JPS61214504A - Manufacture of sm-co magnet - Google Patents
Manufacture of sm-co magnetInfo
- Publication number
- JPS61214504A JPS61214504A JP60054656A JP5465685A JPS61214504A JP S61214504 A JPS61214504 A JP S61214504A JP 60054656 A JP60054656 A JP 60054656A JP 5465685 A JP5465685 A JP 5465685A JP S61214504 A JPS61214504 A JP S61214504A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- magnet
- retort
- grains
- sm2o3
- 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
- H01F1/0553—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 obtained by reduction or by hydrogen decrepitation or embrittlement
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
- C22C1/0441—Alloys based on intermetallic compounds of the type rare earth - Co, Ni
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は５ＩＩｌ−Ｃｏ磁石の製造に係り、より詳細に
は、Ｓｍ源として酸化物ＳｍｔＯ，を用いて加熱還元に
より低源にＳ ｍ −Ｇ ｏ磁石を製造する方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to the production of 5IIIl-Co magnets, and more specifically, the present invention relates to the production of 5IIIl-Co magnets, and more specifically, it uses an oxide SmtO as an Sm source to produce a low source of Sm − by thermal reduction. The present invention relates to a method of manufacturing a Go magnet.
（従来の技術及び問題点）
希土類−〇〇系磁石を代表例とする希土類磁石は、永久
磁石材料としての特性、特に最大エネルギー積（ＢＨ）
ｏ＋ａｘがアルニコ系磁石材料等に比べて著しく高いも
のがあり、家庭電気製品、音響製品、時計部品、自動車
部品、精密機器などの小型軽量化及び高性能化に大きく
貢献している。(Prior art and problems) Rare earth magnets, of which rare earth magnets are a typical example, have poor characteristics as permanent magnet materials, especially maximum energy product (BH).
There are some materials whose o+ax is significantly higher than that of alnico magnet materials, etc., and they greatly contribute to the miniaturization, weight reduction, and high performance of home appliances, audio products, watch parts, automobile parts, precision instruments, etc.
就中、希土類元素を５Ｉ１１とするＳ ｍ −Ｃｏ系磁
石としては、Ｓｎ＋Ｍ、系、Ｓｍ２Ｊ７系（Ｍ：Ｃｏ又
はＣ。In particular, examples of S m -Co based magnets in which the rare earth element is 5I11 include Sn+M, Sm2J7 based (M: Co or C).
の一部をＦｅ、Ｃｕ、Ｚｒ等々で置換した金属元素）な
どがあり、磁気特性が格段に優れているが、高価なＣｏ
を多量に含む上に資源的に余り多くないＳｍを利用する
ため、コストが高いという問題がある。Some metal elements such as Fe, Cu, Zr, etc. have been substituted for a portion of Co, and have extremely excellent magnetic properties, but they are expensive.
Since it contains a large amount of Sm and uses Sm, which is not very abundant in terms of resources, there is a problem of high cost.
一方、Ｓｍ−Ｇｏ系磁石の製造に当っては、従来、Ｇｏ
などの金属Ｍを溶解して金属粉を製造し、他方、５ＩＩ
ｌ源も金属Ｓｍを用いて、これらを誘導炉で溶解して塊
状となし、粉砕してＳｍ−Ｇｏ系合金粉を得て磁場中成
形、焼結等々の所望の熱処理により製品としていた。し
かし、この方法では、原材料として高価な金属ＳＩＩ＋
粉を使用するため、上記の問題に加えて製造コストも高
くなるという欠点があった。On the other hand, in the production of Sm-Go magnets, Go
Metal powder is produced by melting metal M such as 5II.
The metal Sm was also used as a source, melted in an induction furnace to form a lump, crushed to obtain Sm-Go alloy powder, and processed into a product by desired heat treatment such as compaction in a magnetic field, sintering, etc. However, this method uses expensive metal SII+ as a raw material.
Since powder is used, in addition to the above-mentioned problems, the manufacturing cost is also high.
（発明の目的）
本発明は、前述のＳｍ−Ｃｏ系磁石の製造に関する欠点
を解消し、Ｓｍ−Ｃｏ磁石を低源、かつ、効率的に製造
することができる方法を提供することを目的とするもの
である。(Objective of the Invention) An object of the present invention is to eliminate the above-mentioned drawbacks regarding the production of Sm-Co magnets, and to provide a method that can produce Sm-Co magnets efficiently and with low cost. It is something to do.
（発明の構成）
上記目的を達成するため、本発明では、５ＩＩｌ源とし
て高価な金属Ｓｍ粉に代えて安価な酸化物Ｓｍ、○、粉
を使用し、これに金属Ｇｏ粉と特定粒径のＣａ粒とを加
えてレトルト内で特定条件下で加熱還元して５ｅａ−Ｇ
ｏ合金粉を得ることを骨子とするものである。(Structure of the Invention) In order to achieve the above object, in the present invention, an inexpensive oxide Sm powder with a specific particle size is used as a 5IIl source in place of an expensive metal Sm powder, and a metal Go powder with a specific particle size is used. Add Ca grains and reduce by heating under specific conditions in a retort to obtain 5ea-G.
The main point is to obtain o-alloy powder.
以下に本発明を実施例に基づいて詳細に説明する。The present invention will be explained in detail below based on examples.
本発明における原材料としては、Ｓｍ−Ｃｏ磁石を構成
する一成分であるＳｍについては、安価な酸化物Ｓ＋ｏ
２０．粉を用い、ＧｏについてはＣｏ金属粉を用い、更
に５Ｌ１１２０．粉の還元剤として０．５〜１０＋ｏｍ
粒径のＣａ粒を用いる。As raw materials in the present invention, Sm, which is one of the components constituting the Sm-Co magnet, is an inexpensive oxide S+o
20. Co powder was used for Go, and Co metal powder was used for Go, and 5L1120. 0.5-10+om as a powder reducing agent
Ca grains with the same particle size are used.
Ｓｍ、Ｏ，粉としては市販のものでよく、またＧｏ粉は
、遠心噴霧法、アトマイズ法などで粉末化したもの、或
いは溶解凝固後にボールミルやジェットミルなどで機械
的に破砕して粉末化したものを用いることができる。Commercially available Sm, O, and powders may be used, and the Go powder may be powdered by centrifugal spraying, atomization, etc., or powdered by mechanically crushing with a ball mill, jet mill, etc. after melting and solidification. can be used.
Ｃａ粒は還先剤として用いるが、還元効率の向上を期す
るために粒径０．５〜１０ｍｍのものを使用する必要が
あるＳＣａは非常に活性であるので。Ca particles are used as a reducing agent, but in order to improve the reduction efficiency, it is necessary to use particles with a particle size of 0.5 to 10 mm because SCa is very active.
粒径が０．５ｍｍ未満の細粒であると、第１図に示すよ
うに、混合処理してレトルト内に装入するまでのハンド
リング期間中に酸化してＣａＯになる割合が多くなり、
添加量に比べて還元効率が悪化し、還元後の後処理（水
洗、乾燥等）が煩雑になる。If the particle size is less than 0.5 mm, as shown in Figure 1, the proportion of oxidation to CaO increases during the handling period from mixing to charging into the retort.
Reduction efficiency deteriorates compared to the amount added, and post-treatment after reduction (washing, drying, etc.) becomes complicated.
また粒径がｉｏａｍを超えて大きすぎると、第２図に示
すように、処理時間の延長を余儀なくされ、反応効率が
低下する。なお、還元に必要なＣａ量は理論値の約１．
２〜１．５倍とするのが好ましい。Moreover, if the particle size is too large, exceeding ioam, as shown in FIG. 2, the treatment time will have to be extended and the reaction efficiency will decrease. Note that the amount of Ca required for reduction is approximately 1.0% of the theoretical value.
It is preferable to set it as 2 to 1.5 times.
上記のＳ＋ｏ２０．粉、Ｇｏ粉及びＣａ粒を所定量混合
したものをレトルト内で加熱還元する。その除用いる反
応装置の一例を第３図に示す、同図中、１がステンレス
鋼製のレトルトでシリコユニット炉２中に載置されてい
る。レトルト１内には上記混合粉粒を収容する鉄製容器
βを置き、この鉄製容器３の底部には焼付防止用のＣａ
Ｏ粉末４を充填しておく。レトルト１の上端鍔部には上
蓋５との間に水冷用ジャケット６を設け、上蓋４にはＡ
ｒガス通気用及びロータリー真空ポンプ接続用配管が設
けられている。なお、７は熱電対である。S+o20 above. A mixture of a predetermined amount of powder, Go powder, and Ca particles is heated and reduced in a retort. An example of a reaction apparatus used for this purpose is shown in FIG. 3, in which numeral 1 is a stainless steel retort placed in a silico unit furnace 2. Inside the retort 1, there is placed an iron container β containing the mixed powder particles, and at the bottom of this iron container 3 there is a Ca
Fill with O powder 4. A water cooling jacket 6 is provided between the upper end flange of the retort 1 and the upper lid 5.
Piping for gas ventilation and connection to a rotary vacuum pump is provided. Note that 7 is a thermocouple.
レトルト内での反応条件は、Ａｒガス雰囲気下にて還元
温度を１０００”Ｃ以上とする。還元温度は使用するＣ
ａ粒の粒径と処理時間とから還元効率を考慮して決める
が、１０００’Ｃ未満では処理時間を長くし、しかも還
元効率の悪いより細粒のＣａ粒を使用しなければならな
くなる。１２００’ＣＸ２ｈｒの還元温度１時間を一応
の目安とすることが好ましい。The reaction conditions in the retort are an Ar gas atmosphere and a reduction temperature of 1000"C or higher.The reduction temperature is the C used.
It is determined by considering the reduction efficiency based on the particle size of the a grains and the treatment time, but if it is less than 1000'C, the treatment time will be longer and finer Ca grains with poor reduction efficiency will have to be used. It is preferable to use a reduction temperature of 1 hour at 1200'CX2hr as a tentative guideline.
還元後は、必要に応じて水洗、乾燥の後処理を行い、Ｃ
ａＯを除去しＳｍ−Ｇｏ粉を回収する。その際、水洗後
、酢酸を添加して中和し、再び水洗してアルコール洗浄
を行った後、真空乾燥するのが望ましい。After reduction, perform post-treatments such as washing with water and drying as necessary.
Remove aO and collect Sm-Go powder. At that time, it is desirable to wash with water, neutralize by adding acetic acid, wash with water again, wash with alcohol, and then vacuum dry.
得られたＳｍ−Ｇｏ粉は、常法により磁場中成形、焼結
・溶体化処理１時効処理等を行い、Ｓｍ−Ｃ。The obtained Sm-Go powder is subjected to molding in a magnetic field, sintering/solution treatment, 1 aging treatment, etc. in a conventional manner to form Sm-C.
磁石にする。Make it a magnet.
（実施例）
ＳｍＣｏ、磁石を製造するために、原材料として５０％
平均粒径１μｍのＳｍ、Ｏ，粉３５０ｇ、−２００メツ
シュ（−７４μｍ）のＣＯ粉５９０ｇ（いずれも目標値
に対して１００％歩留配合）、還元剤として５ＩＩＩＩ
１１粒径の金属Ｃａ粒ｘ５１ｇ（還元に必要な理論量の
１．２５倍）を混合し、第３図に示した反応装置のレト
ルト内に装填した０次いでガス置換後、Ａｒガスを５ｆ
ｆｉ／ｗｉｎで通気しつ＞１２００”ＣＸ２ｈｒの加熱
還元を行った。(Example) SmCo, 50% as raw material to produce magnets
350 g of Sm, O, powder with an average particle size of 1 μm, 590 g of CO powder with -200 mesh (-74 μm) (all with a yield of 100% relative to the target value), 5III as a reducing agent
51 g of metallic Ca particles (1.25 times the theoretical amount required for reduction) of 11 particle size were mixed and loaded into the retort of the reactor shown in Fig. 3. After gas replacement, 5 f of Ar gas was added.
Thermal reduction was carried out for >1200"CX2hr while aerating with fi/win.
反応処理後、レトルトから取り出して水洗（４Ω×１０
回）→酢酸による中和（ｐＨ＝２．５．２回）→水洗（
４Ｑ Ｘ ２回）→アルコール洗浄（２回）→真空乾燥
を経てＳ ｖａ −Ｇ ｏ粉を回収した。After reaction treatment, remove from retort and wash with water (4Ω x 10
times) → Neutralization with acetic acid (pH = 2.5.2 times) → Washing with water (
S va -G o powder was collected through 4Q x 2 times) → alcohol washing (2 times) → vacuum drying.
このＳｍ−Ｇｏ粉を微粉砕機磁場中成形し、焼結・溶体
化処理、時効処理等を施して５ＩＩＩＣＯ７磁石を得た
。ＳｍＣｏ、磁石の分析値及び磁気特性を第１表に示す
。This Sm-Go powder was molded in a magnetic field using a pulverizer, and subjected to sintering, solution treatment, aging treatment, etc. to obtain a 5IIICO7 magnet. Table 1 shows the analytical values and magnetic properties of SmCo and the magnet.
同表より、還元時の部位により化学成分が若干異なるが
、歩留及び磁気特性とも良好であった。From the same table, although the chemical components differed slightly depending on the site at the time of reduction, both the yield and magnetic properties were good.
（発明の効果）
以上説明したように１本発明によれば、Ｓ＋ｏ −Ｇｏ
磁石の製造に際し、５ＩＩｌ源として安価な酸化物Ｓｍ
、Ｏ，粉を使用するので製造コストを低コスト化でき、
また還元剤として特定粒径サイズのＣａ粒を用いるので
還元効率を向上することができ、良好な歩留の下でＳ
ｍ −Ｇ ｏ磁石を低置に製造することができる。した
がって、Ｓｍ−Ｇｏ系磁石を利用する各種分野での小型
軽量化及び高性能化に加えて低コスト化にも貢献する等
、その実用上の効果は顕著である。(Effect of the invention) As explained above, according to the present invention, S+o -Go
When manufacturing magnets, inexpensive oxide Sm is used as a 5IIIl source.
By using , O, powder, manufacturing costs can be reduced,
In addition, since Ca grains with a specific particle size are used as the reducing agent, the reduction efficiency can be improved, and S
m-G o magnets can be manufactured at low elevations. Therefore, its practical effects are significant, such as contributing to reductions in size, weight, performance, and cost reduction in various fields that use Sm-Go magnets.
第１図及び第２図は還元剤Ｃａの粒径と還元に必要なＣ
ａ量或いは処理時間との関係を示す図。
第３図は本発明の実施に用いる反応装置の一例を示す図
である。
１・・・レトルト、 ２・・・シリコユニット炉、
３・・・鉄製容器、 ４・・・Ｃａ量粉、５・・・上
蓋、 ６・・・水冷ジャケット。
７・・・熱電対。
特許出願人 大同特殊鋼株式会社代理人弁理士
中 村 尚
第１図
Ｃａｆｌ様（＾−
Ｃユ律１ｔイ（辷（訓電−１ン
第３図
ｒFigures 1 and 2 show the particle size of the reducing agent Ca and the amount of C required for reduction.
FIG. 3 is a diagram showing the relationship between the amount of a and the processing time. FIG. 3 is a diagram showing an example of a reaction apparatus used for carrying out the present invention. 1... Retort, 2... Silico unit furnace,
3... Iron container, 4... Ca amount powder, 5... Upper lid, 6... Water cooling jacket. 7...Thermocouple. Patent Applicant Daido Steel Co., Ltd. Representative Patent Attorney Takashi Nakamura
Claims (1)
入れ、加熱還元によりＳｍ−Ｃｏ合金粉を得て、Ｓｍ−
Ｃｏ磁石を製造するに際し、前記Ｃａ粒として０．５〜
１０ｍｍ粒径のものを用い、かつ、アルゴンガス雰囲気
下で還元温度を１０００℃以上とすることを特徴とする
Ｓｍ−Ｃｏ磁石の製造方法。Sm_2O_3 powder and Co powder are put into a retort together with Ca grains, and Sm-Co alloy powder is obtained by heat reduction.
When producing a Co magnet, the Ca grains are 0.5 to
A method for manufacturing an Sm-Co magnet, characterized in that a magnet having a particle size of 10 mm is used and the reduction temperature is set to 1000° C. or higher in an argon gas atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60054656A JPS61214504A (en) | 1985-03-20 | 1985-03-20 | Manufacture of sm-co magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60054656A JPS61214504A (en) | 1985-03-20 | 1985-03-20 | Manufacture of sm-co magnet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS61214504A true JPS61214504A (en) | 1986-09-24 |
Family
ID=12976825
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60054656A Pending JPS61214504A (en) | 1985-03-20 | 1985-03-20 | Manufacture of sm-co magnet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61214504A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010070777A (en) * | 2008-09-16 | 2010-04-02 | Sumitomo Metal Mining Co Ltd | Method for producing rare-earth-iron-nitrogen based alloy powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS497297A (en) * | 1972-04-07 | 1974-01-22 | ||
| 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 |
-
1985
- 1985-03-20 JP JP60054656A patent/JPS61214504A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS497297A (en) * | 1972-04-07 | 1974-01-22 | ||
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010070777A (en) * | 2008-09-16 | 2010-04-02 | Sumitomo Metal Mining Co Ltd | Method for producing rare-earth-iron-nitrogen based alloy powder |
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