JPS6231056B2 - - Google Patents
Info
- Publication number
- JPS6231056B2 JPS6231056B2 JP54129667A JP12966779A JPS6231056B2 JP S6231056 B2 JPS6231056 B2 JP S6231056B2 JP 54129667 A JP54129667 A JP 54129667A JP 12966779 A JP12966779 A JP 12966779A JP S6231056 B2 JPS6231056 B2 JP S6231056B2
- Authority
- JP
- Japan
- Prior art keywords
- atm
- rare earth
- oersted
- elements
- sintering
- 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.)
- Expired
Links
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Description
【発明の詳細な説明】
本発明は希土類元素（Ｒと称する）とそれ以外
の元素の合金の粉末を成型し、焼結・焼鈍の熱処
理として製造する希土類磁石の製造方法に関する
ものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method of manufacturing a rare earth magnet, which involves molding powder of an alloy of a rare earth element (referred to as R) and other elements, and performing heat treatments such as sintering and annealing.
従来、希土類磁石（以後Ｒ・Ｍ磁石と称す。Ｍ
は希土類元素Ｒ以外の元素である。）は磁気特性
が優れるため小型、薄型機器に広く用いられつつ
ある。 Conventionally, rare earth magnets (hereinafter referred to as R/M magnets.M
is an element other than the rare earth element R. ) is becoming widely used in small and thin devices due to its excellent magnetic properties.
そして高い磁気特性を得るにはＲ・Ｍ合金粉末
を圧縮成形し高温で焼結し又場合によつてはその
後焼鈍等の熱処理をする必要がある。 In order to obtain high magnetic properties, it is necessary to compression mold the R/M alloy powder, sinter it at a high temperature, and, depending on the case, to perform heat treatment such as annealing afterwards.
しかしこれらの熱処理は高温700℃〜1300℃の
範囲で行なわれるためにＲ・Ｍ合金中の成形が蒸
発してしまい組成ずれ等が生じて磁気特性の劣化
がおきる欠点を有している。 However, since these heat treatments are carried out at high temperatures in the range of 700 DEG C. to 1300 DEG C., they have the disadvantage that the molding in the R.M alloy evaporates, causing compositional deviations and the like, resulting in deterioration of magnetic properties.
本発明は上記欠点等を改良し磁気特性の優れた
希土類磁石を可能とした製造方法を提供すること
を目的としたものである。 The object of the present invention is to provide a manufacturing method that improves the above-mentioned drawbacks and makes it possible to produce rare earth magnets with excellent magnetic properties.
Ｒ・Ｍ磁石は希土類元素Ｒ（Sc、Ｙ、La、
Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、
Ho、Er、Tm、Yb、Lu）とその他の元素Ｍは
Co、Fe、Cu、を主成分とする場合が多いが、そ
の他にも次の元素が加えられ磁気特性の向上に有
効である。たとえば遷移金属のTi、Zr、Hfや
、、、族元素、Mg、Ca、Ag、Zn、
Ｂ、Al、Ga、In、Ｃ、Si、Ge、Sn、Pb、Ｐ、
As、Sb、Bi、Ｓ、Te、Se、Po、Tl、等が有効で
ある。 R/M magnets are made of rare earth elements R (Sc, Y, La,
Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy,
Ho, Er, Tm, Yb, Lu) and other elements M are
Co, Fe, and Cu are often the main components, but the following elements are also added and are effective in improving magnetic properties. For example, the transition metals Ti, Zr, Hf, group elements Mg, Ca, Ag, Zn, etc.
B, Al, Ga, In, C, Si, Ge, Sn, Pb, P,
As, Sb, Bi, S, Te, Se, Po, Tl, etc. are valid.
これらの元素は秤量され溶解冷却によつて合金
インゴツトが製造され、その後粉砕されて粉末が
得られる。粉末は一般に単磁区粒子にするために
10μ以下である。この粉末は磁場中プレスで圧縮
成形され更に高密度にするために焼結をしその後
必要に応じて焼鈍等の熱処理工程を経て製造され
る。 These elements are weighed, melted and cooled to produce an alloy ingot, and then crushed to obtain powder. Powders are generally made into single domain particles.
It is 10μ or less. This powder is compression molded using a press in a magnetic field, sintered to further increase the density, and then subjected to a heat treatment process such as annealing if necessary.
しかしこのような熱処理は700℃〜1300℃の高
温で行われ又Ar、H2、N2等の大気圧雰囲気で行
われているために、どうしても蒸発しやすい元素
例えば希土類元素ＲやCu、Mg、Zn、In、Pb等が
蒸発し組成ずれが生ずるため磁気特性の劣化が生
じてしまう。 However, since such heat treatment is performed at high temperatures of 700°C to 1300°C and in an atmospheric pressure atmosphere such as Ar, H 2 , N 2 etc., elements that easily evaporate, such as rare earth elements R, Cu, Mg , Zn, In, Pb, etc. evaporate and a compositional shift occurs, resulting in deterioration of magnetic properties.
特に希土類元素は蒸発しやすくそのために磁気
特性の内部保磁力（Hcと称す。）の低下が大きく
優れた磁石を製造することが困難であつた。 In particular, rare earth elements tend to evaporate easily, which makes it difficult to manufacture excellent magnets with a large drop in internal coercive force (referred to as Hc), which is a magnetic characteristic.
このような困難を解決する方法として本発明で
は前記の熱処理工程において、Ar、N2、H2等の
ガス圧を高めることによつて、元素の蒸発を少な
くすることにより磁気特性、特にHcの低下を防
ぎ、優れた磁石を製造することが可能となつた。 In order to solve these difficulties, the present invention improves the magnetic properties, especially Hc, by increasing the gas pressure of Ar, N 2 , H 2, etc. in the heat treatment process to reduce the evaporation of elements. It has become possible to prevent this deterioration and manufacture excellent magnets.
次に本発明による磁石の製造方法について述べ
る。 Next, a method for manufacturing a magnet according to the present invention will be described.
まず希土類元素Ｒとその他の元素Ｍをはかりで
秤量し、真空後置換したAr等の不活性ガス中で
溶解した後金型に鋳造してＲ・Ｍの合金インゴツ
トを製造する。 First, the rare earth element R and other elements M are weighed on a scale, melted in an inert gas such as Ar which is substituted after vacuum, and then cast into a mold to produce an R/M alloy ingot.
場合によつては成分の偏析を均一化するために
このインゴツトを溶体化熱処理をする時がある。 In some cases, this ingot is subjected to solution heat treatment in order to homogenize the segregation of components.
次にインゴツトは不活性ガス中や真空中又は、
水分や不純物を含有しない有機溶媒中例えばトル
エン、アルコール、ダイフロン等にてスタンプミ
ルやクラツシヤー、ハンドミル、ジエツトミル、
振動ミル、ボールミル等の方法で粉砕する。この
粉末を磁場中成形又は単にプレス成形をする、更
に密度を高めるために、真空後Ar、Ne、He、Ne
等の不活性ガス又はN2ガス中で焼結をする。更
にその後焼鈍をし磁気特性を高める。 Next, the ingot is placed in an inert gas, vacuum, or
Stamp mill, crusher, hand mill, jet mill, etc. in an organic solvent containing no water or impurities, such as toluene, alcohol, Diflon,
Grind by vibration mill, ball mill, etc. This powder is molded in a magnetic field or simply press molded, and in order to further increase the density, Ar, Ne, He, Ne,
Sintering is carried out in an inert gas such as or N2 gas. Furthermore, it is then annealed to improve its magnetic properties.
しかしいずれも焼結あるいは焼鈍等の熱処理工
程が行なわれ、温度範囲は700℃〜1300℃であ
る。これより低くしても又高くしても磁気特性が
得られない。 However, both require a heat treatment process such as sintering or annealing, and the temperature range is 700°C to 1300°C. Even if it is lower or higher than this, magnetic properties cannot be obtained.
又この時ガスの圧力は大気圧より高くする程好
ましいが、３気圧以下では効果が少ない又100気
圧以上は装置上高価となり、工業上難かしい。そ
して我々も装置上100気圧以上での製造は出きな
かつた。 At this time, it is preferable to make the gas pressure higher than atmospheric pressure, but if it is less than 3 atm, the effect is small, and if it is more than 100 atm, the equipment becomes expensive and industrially difficult. We were also unable to manufacture the product at a pressure higher than 100 atmospheres due to our equipment.
以下実施例をあげて本発明の説明をする。 The present invention will be explained below with reference to Examples.
実施例 １
金属Sm（99.9％＞）を36重量％、金属Co
（99.9％＞）を64重量％を秤量し、これを真空引
き後Arガス置換した雰囲気中で高周波溶解し金
型に鋳造し合金インゴツトを製造した。これは
1200℃、Ar中で10時間溶体化処理を行なつた。Example 1 36% by weight of metal Sm (99.9%>), metal Co
(99.9%>) was weighed out, and after being evacuated, it was high-frequency melted in an atmosphere replaced with Ar gas and cast into a mold to produce an alloy ingot. this is
Solution treatment was performed at 1200°C in Ar for 10 hours.
このインゴツトはN2ガス中でクラツシヤーで
粉砕し、その後ステンレスポツト中で８mmφ鋼球
とダイフロン溶媒中で振動ミルで粉砕し約10μ以
下までの粒子とする。 This ingot is crushed with a crusher in N 2 gas, and then crushed with a vibration mill in a stainless steel pot using 8 mm diameter steel balls and Diflon solvent to obtain particles of about 10 μm or less.
この粉末は磁気プレス中で磁界約10000エルス
テツド、１〜5t／cm2で湿式プレス成形された。こ
の成形体は400℃で約1h保つことにより溶媒を取
り除ぞかれた。 This powder was wet pressed in a magnetic press with a magnetic field of about 10,000 oersted and 1 to 5 t/cm 2 . This molded body was kept at 400°C for about 1 hour to remove the solvent.
この成形体を真空後高圧ステンレスチヤンバー
内をAr雰囲気にし焼結・焼鈍の熱処理を行なつ
た。 After vacuuming, this compact was heat-treated by sintering and annealing in an Ar atmosphere in a high-pressure stainless steel chamber.
Arガス圧はほぼ大気圧（１気圧）、２気圧、３
気圧、10気圧、50気圧、100気圧で行ない、熱処
理は同一プログラムであり、1170℃×1h焼結後
室温近くまで急冷、その後830℃×3h焼鈍後室温
まで急冷をするパターンである。この結果、磁気
特性のHc（保磁力）は次の通りである。なお残
留磁束密度（Br）はいずれもほぼ同一で8700ガ
ウスである。 Ar gas pressure is approximately atmospheric pressure (1 atm), 2 atm, 3 atm.
The heat treatment was carried out at atmospheric pressure, 10 atmospheres, 50 atmospheres, and 100 atmospheres, and the heat treatment was performed using the same program: sintering at 1170°C for 1 hour, followed by rapid cooling to near room temperature, followed by annealing at 830°C for 3 hours, followed by rapid cooling to room temperature. As a result, the magnetic properties Hc (coercive force) are as follows. The residual magnetic flux density (Br) is almost the same in all cases, 8700 Gauss.
大気圧でHc＝14200エルステツド。 Hc = 14200 oersted at atmospheric pressure.
２気圧でHc＝14300エルステツド。 Hc = 14300 oersted at 2 atm.
３気圧でHc＝15800エルステツド。 Hc = 15800 oersted at 3 atm.
10気圧でHc＝20600エルステツド。 Hc = 20600 oersted at 10 atm.
50気圧でHc＝22700エルステツド。 Hc = 22700 oersted at 50 atm.
100気圧でHc＝25300エルステツド。 Hc = 25300 oersted at 100 atm.
以上のように３気圧以上で効果が出ており、特
に10気圧以上で大きな特性の向上がみられる。 As mentioned above, it is effective at temperatures above 3 atm, and particularly significant improvements in properties are seen at temperatures above 10 atm.
実施例 ２
Smを24重量％、Cuを10重量％、Feを15重量
％、Zrを２％、Ｖを0.2％、Nbを0.2％、Taを0.2
％、Ti、Cr、Mn、Niを各0.1％、残りをCo金属
とした、合金を実施例１と同様して合金インゴツ
トを作り、同様にして粉末を成形した。又ガス圧
等も同一の製造である。ただし熱処理プログラム
は次のようにした。1300℃×1h焼結更に1.250℃
×1h溶体化処理後室温まで急冷した。その後850
℃×1h焼鈍し更に700℃×1h焼鈍した後室温まで
急冷した。その結果を下に示す。なおBrはいず
れもほぼ11900ガウスである。Example 2 24% by weight of Sm, 10% by weight of Cu, 15% by weight of Fe, 2% of Zr, 0.2% of V, 0.2% of Nb, 0.2% of Ta
An alloy ingot was prepared in the same manner as in Example 1, with Ti, Cr, Mn, and Ni at 0.1% each and the remainder being Co metal, and powder was molded in the same manner. Also, gas pressure, etc. are manufactured in the same way. However, the heat treatment program was as follows. 1300℃×1h sintering and further 1.250℃
After solution treatment for ×1 h, the mixture was rapidly cooled to room temperature. then 850
℃×1h, further annealed at 700℃×1h, and then rapidly cooled to room temperature. The results are shown below. Note that Br is approximately 11,900 Gauss in both cases.
大気圧でHc＝5500エルステツド。 Hc = 5500 oersted at atmospheric pressure.
２気圧でHc＝5500エルステツド。 Hc = 5500 oersted at 2 atm.
３気圧でHc＝5800エルステツド。 Hc = 5800 oersted at 3 atm.
10気圧でHc＝6200エルステツド。 Hc = 6200 oersted at 10 atm.
50気圧でHc＝6700エルステツド。 Hc = 6700 oersted at 50 atm.
100気圧でHc＝7200エルステツド。 Hc = 7200 oersted at 100 atm.
以上の結果においても３気圧以上で効果が見ら
れ保磁力Hcの増大が得られる。 In the above results, the effect is seen at 3 atm or higher, and an increase in coercive force Hc can be obtained.
このように雰囲気ガスの圧力を高めることによ
つて蒸発が押えられ組成のずれが少ないため高い
磁気特性、特にHcが優れたものとなつた。 By increasing the pressure of the atmospheric gas in this way, evaporation is suppressed and there is little deviation in composition, resulting in high magnetic properties, especially excellent Hc.
Claims (1)
末を圧粉成型した後、高圧不活性ガス雰囲気中で
焼結・焼鈍の熱処理をすることを特徴とする希土
類磁石の製造方法。 ２ 高圧ガスの圧力が、３気圧から100気圧であ
る特許請求の範囲第１項記載の希土類磁石の製造
方法。 ３ 焼結・焼鈍の熱処理温度が700℃から1300℃
の範囲である特許請求の範囲第１項記載の希土類
磁石の製造方法。[Claims] 1. A method for producing a rare earth magnet, which comprises compacting powder of an alloy consisting of rare earth elements and other elements, and then subjecting the powder to sintering and annealing in a high-pressure inert gas atmosphere. . 2. The method for producing a rare earth magnet according to claim 1, wherein the pressure of the high pressure gas is from 3 atm to 100 atm. 3 Heat treatment temperature for sintering and annealing is 700℃ to 1300℃
A method for manufacturing a rare earth magnet according to claim 1, which is within the scope of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12966779A JPS5655533A (en) | 1979-10-08 | 1979-10-08 | Manufactre of rare earth element magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12966779A JPS5655533A (en) | 1979-10-08 | 1979-10-08 | Manufactre of rare earth element magnet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5655533A JPS5655533A (en) | 1981-05-16 |
| JPS6231056B2 true JPS6231056B2 (en) | 1987-07-06 |
Family
ID=15015163
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12966779A Granted JPS5655533A (en) | 1979-10-08 | 1979-10-08 | Manufactre of rare earth element magnet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5655533A (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6070102A (en) * | 1983-08-19 | 1985-04-20 | Tohoku Metal Ind Ltd | Atmosphere sintering method |
| JPS60131949A (en) * | 1983-12-19 | 1985-07-13 | Hitachi Metals Ltd | Iron-rare earth-nitrogen permanent magnet |
| JP5969750B2 (en) * | 2011-10-14 | 2016-08-17 | 日東電工株式会社 | Rare earth permanent magnet manufacturing method |
| JP5969781B2 (en) * | 2012-03-12 | 2016-08-17 | 日東電工株式会社 | Rare earth permanent magnet manufacturing method |
| JP5969782B2 (en) * | 2012-03-12 | 2016-08-17 | 日東電工株式会社 | Rare earth permanent magnet manufacturing method |
| JP5969783B2 (en) * | 2012-03-12 | 2016-08-17 | 日東電工株式会社 | Rare earth permanent magnet manufacturing method |
| CN105164765A (en) * | 2014-03-20 | 2015-12-16 | 株式会社东芝 | Permanent magnet, motor, and generator |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52103698A (en) * | 1976-02-27 | 1977-08-31 | Fujitsu Ltd | Preparing rare earth cobalt magnet |
| JPS5353514A (en) * | 1976-10-26 | 1978-05-16 | Fujitsu Ltd | Production of rare earth elemens cobalt magnet |
-
1979
- 1979-10-08 JP JP12966779A patent/JPS5655533A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52103698A (en) * | 1976-02-27 | 1977-08-31 | Fujitsu Ltd | Preparing rare earth cobalt magnet |
| JPS5353514A (en) * | 1976-10-26 | 1978-05-16 | Fujitsu Ltd | Production of rare earth elemens cobalt magnet |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5655533A (en) | 1981-05-16 |
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