JPH0620007B2 - Permanent magnet manufacturing method - Google Patents
Permanent magnet manufacturing methodInfo
- Publication number
- JPH0620007B2 JPH0620007B2 JP62269115A JP26911587A JPH0620007B2 JP H0620007 B2 JPH0620007 B2 JP H0620007B2 JP 62269115 A JP62269115 A JP 62269115A JP 26911587 A JP26911587 A JP 26911587A JP H0620007 B2 JPH0620007 B2 JP H0620007B2
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- Prior art keywords
- weight
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- content
- max
- stage aging
- Prior art date
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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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は希土類元素の遷移金属を主成分とするＲ２Ｍ17
系（但しＲはイットリウムを含む希土類元素，Ｍは遷移
金属を表す）永久磁石の製造方法に関し、更に詳しくは
それに銅とジルコニウムと酸素を適量添加した希土類磁
石の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention contains R 2 M 17 containing a rare earth element transition metal as a main component.
The present invention relates to a method for producing a system (where R is a rare earth element containing yttrium and M is a transition metal) permanent magnet, and more specifically to a method for producing a rare earth magnet in which copper, zirconium and oxygen are added in appropriate amounts.
［従来の技術］ Ｒ−Ｃｏ−Ｆｅ−Ｃｕ系の２−１７系希土類永久磁石材
料は従来公知である。この系の合金材料において、Ｃｕ
の添加は保磁力を高める効果があり１０重量％以上は必
要であるとされていた。しかしＣｕの添加量が増大する
と残留磁束密度Ｂｒが低下してしまう問題が生じる。[Prior Art] An R-Co-Fe-Cu-based 2-17 series rare earth permanent magnet material is conventionally known. In this type of alloy material, Cu
It has been said that the addition of 1 has the effect of increasing the coercive force, and it is necessary to add 10% by weight or more. However, if the addition amount of Cu is increased, there arises a problem that the residual magnetic flux density Br is lowered.
この問題を解決するため更に適量のＺｒ（ジルコニウ
ム）を添加することにより低Ｃｕ量の組成で保磁力ｉＨ
ｃと最大エネルギー積（ＢＨ）max を高め得る技術が報
告されている（例えば特公昭５５−４７０９７，特公昭
５５−４８０９４）。In order to solve this problem, by adding an appropriate amount of Zr (zirconium), the coercive force iH can be reduced with a composition having a low Cu content.
A technique capable of increasing c and the maximum energy product (BH) max has been reported (for example, Japanese Patent Publication Nos. 55-47097 and 55-48094).
また近年、このＲ−Ｃｏ−Ｆｅ−Ｃｕ−Ｚｒ系で、Ｃｕ
の添加量を５重量％以下というように更に少なくし、且
つ適切な熱処理を施すことにより保磁力を高める技術も
提案されている（例えば特公昭６０−３４６３２）。In recent years, the R-Co-Fe-Cu-Zr system has a Cu content.
There has also been proposed a technique for further increasing the coercive force by further reducing the amount of addition of 5% by weight or less and performing an appropriate heat treatment (for example, Japanese Patent Publication No. 60-34632).
更に４πＩ−Ｈループの角型を良くするために、Ｒ２Ｍ
17系金属間化合物に酸素を含有させる技術が報告されて
いる（例えば特開昭５７−１３４５３３）。また保磁力
を向上させるために、Ｒ２Ｍ17系金属間化合物に酸素を
含有させる技術も報告されている（例えば特公昭５６−
４０４８４）。In order to further improve the squareness of the 4πI-H loop, R 2 M
A technique for containing oxygen in a 17- based intermetallic compound has been reported (for example, JP-A-57-134533). Further, in order to improve the coercive force, a technique of incorporating oxygen into the R 2 M 17 series intermetallic compound has also been reported (for example, Japanese Patent Publication No. 56-
40484).
［発明が解決しようとする問題点］ Ｃｕの添加量を抑えた組成でのＲ−Ｃｏ−Ｆｅ−Ｃｕ−
Ｚｒ系合金に限っては、非磁性であるＣｕ量を少なくし
たことにより残留磁束密度Ｂｒが向上し、その結果とし
て最大エネルギー積（ＢＨ）max を高めた磁石合金を得
ることができる。しかし従来技術では（ＢＨ）max を向
上させたとは言え、まだ（Ｂｒ）２／４には及ばない。[Problems to be Solved by the Invention] R-Co-Fe-Cu-with a composition in which the added amount of Cu is suppressed.
Only for Zr-based alloys, the residual magnetic flux density Br is improved by reducing the amount of non-magnetic Cu, and as a result, it is possible to obtain a magnet alloy with an increased maximum energy product (BH) max . But although the prior art has improved (BH) max, yet (Br) falls short of 2/4.
本発明の目的は、Ｃｕ量が１〜５重量％という低い領域
で従来品より高い（ＢＨ）maxを有する永久磁石を製造
する方法を提供することにある。An object of the present invention is to provide a method for producing a permanent magnet having a higher (BH) max than that of a conventional product in a region where the Cu content is as low as 1 to 5% by weight.
［問題点を解決するための手段］ 本発明者はＲ−Ｃｏ−Ｆｅ−Ｃｕ−Ｚｒ系の希土類永久
磁石材料に関し、４πＩ−Ｈループの角型を向上させる
こと、つまり（ＢＨ）max を向上させることについて種
々検討した結果、Ｒ−Ｃｏ−Ｆｅ−Ｃｕ−Ｚｒ系にＯ
（酸素）を適量添加した特定の組成をもち、焼結し溶体
化処理を施した材料について、２段時効を行い、第２段
時効を第１段時効よりも高い温度で行い所定の速度で冷
却することによって前記目的を達成できることを見出
し、本発明を完成させるに至ったものである。[Means for Solving Problems] The present inventor has improved the squareness of a 4πI-H loop, that is, (BH) max, with respect to an R-Co-Fe-Cu-Zr-based rare earth permanent magnet material. As a result of various investigations on the effect of O, R-Co-Fe-Cu-Zr-based O
A material having a specific composition to which (oxygen) is added in an appropriate amount, sintered and solution-treated, is subjected to two-step aging, second-step aging at a higher temperature than first-step aging, and at a predetermined rate The inventors have found that the above object can be achieved by cooling, and have completed the present invention.
即ち本発明は、２２〜２８重量％のＲ（但しＲはイット
リウムを含む希土類元素の１種もしくは２種以上），
５．５〜１７．５重量％のＦｅ，１〜５重量％のＣｕ，
０．５〜６重量％のＺｒ，０．０３〜０．８重量％の
Ｏ，残部が実質的にＣｏからなり、ＦｅとＣｏの重量比
率が０．１≦Ｆｅ／Ｃｏ≦０．２８である組成の材料を
用いる。That is, the present invention provides 22 to 28% by weight of R (where R is one or more rare earth elements including yttrium),
5.5 to 17.5 wt% Fe, 1 to 5 wt% Cu,
0.5 to 6% by weight of Zr, 0.03 to 0.8% by weight of O, and the balance substantially Co, and the weight ratio of Fe and Co is 0.1 ≦ Fe / Co ≦ 0.28. A material of a certain composition is used.
このような組成の材料を、まず１１５０〜１２５０℃で
焼結し、１１００〜１２３０℃で且つ焼結温度より低い
温度で溶体化処理を行い、次に第１段時効として４００
〜９００℃で１時間以上等温処理し、第２段時効として
７００〜１０００℃で且つ第１段時効よりも高い温度で
等温処理し、引き続いて毎分０．１〜１０℃の冷却速度
で連続的に３００〜６００℃まで冷却することを特徴と
する永久磁石の製造方法である。A material having such a composition is first sintered at 1150 to 1250 ° C., solution-treated at 1100 to 1230 ° C. and at a temperature lower than the sintering temperature, and then a first stage aging is performed at 400 °
Isothermal treatment at ~ 900 ° C for 1 hour or more, second stage aging at 700-1000 ° C and higher temperature than the first stage aging, and then continuously at a cooling rate of 0.1-10 ° C per minute. It is a method for manufacturing a permanent magnet, which is characterized in that it is cooled to 300 to 600 ° C.
本発明の特徴は、上記のようにＲ−Ｃｏ−Ｆｅ−Ｃｕ−
Ｚｒ系の組成において、Ｃｕ量を抑え適量のＺｒとＯを
添加する点、および第１段時効よりも高い温度で第２段
時効を行い、引き続いて所定の速度で冷却する点にあ
る。The feature of the present invention is that R-Co-Fe-Cu-
In the Zr-based composition, the Cu amount is suppressed and an appropriate amount of Zr and O are added, and the second stage aging is performed at a temperature higher than the first stage aging, and subsequently cooling is performed at a predetermined rate.
本発明における合金の組成比率や熱処理等は全て以下に
述べる実施例に示すような実験結果に基づいている。
Ｒ，Ｃｏ，Ｆｅの比率は、この種の３元系組成物で一般
的に使用されているものとほぼ同様である。The alloy composition ratios, heat treatments, and the like in the present invention are all based on the experimental results as shown in the following examples.
The ratios of R, Co and Fe are almost the same as those generally used in this type of ternary composition.
Ｒを２２〜２８重量％としたのは、２２重量％未満では
保磁力が小さく２８重量％を超えると残留磁束密度が低
下するからである。Ｆｅを５．５〜１７．５重量％とし
たのは、５．５重量％未満では残留磁束密度が低く、１
７．５重量％を超えると保磁力が低下するからである。The reason for setting R to 22 to 28% by weight is that the coercive force is less than 22% by weight and the residual magnetic flux density is reduced if more than 28% by weight. Fe is set to be 5.5 to 17.5% by weight because the residual magnetic flux density is low when it is less than 5.5% by weight.
This is because the coercive force decreases if it exceeds 7.5% by weight.
Ｃｕの含有量を１〜５重量％としたのは、１重量％未満
では保磁力が発生せず、５重量％を超えると残留磁束密
度が低下するからである。Ｚｒの含有量を０．５〜６重
量％としたのは、０．５重量％未満では保磁力が発生せ
ず、６重量％を超えると残留磁束密度が低下するからで
ある。Ｏの含有量を０．０３〜０．８重量％としたの
は、０．０３重量％未満では４πＩ−Ｈループの角型が
向上せず、０．８重量％を超えても４πＩ−Ｈループの
角型が悪くなり、しかも残留磁束密度も低下するからで
ある。The content of Cu is set to 1 to 5% by weight because the coercive force does not occur at less than 1% by weight and the residual magnetic flux density decreases at more than 5% by weight. The content of Zr is set to 0.5 to 6% by weight because the coercive force does not occur at less than 0.5% by weight and the residual magnetic flux density decreases at more than 6% by weight. The content of O is set to 0.03 to 0.8% by weight because the squareness of the 4πI-H loop is not improved when the content is less than 0.03% by weight, and the content of O is 4πI-H even when the content exceeds 0.8% by weight. This is because the square shape of the loop is deteriorated and the residual magnetic flux density is also reduced.
重量比率を０．１≦Ｆｅ／Ｃｏ≦０．２８としたのは、
Ｆｅが５．５〜１７．５重量％の範囲であってもＦｅ／
Ｃｏが０．２８を超えると保磁力が低下するし、Ｆｅ／
Ｃｏが０．１未満になると残留磁束密度が低下するから
である。The weight ratio of 0.1 ≦ Fe / Co ≦ 0.28 means that
Fe / Fe in the range of 5.5 to 17.5% by weight
When Co exceeds 0.28, the coercive force decreases and Fe /
This is because the residual magnetic flux density decreases when Co is less than 0.1.
なお酸素を含有させる方法としては、例えばジェットミ
ルで微粉砕する際にキャリアガスである窒素中に適量の
酸素を混ぜて吸収させる方法がある。As a method of containing oxygen, for example, there is a method of mixing a suitable amount of oxygen with nitrogen which is a carrier gas and absorbing it when finely pulverizing with a jet mill.
焼結温度を１１５０〜１２５０℃としたのは、１１５０
℃未満では焼結密度が上昇せず残留磁束密度が低くなる
し、焼結温度が高いほど密度が上がり残留磁束密度が高
くなるが１２５０℃を超えると焼結体が溶け、残留磁束
密度がかえって低くなるからである。焼結温度より低い
１１００〜１２３０℃で溶体化処理を行うのは、１１０
０℃未満や１２３０℃を超えると、あるいは焼結温度よ
り高い温度ではエネルギー積が改善されないからであ
る。The sintering temperature was set to 1150 to 1250 ° C. was 1150.
If the temperature is lower than ℃, the sintered density does not increase and the residual magnetic flux density decreases, and as the sintering temperature increases, the density increases and the residual magnetic flux density increases, but if the temperature exceeds 1250 ° C, the sintered body melts and the residual magnetic flux density changes. Because it will be low. The solution treatment at 1100 to 1230 ° C, which is lower than the sintering temperature, is 110
This is because the energy product is not improved at a temperature lower than 0 ° C., higher than 1230 ° C., or higher than the sintering temperature.
また第１段時効より高い温度で第２段時効を行い、第２
段時効温度から連続冷却するのは、それによってＣｕが
１〜５重量％でも高い保磁力を保たせることができるか
らである。The second stage aging is performed at a temperature higher than the first stage aging, and the second stage aging is performed.
The reason for continuously cooling from the step aging temperature is that it can maintain a high coercive force even if Cu is 1 to 5% by weight.
［作用］ このような特定の組成と熱処理条件との組み合わせを採
用することによって、Ｒ−Ｃｏ−Ｆｅ−Ｃｕ−Ｚｒ−Ｏ
系の永久磁石材料においてＲ−Ｃｏ−Ｆｅ−Ｃｕ−Ｚｒ
系の永久磁石材料と同等の保磁力が得られ、しかも４π
Ｉ−Ｈループの角型を向上させることが可能となり、結
果として高い最大エネルギー積（ＢＨ）max を得ること
ができる。[Operation] By adopting such a combination of the specific composition and the heat treatment condition, R—Co—Fe—Cu—Zr—O
R-Co-Fe-Cu-Zr
Coercive force equivalent to that of the permanent magnet material of the system is obtained, and 4π
It is possible to improve the squareness of the I-H loop, and as a result, it is possible to obtain a high maximum energy product (BH) max .
［実施例１］ （合金の組成） Ｓｍ＝２４．１重量％，Ｆｅ＝１２．９重量％，Ｃｕ＝
３．９重量％，Ｚｒ＝２．３重量％，Ｏ＝０．０２〜
０．９重量％，残部がＣｏからなる。[Example 1] (Composition of alloy) Sm = 24.1% by weight, Fe = 12.9% by weight, Cu =
3.9 wt%, Zr = 2.3 wt%, O = 0.02
0.9% by weight with the balance being Co.
（前工程） 必要とする合金材料を高周波溶解炉で溶解し、ジョーク
ラッシャによって粗粉砕した後、ジェットミルにより微
粉砕した。微粉砕の際に適量の酸素をジェットに混ぜて
含有させた。この微粉砕粉体を１５ｋＯｅの磁場中で成
形圧３ton/cm２ で圧縮成形した。(Previous Step) The required alloy material was melted in a high frequency melting furnace, coarsely crushed by a jaw crusher, and then finely crushed by a jet mill. An appropriate amount of oxygen was mixed with the jet during the milling. This finely pulverized powder was compression molded in a magnetic field of 15 kOe at a molding pressure of 3 ton / cm 2 .
（熱処理） 酸素の含有量に応じて１１８０〜１２１０℃で３時間の
焼結を行い、１１４０℃以上で且つ焼結温度より低い温
度で２時間の溶体化処理を行った。その後、第１段時効
として６５０℃で３時間保持し、第２段時効を８５０℃
で３時間行い、引き続いて２℃／分の冷却速度で４００
℃まで冷却した。酸素の含有量に対しるｉＨｃ，Ｂｒ，
（ＢＨ）max の測定結果を第１表に示す。(Heat Treatment) Sintering was performed at 1180 to 1210 ° C. for 3 hours depending on the oxygen content, and solution treatment was performed at a temperature of 1140 ° C. or higher and lower than the sintering temperature for 2 hours. Then, as the first stage aging, hold at 650 ° C for 3 hours, and then the second stage aging at 850 ° C.
For 3 hours and then 400 at a cooling rate of 2 ° C / min.
Cooled to ° C. IHc, Br, depending on the oxygen content
Table 1 shows the measurement results of (BH) max .
酸素含有量が０．０３重量％未満では４πＩ−Ｈループ
の角型が悪く、（ＢＨ）max が低い。また酸素含有量が
０．８重量％を超えると残留磁束密度Ｂｒが低下し、し
かも４πＩ−Ｈループの角型が悪く（ＢＨ）max も低く
なる。 When the oxygen content is less than 0.03% by weight, the squareness of the 4πI-H loop is poor and the (BH) max is low. When the oxygen content exceeds 0.8% by weight, the residual magnetic flux density Br decreases, and the squareness of the 4πI-H loop is poor, and (BH) max also decreases.
［実施例２］ （合金の組成） Ｓｍ＝２４．１重量％，Ｆｅ＝１２．９重量％，Ｃｕ＝
０．７〜５．５重量％，Ｚｒ＝２．３重量％，Ｏ＝０．
０２〜０．９重量％，残部がＣｏからなる。Example 2 (Composition of alloy) Sm = 24.1% by weight, Fe = 12.9% by weight, Cu =
0.7-5.5% by weight, Zr = 2.3% by weight, O = 0.
02 to 0.9% by weight, the balance being Co.
（前工程） 実施例１に同じ。(Previous Step) Same as in Example 1.
（熱処理） Ｃｕの含有量に応じて１１７０〜１２１０℃で３時間の
焼結を行い、１１３０℃以上で且つ焼結温度より低い温
度で２時間の溶対化処理を行った。その後、第１段時効
として６５０℃で３時間保持し、第２段時効を８５０℃
で３時間行い、引き続いて２℃／分の冷却速度で４００
℃まで冷却した。Ｃｕの含有量に対するｉＨｃ，Ｂｒ，
（ＢＨ）max の測定結果を第２表に示す。(Heat Treatment) Sintering was performed at 1170 to 1210 ° C. for 3 hours depending on the Cu content, and solution treatment was performed at 1130 ° C. or higher and lower than the sintering temperature for 2 hours. Then, as the first stage aging, hold at 650 ° C for 3 hours, and then the second stage aging at 850 ° C.
For 3 hours and then 400 at a cooling rate of 2 ° C / min.
Cooled to ° C. IHc, Br, for the Cu content
The measurement results of (BH) max are shown in Table 2.
このようにＣｕ含有量が１．０重量％未満では保磁力ｉ
Ｈｃが低くなる。またＣｕ含有量が５重量％を超えると
残留磁束密度Ｂｒが低くなる。 Thus, when the Cu content is less than 1.0% by weight, the coercive force i
Hc becomes low. Further, when the Cu content exceeds 5% by weight, the residual magnetic flux density Br becomes low.
［実施例３］ （合金の組成） Ｓｍ＝２４．１重量％，Ｆｅ＝１２．９重量％，Ｃｕ＝
３．９重量％，Ｚｒ＝０．３〜６．７重量％，Ｏ＝０．
０２重量％，残部がＣｏからなる。[Example 3] (Composition of alloy) Sm = 24.1% by weight, Fe = 12.9% by weight, Cu =
3.9% by weight, Zr = 0.3 to 6.7% by weight, O = 0.
02% by weight, the balance being Co.
（前工程） 実施例１に同じ。(Previous Step) Same as in Example 1.
（熱処理） Ｚｒの含有量に応じて１１７０〜１２０５℃で３時間の
焼結を行い、１１３０℃以上で且つ焼結温度より低い温
度で２時間の溶対化処理を行った。その後、第１段時効
として６５０℃で３時間保持し、第２段時効を８５０℃
で３時間行い、引き続いて２℃／分の冷却速度で４００
℃まで冷却した。Ｚｒの含有量に対するｉＨｃ，Ｂｒ，
（ＢＨ）max の測定結果を第３表に示す。(Heat Treatment) Sintering was performed at 1170 to 1205 ° C. for 3 hours depending on the content of Zr, and solution treatment was performed at 1130 ° C. or higher and lower than the sintering temperature for 2 hours. Then, as the first stage aging, hold at 650 ° C for 3 hours, and then the second stage aging at 850 ° C.
For 3 hours and then 400 at a cooling rate of 2 ° C / min.
Cooled to ° C. IHc, Br, relative to the content of Zr
The measurement results of (BH) max are shown in Table 3.
Ｚｒ含有量が０．５重量％未満では保磁力ｉＨｃが低く
なる。またＺｒ含有量が６．０重量％を超えると残留磁
束密度Ｂｒが低下する。 When the Zr content is less than 0.5% by weight, the coercive force iHc becomes low. If the Zr content exceeds 6.0% by weight, the residual magnetic flux density Br decreases.
［実施例４］ （合金の組成） Ｓｍ＝１２．１〜２４．１重量％，Ｃｅ＝０〜１２．０
重量％（但しＳｍ＋Ｃｅ＝２４．１重量％），Ｆｅ＝１
２．９重量％，Ｃｕ＝３．９重量％，Ｚｒ＝２．３重量
％，Ｏ＝０．２重量％，残部がＣｏからなる。[Example 4] (Composition of alloy) Sm = 12.1 to 24.1% by weight, Ce = 0 to 12.0
Wt% (however, Sm + Ce = 24.1 wt%), Fe = 1
2.9% by weight, Cu = 3.9% by weight, Zr = 2.3% by weight, O = 0.2% by weight, and the balance being Co.
（前工程） 実施例１に同じ。(Previous Step) Same as in Example 1.
（熱処理） Ｃｅの含有量に応じて１１６５〜１２０５℃で３時間の
焼結を行い、１１３０℃以上で且つ焼結温度より低い温
度で２時間の溶対化処理を行った。その後、第１段時効
として６５０℃で３時間保持し、第２段時効を８５０℃
で３時間行い、引き続いて２℃／分の冷却速度で４００
℃まで冷却した。Ｃｅの含有量に対するｉＨｃ，Ｂｒ，
（ＢＨ）max の測定結果を第４表に示す。(Heat Treatment) Sintering was performed at 1165 to 1205 ° C. for 3 hours depending on the content of Ce, and solution treatment was performed at a temperature of 1130 ° C. or higher and lower than the sintering temperature for 2 hours. Then, as the first stage aging, hold at 650 ° C for 3 hours, and then the second stage aging at 850 ° C.
For 3 hours and then 400 at a cooling rate of 2 ° C / min.
Cooled to ° C. IHc, Br, with respect to the content of Ce,
The measurement results of (BH) max are shown in Table 4.
このようにＣｅの置換量が多くなるほど特性は悪くなる
が、Ｓｍの一部をＣｅで置換しても実用上は十分な特性
が得られる。このことはＳｍ以外の希土類元素（イット
リウムを含む）の場合でも本発明は有効であることを示
唆している。 As described above, the characteristics deteriorate as the amount of substitution of Ce increases, but even if a part of Sm is substituted with Ce, practically sufficient characteristics can be obtained. This suggests that the present invention is effective even in the case of rare earth elements (including yttrium) other than Sm.
［実施例５］ （合金の組成） Ｓｍ＝２４．１重量％，Ｃｕ＝３．９重量％，Ｚｒ＝
２．３重量％，Ｏ＝０．２重量％，Ｆｅ＝６．２，〜１
５．８重量％，Ｃｏ＝５３．７〜６３．３重量％（但し
Ｆｅ＋Ｃｏ＝６９．５重量％）からなる。[Example 5] (Composition of alloy) Sm = 24.1% by weight, Cu = 3.9% by weight, Zr =
2.3% by weight, O = 0.2% by weight, Fe = 6.2, -1
It is composed of 5.8 wt% and Co = 53.7 to 63.3 wt% (however, Fe + Co = 69.5 wt%).
（前工程） 実施例１に同じ。(Previous Step) Same as in Example 1.
（熱処理） Ｆｅの含有量に応じて１１８０〜１２０５℃で３時間の
焼結を行い、１１４０℃以上で且つ焼結温度より低い温
度で２時間の溶体化処理を行った。その後、第１段時効
として６５０℃で３時間保持し、第２段時効を８５０℃
で３時間行い、引き続いて２℃／分の冷却速度で４００
℃まで冷却した。Ｆｅの含有量に対するｉＨｃ，Ｂｒ，
（ＢＨ）max の測定結果を第５表に示す。(Heat Treatment) Sintering was performed at 1180 to 1205 ° C. for 3 hours depending on the content of Fe, and solution treatment was performed at 1140 ° C. or higher and lower than the sintering temperature for 2 hours. Then, as the first stage aging, hold at 650 ° C for 3 hours, and then the second stage aging at 850 ° C.
For 3 hours and then 400 at a cooling rate of 2 ° C / min.
Cooled to ° C. IHc, Br, with respect to the content of Fe,
Table 5 shows the measurement results of (BH) max .
Ｆｅが５．５〜１７．５重量％の範囲内であっても重量
比率でＦｅ／Ｃｏが０．２８を超えると４πＩ−Ｈルー
プの角型が悪くなり（ＢＨ）max が低くなる。またＦｅ
／Ｃｏが０．１０未満だと残留磁束密度Ｂｒが低くなり
（ＢＨ）max も低くなる。 Even if Fe is in the range of 5.5 to 17.5 wt%, if the weight ratio of Fe / Co exceeds 0.28, the squareness of the 4πI-H loop becomes poor and (BH) max becomes low. Also Fe
When / Co is less than 0.10, the residual magnetic flux density Br becomes low and (BH) max also becomes low.
［実施例６］ （合金の組成） Ｓｍ＝２４．１重量％，Ｆｅ＝１２．９重量％，Ｃｕ＝
３．９重量％，Ｚｒ＝２．３重量％，Ｏ＝０．２重量
％，残部がＣｏからなる。[Example 6] (Composition of alloy) Sm = 24.1% by weight, Fe = 12.9% by weight, Cu =
3.9% by weight, Zr = 2.3% by weight, O = 0.2% by weight, and the balance being Co.
（前工程） 実施例１に同じ。(Previous Step) Same as in Example 1.
（熱処理） １１９０℃で３時間の焼結を行い、１１６０℃で２時間
の溶対化処理を行った。その後、第１段時効を６００〜
８００℃で３時間行い、第２段時効として８５０℃で３
時間保持し、引き続いて２℃／分の冷却速度で４００℃
まで冷却した。第１段時効の温度に対するｉＨｃ，Ｂ
ｒ，（ＢＨ）max の測定結果を第６表に示す。(Heat Treatment) Sintering was performed at 1190 ° C. for 3 hours, and solution treatment was performed at 1160 ° C. for 2 hours. After that, the first stage aging is 600 ~
Perform at 800 ° C for 3 hours, then as second aging at 850 ° C for 3 hours
Hold for a time and then 400 ℃ at a cooling rate of 2 ℃ / min
Cooled down. IHc, B against the temperature of the first stage aging
Table 6 shows the measurement results of r, (BH) max .
第７表は６５０℃で１〜８時間の第１段時効処理後、第
２段時効として８５０℃で３時間処理し、引き続いて２
℃／分の冷却速度で４００℃まで冷却した場合のｉＨ
ｃ，Ｂｒ，（ＢＨ）max の測定結果である。Table 7 shows that after the first stage aging treatment at 650 ° C. for 1 to 8 hours, the second stage aging treatment was performed at 850 ° C. for 3 hours, followed by 2
IH when cooled to 400 ° C at a cooling rate of ° C / min
It is a measurement result of c, Br, (BH) max .
第８表は６５０℃で３時間の第１段時効処理後、第２段
時効として８００〜９００℃で３時間処理し、引き続い
て２℃／分の冷却速度で４００℃まで冷却した場合のｉ
Ｈｃ，Ｂｒ，（ＢＨ）max の測定結果である。Table 8 shows i in the case where after the first stage aging treatment at 650 ° C. for 3 hours, the second stage aging treatment was performed at 800 to 900 ° C. for 3 hours, followed by cooling to 400 ° C. at a cooling rate of 2 ° C./min.
It is a measurement result of Hc, Br, (BH) max .
第９表は６５０℃で３時間の第１段時効処理後、第２段
時効として８５０℃で１〜８時間処理し、引き続いて２
℃／分の冷却速度で４００℃まで冷却した場合のｉＨ
ｃ，Ｂｒ，（ＢＨ）max の測定結果である。Table 9 shows that after the first stage aging treatment at 650 ° C. for 3 hours, the second stage aging treatment was performed at 850 ° C. for 1 to 8 hours, followed by 2
IH when cooled to 400 ° C at a cooling rate of ° C / min
It is a measurement result of c, Br, (BH) max .
第１０表は６５０℃で３時間の第１段時効処理後、第２
段時効として８５０℃で３時間処理し、引き続いて０．
１〜１０℃／分の冷却速度で４００℃まで冷却した場合
のｉＨｃ，Ｂｒ，（ＢＨ）max の測定結果である。Table 10 shows that after the first stage aging treatment at 650 ° C for 3 hours, the second
As a step aging, treatment was carried out at 850 ° C. for 3 hours, and then 0.
It is a measurement result of iHc, Br, (BH) max in the case of cooling to 400 ° C. at a cooling rate of 1 to 10 ° C./min.
これら第６表〜第１０表から分かるように、１つの組成
であっても熱処理条件を変えることによって種々の用途
に適した高性能の永久磁石合金が得られる。As can be seen from Tables 6 to 10, even with one composition, a high-performance permanent magnet alloy suitable for various applications can be obtained by changing the heat treatment conditions.
これらの表から分かるように、一つの組成であっても熱
処理条件を変えることによって種々の用途に適した高性
能の永久磁石合金が得られる。 As can be seen from these tables, high performance permanent magnet alloys suitable for various applications can be obtained by changing the heat treatment conditions even with one composition.
［発明の効果］ 本発明は上記のような特定組成のＲ−Ｃｏ−Ｆｅ−Ｃｕ
−Ｚｒ−Ｏ系の材料に特殊な熱処理を施すように構成し
たから、従来技術と同等の保磁力を発生させることが可
能であり、また従来技術より４πＩ−Ｈループの角型が
良好となり、最大エネルギー積（ＢＨ）max も向上させ
ることができる効果が生じる。EFFECTS OF THE INVENTION The present invention has the above-described specific composition of R—Co—Fe—Cu.
Since the -Zr-O-based material is configured to be subjected to a special heat treatment, it is possible to generate a coercive force equivalent to that of the conventional technique, and the square shape of the 4πI-H loop becomes better than that of the conventional technique. There is an effect that the maximum energy product (BH) max can also be improved.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 水野 保敏 東京都港区新橋５丁目36番11号 富士電気 化学株式会社内 (56)参考文献 特開 昭61−135102（ＪＰ，Ａ) 特開 昭57−134533（ＪＰ，Ａ) 特開 昭56−24903（ＪＰ，Ａ) 特開 昭61−136631（ＪＰ，Ａ) 特開 昭58−45302（ＪＰ，Ａ) 特開 昭61−210161（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Yasutoshi Mizuno 5-36-11 Shinbashi, Minato-ku, Tokyo Fuji Electric Chemical Co., Ltd. (56) Reference JP-A-61-135102 (JP, A) JP JP-A-57-134533 (JP, A) JP-A-56-24903 (JP, A) JP-A-61-136631 (JP, A) JP-A-58-45302 (JP, A) JP-A-61-210161 (JP , A)
Claims (1)
ウムを含む希土類元素の１種もしくは２種以上），５．
５〜１７．５重量％のＦｅ，１〜５重量％のＣｕ，０．
５〜６重量％のＺｒ，０．０３〜０．８重量％のＯ，残
部が実質的にＣｏからなり、ＦｅとＣｏの重量比率が
０．１≦Ｆｅ／Ｃｏ≦０．２８である組成の合金を、１
１５０〜１２５０℃で焼結し、１１００〜１２３０℃で
且つ焼結温度より低い温度で溶体化処理を行い、次に第
１段時効として４００〜９００℃で１時間以上等温処理
し、第２段時効として７００〜１０００℃で且つ第１段
時効よりも高い温度で等温処理し、引き続いて毎分０．
１〜１０℃の冷却速度で連続的に３００〜６００℃まで
冷却することを特徴とする永久磁石の製造方法。1. 22 to 28% by weight of R (where R is one or more rare earth elements including yttrium),
5 to 17.5 wt% Fe, 1 to 5 wt% Cu, 0.
A composition in which 5 to 6% by weight of Zr, 0.03 to 0.8% by weight of O, and the balance substantially Co, and the weight ratio of Fe and Co is 0.1 ≦ Fe / Co ≦ 0.28. Alloy of 1
Sintering is performed at 150 to 1250 ° C., solution treatment is performed at a temperature of 1100 to 1230 ° C. and lower than the sintering temperature, and then isothermal treatment is performed at 400 to 900 ° C. for 1 hour or more as the first aging, and then the second The aging treatment was carried out isothermally at 700 to 1000 ° C. and at a temperature higher than that of the first stage aging, and then 0.
A method for producing a permanent magnet, which comprises continuously cooling to 300 to 600 ° C at a cooling rate of 1 to 10 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62269115A JPH0620007B2 (en) | 1987-10-24 | 1987-10-24 | Permanent magnet manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62269115A JPH0620007B2 (en) | 1987-10-24 | 1987-10-24 | Permanent magnet manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01111304A JPH01111304A (en) | 1989-04-28 |
| JPH0620007B2 true JPH0620007B2 (en) | 1994-03-16 |
Family
ID=17467883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62269115A Expired - Lifetime JPH0620007B2 (en) | 1987-10-24 | 1987-10-24 | Permanent magnet manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0620007B2 (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5829603B2 (en) * | 1979-08-07 | 1983-06-23 | セイコーエプソン株式会社 | Permanent magnet manufacturing method |
| JPS57134533A (en) * | 1981-02-12 | 1982-08-19 | Namiki Precision Jewel Co Ltd | Permanent magnet alloy |
| JPS6034632A (en) * | 1983-08-05 | 1985-02-22 | 東レエンジニアリング株式会社 | Orienting and false twisting method and apparatus |
| JPS61135102A (en) * | 1984-12-06 | 1986-06-23 | Hitachi Metals Ltd | Manufacture of rare earth metal permanent magnet |
-
1987
- 1987-10-24 JP JP62269115A patent/JPH0620007B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01111304A (en) | 1989-04-28 |
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