JPS61114502A - Manufacture of samarium-cobalt magnet powder for resin magnet - Google Patents

Manufacture of samarium-cobalt magnet powder for resin magnet

Info

Publication number
JPS61114502A
JPS61114502A JP59235077A JP23507784A JPS61114502A JP S61114502 A JPS61114502 A JP S61114502A JP 59235077 A JP59235077 A JP 59235077A JP 23507784 A JP23507784 A JP 23507784A JP S61114502 A JPS61114502 A JP S61114502A
Authority
JP
Japan
Prior art keywords
samarium
powder
magnet powder
magnet
weight
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
Application number
JP59235077A
Other languages
Japanese (ja)
Inventor
Junichi Ishii
純一 石井
Koichi Oka
岡 公一
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Metal Mining Co Ltd
Original Assignee
Sumitomo Metal Mining Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sumitomo Metal Mining Co Ltd filed Critical Sumitomo Metal Mining Co Ltd
Priority to JP59235077A priority Critical patent/JPS61114502A/en
Priority to US06/796,224 priority patent/US4664723A/en
Publication of JPS61114502A publication Critical patent/JPS61114502A/en
Pending legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/0555Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
    • H01F1/0558Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together bonded together
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/0551Alloys 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

PURPOSE:To manufacture SmCo5 magnet powder by performing a reduction- diffusing method without adding other elements by a method wherein the impurities containing a samarium oxide, the percentage of content of the samarium oxide, and the percentage of content of the samarium contained in the magnet powder are specified properly. CONSTITUTION:The samarium oxide, to be used as the material for magnetic powder, contains lanthanum, cerium, praseoxymium and neodymium of 1.3wt% or below as impurities. The above-mentioned materials are contained in the ratio of 1.7wt% in total. The compounding of materials is performed in such a manner that the samarium contained in the magnetic powder becomes 32.7-33.4wt%. By compounding the materials as above-mentioned, the magnet powder having excellent magnetic characteristics can be stably manufactured at low cost by performing a reduction-diffusing method without adding other elements.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、優れた磁気的特性を有し樹脂磁石用に好適の
5inos系磁石粉末を°還元拡散法によって安定して
簡便に製造する方法に関する。
[Detailed Description of the Invention] [Industrial Application Field] The present invention provides a method for stably and easily producing 5inos-based magnet powder, which has excellent magnetic properties and is suitable for resin magnets, by a reduction diffusion method. Regarding.

〔従来の技術〕[Conventional technology]

従来、樹脂磁石用の5IIICO5系磁石粉末を製造す
るのに、サマリウム酸化物とコバルト粉末を配合した混
合物を加熱して、該サマリウム酸化物を蒸気状や混合し
た固体状のカルシウムのような還元剤で還元し生成した
サマリウムを該コバルト粉末中に拡散させた後、得られ
た反応生成物を水中に投入してスラリー状にし、該スラ
リーを水および酸水溶液で処理する、いわゆる還元拡散
法等が採用されている。そして、このような方法によっ
て製造されるSmC:os系磁石粉末の磁気的特性を向
上させるために、プラセオジム、ゲルマニウム等の元素
を添加する方法は公知である。
Conventionally, to produce 5IIICO5-based magnet powder for resin magnets, a mixture of samarium oxide and cobalt powder is heated, and the samarium oxide is mixed with a reducing agent such as vapor or solid calcium. The so-called reduction-diffusion method involves diffusing the samarium produced by reduction into the cobalt powder, pouring the resulting reaction product into water to form a slurry, and treating the slurry with water and an acid aqueous solution. It has been adopted. In order to improve the magnetic properties of the SmC:os magnet powder produced by such a method, a method of adding elements such as praseodymium and germanium is known.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

しかしながら、上記添加による方法は、繁雑であり、ま
た得られるSmCo5系磁石粉末の磁気的特性がバラク
いて不安定である傾向を存する。
However, the above-mentioned addition method is complicated, and the magnetic properties of the obtained SmCo5-based magnet powder tend to vary and become unstable.

本発明者等は、このような観点から優れた磁気的特性を
有し樹脂磁石用に好適のSmCo5系磁石粉末を、還元
拡散法によって他元素を添加することなく、安定して簡
便に製造することのできる方法を提供すべく、鋭意研究
した。
From this point of view, the present inventors aim to stably and easily produce SmCo5-based magnet powder, which has excellent magnetic properties and is suitable for resin magnets, by a reduction diffusion method without adding other elements. We have conducted extensive research to find a way to do this.

〔問題点を解決するための手段〕[Means for solving problems]

その結果、原料としてサマリウム酸化物は、不純物とし
てランタン、セリウム、プラセオジムおよびネオジムを
いずれも1.3重量%以下で、それらの合計が1.7重
量%以下含有するものを使用し、且つ原料の配合は製造
されるSmCo5系磁石粉末中のサマリウムが32.7
〜33.4重量%になるように行なうことによりて、前
記目的が達成され得ることを見出したものである。
As a result, we used samarium oxide as a raw material that contained lanthanum, cerium, praseodymium, and neodymium as impurities at 1.3% by weight or less, and the total of these was 1.7% by weight or less, and The composition is such that samarium in the manufactured SmCo5 magnet powder is 32.7.
It has been found that the above object can be achieved by adjusting the amount to 33.4% by weight.

〔作  用〕[For production]

以下、本発明を更に詳細に説明する。 The present invention will be explained in more detail below.

本発明において原料として使用するサマリウム酸化物を
不純物としてランタン、セリウム、プラセオジムおよび
ネオジムをいずれも1.3重量%以下で、それらの合計
が1.7重量%以下含有するものに限定したのは、含有
されるランタン、セリウム、プラセオジムおよびネオジ
ムのうち少くとも1つが1.3重量%を超えるか、それ
らの合計が1.7を量%を超えると、製造される磁石粉
末の磁気的特性、特に保磁力が急激に低下するからであ
る。
The samarium oxide used as a raw material in the present invention is limited to containing impurities of lanthanum, cerium, praseodymium, and neodymium in an amount of 1.3% by weight or less, and a total of 1.7% by weight or less. If at least one of lanthanum, cerium, praseodymium, and neodymium contained exceeds 1.3% by weight, or the sum of them exceeds 1.7% by weight, the magnetic properties of the produced magnet powder, especially This is because the coercive force decreases rapidly.

次に、原料の配合を、製造される磁石粉末中のサマリウ
ムが32.7〜33.4重量%になるように行なうよう
にしたのは、32.7重量%未満では製造された磁石粉
末中にS [llC01?相が生成し過ぎ、保磁力が急
激に低下し、一方、33.4重量%を超えるとSm2C
ot相が生成し残留磁束密度が低下するからである。
Next, the raw materials were blended so that samarium in the manufactured magnet powder was 32.7 to 33.4% by weight. niS [llC01? Excessive phase formation causes a sudden drop in coercive force.On the other hand, when it exceeds 33.4% by weight, Sm2C
This is because the ot phase is generated and the residual magnetic flux density decreases.

還元拡散反応で得られた反応生成物には、溶体化処理、
時効処理、均一化処理などの熱処理を施さないことが必
要である。このような熱処理を施すと、施さない場合よ
り磁気的特性が低下する。
The reaction products obtained from the reduction-diffusion reaction are subjected to solution treatment,
It is necessary not to perform heat treatments such as aging treatment and homogenization treatment. When such heat treatment is performed, the magnetic properties are lower than when no heat treatment is performed.

この磁気的特性の低下は、熱処理によって磁石粉末中の
サマリウムが上記の限定範囲である32.7〜33.4
重量%から外れたり、またはこの範囲内にあってもSm
Co5相以外にS mIC017、Sm2Cot、5I
IIC03などの相が生成したりすることによるものと
推察される。
This decrease in magnetic properties is caused by heat treatment when samarium in the magnet powder falls within the above limited range of 32.7 to 33.4.
Even if it deviates from the weight% or is within this range, Sm
In addition to Co5 phase, S mIC017, Sm2Cot, 5I
It is presumed that this is due to the formation of phases such as IIC03.

〔実 施 例〕〔Example〕

以下、本発明を実施例について説明する。 Hereinafter, the present invention will be explained with reference to examples.

実施例1 不純物としてLa、 Ce、 Pr、 Ndを第1表の
上うに含有する5IIltO1粉132〜147g、C
o粉た。
Example 1 132 to 147 g of 5IIltO1 powder containing La, Ce, Pr, and Nd as impurities as shown in Table 1, C
o powder.

(以下空白) #51表 このポットを反応装置に装入し、Arガス中で装置を加
熱し980℃で1時間保持した後、加熱を停止して常温
まで冷却した。得られた反応生成物を水およびpH約2
.5の希酢酸で処理して、含有されるCaO1未反応C
aを分離除去した。得られた粉末は、付着水分をアルコ
ールで置換した後、乾燥した。更に、これらの粉末を回
転ボールミルに装入し、エチルアルコールを満たして2
hr粉砕した。こうして得られた粉末の組成を第2表に
示す。これら粉末の一部をX線分析にかけた所、試験N
o、1.3はいずれも単−相のSmCo1金属間化合物
から成っていることが判った。しかし、試験No、13
.16はいず・れもSmCo5相の他に5111cO+
、相が認められ、また試験No、15,17はいずれも
5IIICos相の他に5IIIC03相、5ffit
COr相が認められた。
(Blank below) Table #51 This pot was placed in a reaction apparatus, heated in Ar gas and held at 980°C for 1 hour, then heating was stopped and cooled to room temperature. The resulting reaction product was mixed with water and pH approx.
.. 5 of dilute acetic acid to remove the contained CaO1 and unreacted C.
a was separated and removed. The obtained powder was dried after the adhering moisture was replaced with alcohol. Furthermore, these powders were charged into a rotary ball mill, filled with ethyl alcohol, and heated for 2 hours.
Pulverized for hr. The composition of the powder thus obtained is shown in Table 2. When some of these powders were subjected to X-ray analysis, test N
It was found that both samples 0 and 1.3 were composed of a single-phase SmCo1 intermetallic compound. However, test No. 13
.. 16 is 5111cO+ in addition to SmCo5 phase.
, phase was observed, and in test Nos. 15 and 17, in addition to the 5IIICos phase, 5IIIC03 phase and 5ffit
A COr phase was observed.

!IP&2表 以上のようにして用意した磁石粉末に対して、樹脂とし
てポリアミド樹脂(ナイロン6)を外削で8.5重量%
添加混練し、ベレット化した後、15KOeの磁場中で
射出成形した。得られた樹脂磁石の磁気的特性を測定し
た結果を第3表に示す。
! 8.5% by weight of polyamide resin (nylon 6) was added by external cutting to the magnet powder prepared as shown in the IP & 2 table above.
After addition, kneading, and pelletizing, injection molding was performed in a magnetic field of 15 KOe. Table 3 shows the results of measuring the magnetic properties of the obtained resin magnet.

比較例1 実施例1の試験No、1のSm*Os粉、Ca粉および
Ca粒を夫々137g、242g、70gの配合で混合
したこ′と、980℃で1時間保持した後、1150℃
に昇温しその温度で1時間保持し、次に850℃まで冷
却し、その温度で6時間保持して、常温まで冷却したこ
と以外は実施例1と全く同様に操作した。得られた磁石
粉末の組成と樹脂磁石の磁気的特性を第4表に示す。
Comparative Example 1 The Sm*Os powder, Ca powder, and Ca grains of Test No. 1 of Example 1 were mixed in a proportion of 137 g, 242 g, and 70 g, respectively, and after being held at 980°C for 1 hour, the mixture was heated to 1150°C.
It was operated in exactly the same manner as in Example 1 except that the temperature was raised to 850° C., held at that temperature for 1 hour, then cooled to 850° C., held at that temperature for 6 hours, and cooled to room temperature. Table 4 shows the composition of the obtained magnet powder and the magnetic properties of the resin magnet.

第  4  表 比較例2 実施例1の試験NO35の5l11203粉、Ca粒お
よびCa粒を夫々145g、243g172gの配合で
混合したこと以外は比較例1と全く同様に操作した。得
られた磁石粉末の組成と樹脂磁石の磁気的特性を第5表
に示す。
Table 4 Comparative Example 2 The procedure was exactly the same as in Comparative Example 1 except that 5l11203 powder of Test No. 35 of Example 1, Ca grains, and Ca grains were mixed in the proportions of 145 g, 243 g, and 172 g, respectively. Table 5 shows the composition of the obtained magnet powder and the magnetic properties of the resin magnet.

第  5  表 〔発明の効果〕 以上から明らかなように、本発明は、還元拡散法によっ
て、残留磁束密度、保磁力、最大エネルギー積の磁気的
特性の優れた樹脂磁石用に好適のSmCo5系磁石粉末
を、不純物量の限定されたサマリウム酸化物原料を使用
し、かつ該粉末中のサマリウムが限定された組成になる
ように配合することによって、熱処理を行なうことなく
製造するとかできるものである。この熱処理は特に主要
元素であるサマリウムの組成を変動させ易いものであり
、従って、樹脂磁石用に好適の5IIICO6系磁石粉
末を安定して簡便に製造することのできる本発明の工業
的意義は非常に大である。
Table 5 [Effects of the Invention] As is clear from the above, the present invention produces a SmCo5-based magnet suitable for resin magnets, which has excellent magnetic properties such as residual magnetic flux density, coercive force, and maximum energy product, using the reduction diffusion method. The powder can be manufactured without heat treatment by using samarium oxide raw materials with a limited amount of impurities and by blending the powder so that the samarium in the powder has a limited composition. This heat treatment is particularly likely to change the composition of samarium, which is a major element, and therefore the present invention, which can stably and easily produce 5III CO6 magnet powder suitable for resin magnets, has great industrial significance. It is large.

Claims (1)

【特許請求の範囲】[Claims] (1)サマリウム酸化物とコバルト粉末を配合した混合
物を加熱還元し生成したサマリウムを該コバルト粉末中
に拡散させた後、得られた反応生成物を水中に投入して
スラリー状にし、該スラリーを水および酸水溶液で処理
することによって磁石粉末を製造する方法において、前
記サマリウム酸化物は不純物としてランタン、セリウム
、プラセオジムおよびネオジムをいずれも1.3重量%
以下で、それらの合計が、1.7重量%以下含有するも
のを使用し、且つ前記磁石粉末中に含有されるサマリウ
ムが32.7〜33.4重量%になるように前記配合を
行なうことを特徴とする樹脂磁石用サマリウム−コバル
ト系磁石粉末の製造方法。
(1) After heating and reducing a mixture of samarium oxide and cobalt powder and diffusing the produced samarium into the cobalt powder, the resulting reaction product is poured into water to form a slurry. In a method for producing magnetic powder by treatment with water and an acid aqueous solution, the samarium oxide contains lanthanum, cerium, praseodymium, and neodymium in an amount of 1.3% by weight as impurities.
In the following, use materials whose total content is 1.7% by weight or less, and perform the blending so that samarium contained in the magnet powder is 32.7 to 33.4% by weight. A method for producing samarium-cobalt magnet powder for resin magnets, characterized by:
JP59235077A 1984-11-09 1984-11-09 Manufacture of samarium-cobalt magnet powder for resin magnet Pending JPS61114502A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP59235077A JPS61114502A (en) 1984-11-09 1984-11-09 Manufacture of samarium-cobalt magnet powder for resin magnet
US06/796,224 US4664723A (en) 1984-11-09 1985-11-08 Samarium-cobalt type magnet powder for resin magnet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59235077A JPS61114502A (en) 1984-11-09 1984-11-09 Manufacture of samarium-cobalt magnet powder for resin magnet

Publications (1)

Publication Number Publication Date
JPS61114502A true JPS61114502A (en) 1986-06-02

Family

ID=16980718

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59235077A Pending JPS61114502A (en) 1984-11-09 1984-11-09 Manufacture of samarium-cobalt magnet powder for resin magnet

Country Status (1)

Country Link
JP (1) JPS61114502A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5348020A (en) * 1976-10-04 1978-05-01 Bbc Brown Boveri & Cie Method of making plastically combined *ln co*magnets
JPS5415415A (en) * 1978-07-18 1979-02-05 Seiko Epson Corp Method of producing intermetallic compound magnet
JPS556478A (en) * 1978-06-29 1980-01-17 Seiko Epson Corp Production of intermetallic compound magnet
JPS5617003A (en) * 1979-06-20 1981-02-18 Tohoku Metal Ind Ltd Material for permanent magnet
JPS59179703A (en) * 1983-03-30 1984-10-12 Tdk Corp Manufacture of rare earth cobalt alloy powder having two-phase separation type coercive force producing mechanism

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5348020A (en) * 1976-10-04 1978-05-01 Bbc Brown Boveri & Cie Method of making plastically combined *ln co*magnets
JPS556478A (en) * 1978-06-29 1980-01-17 Seiko Epson Corp Production of intermetallic compound magnet
JPS5415415A (en) * 1978-07-18 1979-02-05 Seiko Epson Corp Method of producing intermetallic compound magnet
JPS5617003A (en) * 1979-06-20 1981-02-18 Tohoku Metal Ind Ltd Material for permanent magnet
JPS59179703A (en) * 1983-03-30 1984-10-12 Tdk Corp Manufacture of rare earth cobalt alloy powder having two-phase separation type coercive force producing mechanism

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