JPS60173804A - Manufacture of rare earth cobalt magnet - Google Patents

Manufacture of rare earth cobalt magnet

Info

Publication number
JPS60173804A
JPS60173804A JP59029407A JP2940784A JPS60173804A JP S60173804 A JPS60173804 A JP S60173804A JP 59029407 A JP59029407 A JP 59029407A JP 2940784 A JP2940784 A JP 2940784A JP S60173804 A JPS60173804 A JP S60173804A
Authority
JP
Japan
Prior art keywords
mixing
rare earth
magnet
lubricant
earth cobalt
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
JP59029407A
Other languages
Japanese (ja)
Inventor
Hiromichi Sakojiri
弘通 迫尻
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.)
Seiko Instruments Inc
Original Assignee
Seiko Instruments Inc
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 Seiko Instruments Inc filed Critical Seiko Instruments Inc
Priority to JP59029407A priority Critical patent/JPS60173804A/en
Publication of JPS60173804A publication Critical patent/JPS60173804A/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
    • H01F1/0557Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered

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

PURPOSE:To improve internal defects and magnetic characteristics by using ball mill mixing in the method of mixing lubricant. CONSTITUTION:In the case of mixing lubricant in minute powder of rare earth cobalt alloy, ball mill mixing is used in the method of mixing. In this method, a solvent of hydrocarbon chloride fluoride which does not dissolve lubricant can be used. The hydrocarbon chloride fluoride is not so harmful against a human body and not so dangerous against ignition and due to minute and uniform dispersion in minute powder of magnet, the magnetic field orientation at the time of magnetic field forming is improved and a magnet is sintered in high density wherein almost no internal defect is found in the magnet after sintering so the magnetic characteristics can be improved.

Description

【発明の詳細な説明】 本発明は、希土類コバルト磁石の製造方法に関し、特に
、潤滑剤の混合方法を改良して磁久特性・ を高めた希
土類コバルト磁石の製造方法に1714するものである
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing rare earth cobalt magnets, and in particular, to a method for manufacturing rare earth cobalt magnets with improved magnetic properties by improving a lubricant mixing method.

一般に、希土類コバルト磁石は、磁石の粉末を磁場中で
加圧成形後焼結して永久磁石化さする。
Generally, rare earth cobalt magnets are made into permanent magnets by press-molding magnet powder in a magnetic field and then sintering it.

この様な磁場成形法には、アルコール、トルエンtヘキ
サン、塩化フッ化炭化水素などの有機溶剤と磁石微粉末
の混合物を磁場中で成形する湿式成形法と、乾燥した磁
石微粉末を磁場中で成形する乾式成形法がある。
Such magnetic field molding methods include a wet molding method in which a mixture of organic solvents such as alcohol, toluene t-hexane, and chlorofluorohydrocarbons and fine magnet powder are molded in a magnetic field, and a wet molding method in which a mixture of fine magnet powder and dried magnet powder is molded in a magnetic field. There is a dry molding method for molding.

乾式成形法は、湿式成形法に比べ成形時間が短かく、枚
雑形状、小屋形状の成形に適しているなどの長所を有し
ている反面、礎石微粉末の磁場配向が阻害さ2’Lやす
く、酸化しやすい為、磁気特性が低下するという欠点が
ある。これを改善する為に、固形パラフィン、ステアリ
ン酸、ヌテ了す/酸亜鉛などの潤滑剤を混合して磁石微
粉末間の摩擦を小さくし磁場配向性を良くするなどの試
みがなさnている。従来、潤滑剤の混合方法は万能混合
機などでアルコール、トルエン、ヘキサンナトの溶剤と
ともに混合さnているにすぎず、混合方法に特に注意が
払わnていなかった。この様な従来の混合方法では微量
な潤滑剤が均一に混合さ扛ず、焼結後の磁石の内部には
潤滑剤のかたまジが蒸発した跡である内部欠陥(ボアク
が多数みられ、また、蒸気特性も大きな向上はみられな
かった本発明は、上記の入点を解決するものであり、内
部欠陥(ボア)を改善するとともに磁気特性を大きく向
上させた希土類コバル) 11石の製造方法を千1供す
るものである◇ 本発明の方法は、希土類コバルト合金微粉末に潤滑剤を
混合する場合、その混合方法としてボールミル混合を用
いるものである。この方法によ牡ば、従来の混合方法で
は潤滑剤を溶解するアルコール、トルエン、ヘキサンな
どの溶剤しか使用できないのに対し、潤滑剤を溶解しな
い商品名ダイフロ/として代表さnる塩化フッ化炭化水
素の溶剤も使用できる。この塩化フッ化炭化水素は人体
の有害性、発火の危険性の少ない溶剤であジ工業的に有
利である。また、礎石微粉末中に微細に均一に分散さn
る為、磁場成形時の磁場配向性はさらに改善さn1焼結
後の磁石の内部には内部欠陥(ボア〕がほとんどみらf
Lない高い密度に焼結される為、磁気特性は大きな向上
がばから牡る。
Dry molding has advantages such as shorter molding time than wet molding and is suitable for molding irregular shapes and shed shapes, but on the other hand, the magnetic field orientation of fine foundation stone powder is inhibited. It has the disadvantage that magnetic properties deteriorate because it is easily oxidized. In order to improve this, attempts have been made to mix lubricants such as solid paraffin, stearic acid, and zinc acid to reduce the friction between the fine magnet powder and improve the magnetic field orientation. . Conventionally, lubricants have only been mixed with solvents such as alcohol, toluene, and hexanat using a universal mixer, and no particular attention has been paid to the mixing method. In this conventional mixing method, the small amount of lubricant is not mixed uniformly, and the inside of the magnet after sintering has many internal defects (bores), which are traces of evaporation of lubricant lumps, and The present invention solves the above-mentioned problems, and is a method for producing rare earth (cobal) 11 stone, which improves internal defects (bores) and greatly improves magnetic properties. ◇ In the method of the present invention, when a lubricant is mixed into rare earth cobalt alloy fine powder, ball mill mixing is used as the mixing method. With this method, conventional mixing methods can only use solvents such as alcohol, toluene, and hexane that dissolve lubricants, whereas chlorofluorocarbons, represented by the trade name Dyflo/, which do not dissolve lubricants, are used. Hydrogen solvents can also be used. The chlorofluorinated hydrocarbons are industrially advantageous because they are solvents that are less harmful to the human body and have less risk of ignition. In addition, it is finely and uniformly dispersed in the foundation stone fine powder.
As a result, the magnetic field orientation during magnetic field forming is further improved.There are almost no internal defects (bores) inside the magnet after n1 sintering.
Since it is sintered to a very high density, the magnetic properties will be greatly improved.

以下、本発明の実施例を詳細に説明する。Examples of the present invention will be described in detail below.

(実施例1) S m C(1g 合金(Sm36.5重量%、a06
3.5重量%〕を振動ミルにより湿式粉砕して約3μに
微粉末化した。この微粉末と、潤滑剤としてステアリン
酸0.1iii%をヘキサンに溶解した溶液をボールミ
ルで混合した後乾燥した。この粉末にヘキサンを加え造
粒し乾燥した。次にこの粉末を10KOgの砧界中で磁
場と平行方向に2 tonZ−の圧力で加圧し、直径1
0閾φ、厚さ12+mの成形体を作成した。この成形体
を真空中400℃で脱ガス処理してステアリン酸を蒸発
させた後、アルゴンで雰囲気中1100℃で焼結し、徐
冷後850℃で熱処理してアルゴン吹付冷却により急冷
した。
(Example 1) S m C (1 g Alloy (Sm36.5% by weight, a06
3.5% by weight] was wet-pulverized using a vibration mill to form a fine powder of about 3 μm. This fine powder and a solution of 0.1% stearic acid dissolved in hexane as a lubricant were mixed in a ball mill and then dried. Hexane was added to this powder, which was then granulated and dried. Next, this powder was pressurized in a 10 KOg field in a direction parallel to the magnetic field at a pressure of 2 ton Z-, and a diameter of 1
A molded body with a threshold φ of 0 and a thickness of 12+m was created. This compact was degassed at 400° C. in vacuum to evaporate stearic acid, then sintered at 1100° C. in an argon atmosphere, slowly cooled, heat treated at 850° C., and rapidly cooled by argon spray cooling.

第1表に本発明方法の山気特性の結果を示し、比較の為
、本発明と同一条件で作成し念従来の万能混合機による
混合方法の磁気特性を示す。
Table 1 shows the results of the magnetic properties of the method of the present invention, and for comparison, shows the magnetic properties of a mixing method using a conventional universal mixer prepared under the same conditions as the present invention.

第 工 宍 第1表から明らかな様に、本発明方法によnは従来方法
よりも大幅な磁気特性の改善がなさnた、また、磁石の
内部欠陥〔ボア〕も従来方法のものには多数みらtLる
が本発明方法のものはほとんどみらCず、本発明方法は
内部欠陥(ポア〕の改善にも大きく寄与している。
As is clear from Table 1, the method of the present invention did not significantly improve the magnetic properties compared to the conventional method, and the internal defects (bore) of the magnet were also lower than those of the conventional method. Although there are many examples, the method of the present invention is hardly found, and the method of the present invention greatly contributes to the improvement of internal defects (pores).

(実施例2) 実施例1では混合溶剤としてステアリン酸を溶解するヘ
キサンを使用したが、この溶剤は人体に有害で発火の危
険性がある為、取扱いには注意が必要で作条性、生産性
が悪くなる。そこで、実施例1と同様の方法で製造した
S’MO8ll微粉末に溶剤として人体への有害性、発
火の危険性の少ないダイフロンに代表さnる塩化フッ化
炭化水素を用いてステアリン酸をボールミル混合し、こ
の添加量を変えて作成し、実施例1と同様の方法で成形
、焼結した。
(Example 2) In Example 1, hexane, which dissolves stearic acid, was used as a mixed solvent, but since this solvent is harmful to the human body and has the risk of ignition, care must be taken when handling it. Sexuality becomes worse. Therefore, we added stearic acid to the S'MO8ll fine powder produced in the same manner as in Example 1 using a chlorinated fluorohydrocarbon such as Diflon, which is less harmful to the human body and has less risk of ignition, as a solvent. They were mixed, prepared by changing the amount added, and molded and sintered in the same manner as in Example 1.

第2表に本発明方法のa気特性の結果を示し、比較の為
、本発明と同一条件で作成した従来の万能混廿機による
混合方法の磁気特性を示す。
Table 2 shows the results of the a-air characteristics of the method of the present invention, and for comparison, shows the magnetic characteristics of a conventional mixing method using a universal mixer prepared under the same conditions as the present invention.

第 2 弄 第2表から明らかな様に、本発明方法によnばヌテ了リ
ン酸添加量が0.03重量−の微量添加であってもヌテ
アリン酸添刀口量0.1重量%の従来方法に比較して大
きな磁気特性の向上が得ら牡ることがわかる。また、ス
テアリン酸の混合溶剤として人体への有害性、%火の危
険性などの少ない塩化フッ化炭化水垢を用いても山気特
性の大幅な向上、内部欠陥の改善がはからnることから
′、本発明方法は実用上きわめて有益な方法といえる(
実施例3) SmOoxy付金(Sm合金、25重量%、Fgl5.
0重fi%、0w8.0重fa%、Zrl 、77重量
係、残りC6)をジェットミルにより約3μに微扮砕し
た。
As is clear from Table 2, according to the method of the present invention, even if the amount of nutary phosphoric acid added is as small as 0.03% by weight, compared to the conventional method where the amount of added nutarylic acid is 0.1% by weight. It can be seen that a large improvement in magnetic properties was obtained compared to the method. In addition, even if chlorinated fluoride carbonized water scale is used as a mixed solvent for stearic acid, which is less harmful to the human body and has less fire hazard, it is possible to significantly improve the mountain properties and improve internal defects. ′, the method of the present invention can be said to be extremely useful in practice (
Example 3) SmOoxy metal fitting (Sm alloy, 25% by weight, Fgl5.
0 weight fi%, 0w 8.0 weight fa%, Zrl, 77 weight ratio, remaining C6) was finely ground to about 3μ by a jet mill.

この微粉末と、潤滑剤としてステアリン酸0゜1重面係
を塩化フッ化炭化水素に分散した溶液をボールミルで混
合した。こjLを磁場中で湿式成形し、アルゴン雰囲気
で焼結して熱処理を行なった。
This fine powder was mixed in a ball mill with a solution of stearic acid 0°1 as a lubricant dispersed in chlorofluorocarbon. This jL was wet-molded in a magnetic field, sintered in an argon atmosphere, and heat-treated.

第3表に本発明方法の磁気特性を示し、比較の為に本発
明と同一条件で作成したヌテアリン酸無添カロの従来方
法の磁気特性を示す。
Table 3 shows the magnetic properties of the method of the present invention, and for comparison, shows the magnetic properties of the conventional method of Calo without the addition of nutearic acid, which was prepared under the same conditions as the present invention.

第 3 表 第3表から分かる様に、本発明の湿式成形法に」?いて
もステアリン酸のボールミル混合効果がよくみらn1従
来の湿式成形法に比べ大きな磁侃特以上各実施例で説明
した様に、本発明方法は、1−5系希土類コバルト磁石
、2−17系希土類コバルト磁石に適用し得ることは勿
論のこと、乾式成形法だけでなく湿式成形法に適用して
も十分な効果が得られることが分かる。
Table 3 As can be seen from Table 3, the wet molding method of the present invention "?" The ball mill mixing effect of stearic acid is good even when the stearic acid is mixed with n1. As explained in each example, the method of the present invention has a large magnetic characteristic compared to the conventional wet molding method. It can be seen that not only can the present invention be applied to rare earth cobalt magnets, but also sufficient effects can be obtained when applied not only to dry molding methods but also to wet molding methods.

以上 出願人 セイコー電子工業株式会社that's all Applicant: Seiko Electronics Industries Co., Ltd.

Claims (1)

【特許請求の範囲】[Claims] 希土類コバルト付合微粉末に、成形時の摩擦を軽減させ
る為、絹滑剤を0〜0.1重景襲(0を含まず)混付し
、磁場中で加圧成形後焼結する希土類コバルト磁石の製
造方法において、潤滑剤の混合方法がボールミル混性で
ちることを特徴とする希土類コバルト磁石の製造方法。
Rare earth cobalt is mixed with rare earth cobalt fine powder, mixed with 0 to 0.1 silk lubricant (not including 0) to reduce friction during molding, and sintered after pressure molding in a magnetic field. A method for producing a rare earth cobalt magnet, characterized in that the lubricant is mixed by ball milling.
JP59029407A 1984-02-17 1984-02-17 Manufacture of rare earth cobalt magnet Pending JPS60173804A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59029407A JPS60173804A (en) 1984-02-17 1984-02-17 Manufacture of rare earth cobalt magnet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59029407A JPS60173804A (en) 1984-02-17 1984-02-17 Manufacture of rare earth cobalt magnet

Publications (1)

Publication Number Publication Date
JPS60173804A true JPS60173804A (en) 1985-09-07

Family

ID=12275276

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59029407A Pending JPS60173804A (en) 1984-02-17 1984-02-17 Manufacture of rare earth cobalt magnet

Country Status (1)

Country Link
JP (1) JPS60173804A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6297311A (en) * 1985-10-24 1987-05-06 Seiko Epson Corp Manufacture of permanent magnet
FR2707192A1 (en) * 1993-07-08 1995-01-13 Aimants Ugimag Sa Process for the preparation of fluorine-containing cobalt rare earth type magnetic powders and corresponding densified permanent magnets

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5024799A (en) * 1973-07-04 1975-03-17
JPS5719030A (en) * 1980-07-08 1982-02-01 Mitsubishi Metal Corp Improvement in method and apparatus for fluidized bed reaction

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5024799A (en) * 1973-07-04 1975-03-17
JPS5719030A (en) * 1980-07-08 1982-02-01 Mitsubishi Metal Corp Improvement in method and apparatus for fluidized bed reaction

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6297311A (en) * 1985-10-24 1987-05-06 Seiko Epson Corp Manufacture of permanent magnet
FR2707192A1 (en) * 1993-07-08 1995-01-13 Aimants Ugimag Sa Process for the preparation of fluorine-containing cobalt rare earth type magnetic powders and corresponding densified permanent magnets
WO1995002252A1 (en) * 1993-07-08 1995-01-19 Ugimag S.A. Process for the preparation of cobalt/rare earth type magnetic powders containing fluorine and corresponding densified permanent magnets
EP0707739A1 (en) * 1993-07-08 1996-04-24 Ugimag Sa Process for the preparation of cobalt/rare earth type magnetic powders containing fluorine and corresponding densified permanent magnets

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