embodiment.
１ 製膜室（容器） ２ 撹拌羽 ３ 偏芯モータ ７ カソード ９ スパッタターゲット ２０ モータ １００ 磁石粉末 DESCRIPTION OF SYMBOLS 1 Film-forming chamber (vessel) 2 Stirring blade 3 Eccentric motor 7 Cathode 9 Sputter target 20 Motor 100 Magnet powder
Claims (4)
の表面を被覆する保磁力の大きい磁性薄膜とで構成さ
れ、かつ、磁石粉末と磁性薄膜との間に交換結合力が作
用していることを特徴とする永久磁石粉末。1. A magnetic powder comprising reverse magnetic domain nucleation type magnetic powder and a magnetic thin film having a large coercive force covering the surface of the magnetic powder, and an exchange coupling force acts between the magnetic powder and the magnetic thin film. Permanent magnet powder characterized by having.
Ｃｏ5系、Ｓｍ2Ｆｅ17Ｎ3系、及び、Ｎｄ2Ｆｅ14Ｂ1系
から選択されたいずれかの希土類−遷移金属系磁石粉末
で構成されていることを特徴とする請求項１記載の永久
磁石粉末。2. The method according to claim 1, wherein said reverse magnetic domain nucleation type magnet powder is Sm 1
Co 5 system, Sm 2 Fe 17 N 3 based, and, either selected from Nd 2 Fe 14 B 1 type rare earth - according to claim 1, characterized in that it is constituted by a transition metal-based magnetic powder Permanent magnet powder.
るアモルファス合金にて構成されていることを特徴とす
る請求項１または２記載の永久磁石粉末。3. The permanent magnet powder according to claim 1, wherein the magnetic thin film is made of an amorphous alloy comprising a rare earth and a transition metal.
室温で正であることを特徴とする請求項１、２または３
記載の永久磁石粉末。4. The magnetic thin film according to claim 1, wherein the temperature coefficient of coercive force is positive at room temperature.
The permanent magnet powder as described.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9309871A JPH11135312A (en) | 1997-10-24 | 1997-10-24 | Permanent magnet powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9309871A JPH11135312A (en) | 1997-10-24 | 1997-10-24 | Permanent magnet powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11135312A true JPH11135312A (en) | 1999-05-21 |
Family
ID=17998311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9309871A Pending JPH11135312A (en) | 1997-10-24 | 1997-10-24 | Permanent magnet powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11135312A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008251993A (en) * | 2007-03-30 | 2008-10-16 | Tdk Corp | Magnetic material and magnet using the same |
| JP2013219352A (en) * | 2012-04-04 | 2013-10-24 | Gm Grobal Technology Operations Llc | Vibrator for performing powder coating |
| DE102012000421B4 (en) | 2011-01-14 | 2023-09-28 | GM Global Technology Operations, LLC (n.d. Ges. d. Staates Delaware) | Method for producing sintered Nd-Fe-B magnets with Dy or Tb |
-
1997
- 1997-10-24 JP JP9309871A patent/JPH11135312A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008251993A (en) * | 2007-03-30 | 2008-10-16 | Tdk Corp | Magnetic material and magnet using the same |
| DE102012000421B4 (en) | 2011-01-14 | 2023-09-28 | GM Global Technology Operations, LLC (n.d. Ges. d. Staates Delaware) | Method for producing sintered Nd-Fe-B magnets with Dy or Tb |
| JP2013219352A (en) * | 2012-04-04 | 2013-10-24 | Gm Grobal Technology Operations Llc | Vibrator for performing powder coating |
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