JPH0354805A - Rare-earth permanent magnet and manufacture thereof - Google Patents
Rare-earth permanent magnet and manufacture thereofInfo
- Publication number
- JPH0354805A JPH0354805A JP1190168A JP19016889A JPH0354805A JP H0354805 A JPH0354805 A JP H0354805A JP 1190168 A JP1190168 A JP 1190168A JP 19016889 A JP19016889 A JP 19016889A JP H0354805 A JPH0354805 A JP H0354805A
- Authority
- JP
- Japan
- Prior art keywords
- minutes
- permanent magnet
- hours
- rare
- 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.)
- Pending
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 22
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 239000000956 alloy Substances 0.000 claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 7
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 4
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 4
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 3
- 229910052689 Holmium Inorganic materials 0.000 claims abstract 2
- 229910052735 hafnium Inorganic materials 0.000 claims abstract 2
- 229910052758 niobium Inorganic materials 0.000 claims abstract 2
- 229910052715 tantalum Inorganic materials 0.000 claims abstract 2
- 229910052719 titanium Inorganic materials 0.000 claims abstract 2
- 229910052721 tungsten Inorganic materials 0.000 claims abstract 2
- 229910052726 zirconium Inorganic materials 0.000 claims abstract 2
- 230000032683 aging Effects 0.000 claims description 23
- 238000005245 sintering Methods 0.000 claims description 22
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims description 2
- 230000005415 magnetization Effects 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 8
- 230000004907 flux Effects 0.000 abstract description 4
- 229910017052 cobalt Inorganic materials 0.000 abstract description 2
- 239000010941 cobalt Substances 0.000 abstract description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910052723 transition metal Inorganic materials 0.000 abstract description 2
- 150000003624 transition metals Chemical class 0.000 abstract description 2
- -1 cobalt Chemical class 0.000 abstract 1
- 230000006835 compression Effects 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 229910052720 vanadium Inorganic materials 0.000 abstract 1
- 229910052727 yttrium Inorganic materials 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VZUGBLTVBZJZOE-KRWDZBQOSA-N n-[3-[(4s)-2-amino-1,4-dimethyl-6-oxo-5h-pyrimidin-4-yl]phenyl]-5-chloropyrimidine-2-carboxamide Chemical compound N1=C(N)N(C)C(=O)C[C@@]1(C)C1=CC=CC(NC(=O)C=2N=CC(Cl)=CN=2)=C1 VZUGBLTVBZJZOE-KRWDZBQOSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
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
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、広い温度範囲にわたって磁束変化の少ない、
温度特性に優れた希土類永久磁石とその製造方法に関す
るものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention provides a magnetic flux that exhibits small changes in magnetic flux over a wide temperature range.
The present invention relates to a rare earth permanent magnet with excellent temperature characteristics and a method for manufacturing the same.
（従来の技術）
従来のＳｍ系２−１７型希土類永久磁石は、Ｎｄ系、Ｃ
ｅ系と比較すると磁化の温度特性（可逆温度係数で表わ
すと、Ｓｍ系−０．０３％／”Ｃ，Ｎｄ系一〇．ｌ３％
／℃、Ｃｅ系−０．０９％／℃となる）は良いが、広い
温度範囲、例えば−２０〜１００℃で使用する航空機、
計測器等の精密電子機器の制御には温度に対する磁束の
変化量がさらに少ない温度特性の良いものが求められて
いた。(Prior art) Conventional Sm-based 2-17 type rare earth permanent magnets include Nd-based, C
When compared with the e-type, the temperature characteristics of magnetization (expressed as a reversible temperature coefficient: Sm-0.03%/C, Nd-10.13%)
/℃, Ce-based -0.09%/℃) is good, but aircraft used in a wide temperature range, for example -20 to 100℃,
For the control of precision electronic equipment such as measuring instruments, there has been a demand for devices with better temperature characteristics that have even smaller changes in magnetic flux with respect to temperature.
また、Ｓｌｏ系ｌ−５型磁石のＳｍをＧｄ． Ｅｒ．
Ｄｙ等の重希土類元素で置換した磁石は飽和磁気履歴曲
線（以下、ヒステリシスカーブと略称する）の角型性が
悪く、比較的磁気特性の低いものしか得られていなかっ
た（参考文献：１）Ｄｏｎｇ Ｌｉ，Ｅｒｄａ Ｘｕ：
ＩＥＥＥ ＴＲＡＮＳ Ｖｏｌ．ＭＡＧ−１６ Ｎ
ｏ．５，Ｓｅｐｔ．１９８０、 ２）Ｆ．Ｇ． Ｊｏ
ｎｅｓａｎｄ Ｍ．Ｔｏｋｕｎａｇａ：ＩＥＥＥ
ＴＲＡＮＳ Ｖｏｌ．ＭＡＧ−１２， Ｎｏ．６，
Ｎｏｖ．１９７６） ．さらにＳｍ系２−１７型希土類
磁石を基礎とし、ＳｍをＧｄ． Ｅｒ， Ｄｙ等の重希
土類元素で置換した磁石も角型性が悪く、着磁に際し大
型の着磁装置を必要とする欠点があった（参考文献：３
）熊坂、星野、小野：低温度係数Ｒ＊ （ＣｏＦｅＣ：
ｕＺｒ） ＋ ７系希土類磁石：電気通信学会技報、Ｃ
ＰＭ８３−３６， ｐ．９９１〜９９７． １９８３）
。In addition, Sm of the Slo type l-5 type magnet is Gd. Er.
Magnets substituted with heavy rare earth elements such as Dy have poor squareness in their saturation magnetic hysteresis curves (hereinafter referred to as hysteresis curves), and only those with relatively low magnetic properties were obtained (Reference: 1) Dong Li, Erda Xu:
IEEE TRANS Vol. MAG-16N
o. 5, Sept. 1980, 2) F. G. Jo
nesand M. Tokunaga: IEEE
TRANS Vol. MAG-12, No. 6,
Nov. 1976). Furthermore, based on Sm type 2-17 type rare earth magnet, Sm is Gd. Magnets substituted with heavy rare earth elements such as Er and Dy also have poor squareness and have the disadvantage of requiring a large magnetizing device for magnetization (Reference: 3).
) Kumasaka, Hoshino, Ono: Low temperature coefficient R* (CoFeC:
uZr) + 7-series rare earth magnet: Institute of Electrical Communication Engineers Technical Report, C
PM83-36, p. 991-997. 1983)
.
（発明が解決しようとする課題）
本発明は、このような従来の磁石の持つ欠点を除去する
ため、Ｓｍ系２−１７型希土類磁石を基礎として、Ｓｍ
をＧｄ． Ｅｒ． Ｄｙ等の重希土類元素で置換し、多
段焼結、多段時効処理の最適条件を組み合わせることに
よって、磁化の温度特性を大幅に向上し、かつ、角型性
の良い希土類永久磁石を提供することにある。(Problems to be Solved by the Invention) In order to eliminate the drawbacks of such conventional magnets, the present invention is based on the Sm type 2-17 type rare earth magnet.
Gd. Er. By substituting with heavy rare earth elements such as Dy, and combining the optimal conditions of multi-stage sintering and multi-stage aging treatment, we have significantly improved the temperature characteristics of magnetization and provided rare earth permanent magnets with good squareness. be.
（課題を解決するための手段）
本発明者等は、かかる課題を解決するために磁石合金組
成、磁化条件について鋭意検討した結果、本発明を完成
した。その要旨とするところは、１．一般式 ＳＩＩ
＋＋−ｘＲｘ（Ｇｏｔ−ｕ−ｖ−ｙＦｅｕｃｕｖＭｙ）
ｚ（ここにＲはＧｄ， Ｔｂ． Ｄｙ． Ｈｏ． Ｅｒ
．Ｔｍから選ばれる少なくとも１種以上、ＭはＴｉ．
Ｚｒ． Ｈｆ． Ｎｂ． Ｔａ． Ｗから選ばれる少な
くとも１種以上、０．２≦Ｘ≦０．６、０．１≦ＩＪ≦
０．３、０．０２≦Ｖ ≦０．０６、０．００３ ≦Ｙ
≦０．０５、６．５≦Ｚ≦８．０）で表わされる合金
組成物からなる希土類永久磁石および
２．請求項１に記載の合金組成物を微粉砕し、この微粉
を磁界中で所定形状に圧縮成形した後、焼結、溶体化お
よび時効処理する永久磁石の製造方法において、ａ）１
，１００ 〜１，２５０℃の範囲内で２段階以上の多段
填結を合計３０分間〜５時間行なった後、ｂ）１，００
０〜１，２００℃の範囲内で２０分間〜３時間溶体化処
理するが、ｃ） ａ）の焼結時間およびｂ）の溶体化時
間の合計を５０分間〜８時間内とし、次いでｄ）４００
〜１，０００℃の範囲内で２回以上の時効処理を行なう
ことを特徴とする希土類永久磁石の製造方法にある。(Means for Solving the Problems) In order to solve the problems, the present inventors have completed the present invention as a result of intensive studies on magnet alloy composition and magnetization conditions. The main points are: 1. General formula SII
++-xRx (Got-u-v-yFeucuvMy)
z (here R is Gd, Tb. Dy. Ho. Er
．． At least one species selected from Tm, M is Ti.
Zr. Hf. Nb. Ta. At least one type selected from W, 0.2≦X≦0.6, 0.1≦IJ≦
0.3, 0.02≦V ≦0.06, 0.003≦Y
2. a rare earth permanent magnet consisting of an alloy composition represented by 0.05, 6.5 ≦ Z ≦ 8.0); and 2. A method for producing a permanent magnet, which comprises finely pulverizing the alloy composition according to claim 1, compression molding the fine powder into a predetermined shape in a magnetic field, and then sintering, solutionizing and aging treatment, comprising: a)1.
, 100 to 1,250°C for a total of 30 minutes to 5 hours, b) 1,00
Solution treatment is carried out at a temperature of 0 to 1,200°C for 20 minutes to 3 hours, but c) the total of the sintering time in a) and the solution treatment time in b) is within 50 minutes to 8 hours, and then d) 400
A method for producing a rare earth permanent magnet, characterized by performing aging treatment two or more times within the range of ~1,000°C.
？下、本発明を詳細に説明する。? Below, the present invention will be explained in detail.
先ず、永久磁石合金組成について述べる。First, the composition of the permanent magnet alloy will be described.
一般に、希土類二相分離型磁石はＲＴｇ−ｓ． ｓ （
式中Ｒは希土類元素、丁はコバルトを含む遷移金属）で
表わされるが、本発明においては、一般式Ｓｍ＋ −ｘ
Ｒｘ （Ｃｏｔ−ｕ−ｖ−ＪｅｕＣｕｖＭｙ） ｚの組
成式が有効である。ここにＲはＧｄ．Ｔｂ， Ｄｙ．
Ｈｏ． Ｅｒ． Ｔｍから選ばれる少なくとも１種以上
とされ、温度特性の点からＧｄが好ましい。、ＭはＴｉ
． Ｚｒ． Ｈｆ． Ｎｂ； Ｔａ． Ｗから選ばれる
少なくとも１種以上とされ、角型比向上のの点からＺｒ
． Ｔｉが好ましい。ＲとＴ５〜６■に相当する（Ｓｍ
＋−ｘＲｘ）と（ＧＯ＋−ｕ−ｖ−ＹＦｅｕＣｕｖＭｙ
）ｚとの比Ｚは６．５≦Ｚ≦８．０に限定され、好まし
くは７．２≦Ｚ≦７．８である。６．５未満では飽和磁
化の低下が大となり、８．０を超えると充分な保磁力が
得られなくなる。また、Ｘは０．２≦Ｘ≦０．６の範囲
、好ましくは０．３≦Ｘ≦０．５が良く、０．２未満で
は重粕土類を添加しても、磁化の温度特性の改善効果が
顕著でなくなり、０．６を越えると飽和磁化の低下が大
きく、実用上有効でない。他方、Ｕおよび■の値を０．
１≦Ｕ≦０．３ 、０．０２≦Ｖ ≦０．０６と限定し
たのは一般公知の経験に基づき、二相分離型磁石におけ
る高特性実現の範囲であり、かつ、本発明の製造方法に
おいて有効であることが確認されたからである。即ち、
Ｕが０．１未満では飽和磁化は充分上がらず、０．３を
越えると飽和磁化は上がるが、充分な保持力を確保出来
ないためである。Generally, rare earth two-phase separated magnets are RTg-s. s (
In the formula, R is a rare earth element and D is a transition metal containing cobalt), but in the present invention, the general formula Sm+ -x
The compositional formula Rx (Cot-uv-JeuCuvMy)z is effective. Here R is Gd. Tb, Dy.
Ho. Er. It is at least one selected from Tm, and Gd is preferred from the viewpoint of temperature characteristics. , M is Ti
．． Zr. Hf. Nb; Ta. At least one kind selected from W, and from the viewpoint of improving the squareness ratio, Zr
．． Ti is preferred. Corresponds to R and T5~6■ (Sm
+-xRx) and (GO+-u-v-YFeuCuvMy
) Z is limited to 6.5≦Z≦8.0, preferably 7.2≦Z≦7.8. If it is less than 6.5, the saturation magnetization will decrease significantly, and if it exceeds 8.0, sufficient coercive force will not be obtained. In addition, X should be in the range of 0.2≦X≦0.6, preferably 0.3≦X≦0.5, and if it is less than 0.2, even if heavy lees earth is added, the temperature characteristics of magnetization will be affected. The improvement effect becomes less noticeable, and if it exceeds 0.6, the saturation magnetization decreases so much that it is not practically effective. On the other hand, the values of U and ■ are set to 0.
The limitations of 1≦U≦0.3 and 0.02≦V≦0.06 are based on generally known experience, and are within the range of achieving high characteristics in a two-phase separated magnet, and also within the manufacturing method of the present invention. This is because it has been confirmed to be effective. That is,
If U is less than 0.1, the saturation magnetization will not increase sufficiently, and if it exceeds 0.3, the saturation magnetization will increase, but sufficient coercive force cannot be ensured.
■の値を限定した理由もＵの場合と同様に０，０２未満
では保持力が充分確保出来ず、逆に０．０６を越えると
、充分な飽和磁化を確保できないためである。微量添加
物ＭはＹの値が０． ００３≦Ｙ≦０．０５が良＜ ，
０．００３未満では本発明の熱処理効果が実現されず
、逆に０．０５を越えると逆効果のみが表われ、磁石の
磁気特性が悪くなる。The reason for limiting the value of (2) is that, as in the case of U, if it is less than 0.02, sufficient coercive force cannot be ensured, and conversely, if it exceeds 0.06, sufficient saturation magnetization cannot be ensured. The trace additive M has a Y value of 0. 003≦Y≦0.05 is good<,
If it is less than 0.003, the heat treatment effect of the present invention will not be achieved, and if it exceeds 0.05, only the opposite effect will appear and the magnetic properties of the magnet will deteriorate.
次に第２の発明である希土類永久磁石の製造方法につい
て述べる。 本発明に係わる永久磁石の成形物は、公知
の粉末冶金法によって製造することが出来る。即ち、所
定の磁石合金組成の割合に配合した原料金属混合物をア
ルゴン雰囲気中で高周波誘導加熱により溶解し、水冷鉄
板に鋳湯してインゴットを得、このインゴットをブラウ
ンミル等の粉砕機を用いて、粗粒状に粉砕し、更にこの
粗粒をジェットミルにより微粉状に粉砕した後、１５，
０００エルステッド程度の磁界中で所定の任意形状にプ
レス成形する。Next, a method for manufacturing a rare earth permanent magnet, which is the second invention, will be described. The molded permanent magnet according to the present invention can be manufactured by a known powder metallurgy method. That is, a raw metal mixture blended to a predetermined magnet alloy composition ratio is melted by high-frequency induction heating in an argon atmosphere, cast onto a water-cooled iron plate to obtain an ingot, and this ingot is crushed using a crusher such as a Brown mill. , after pulverizing into coarse particles and further pulverizing the coarse particles into fine powder with a jet mill, 15,
It is press-molded into a predetermined arbitrary shape in a magnetic field of approximately 000 Oe.
このようにして得られた成型物は、先ず１．１００〜１
，２５０℃で填結されるが、多段階的に境結するのが好
ましく、各段階の焼結時間を合計して３０分間〜５時間
行なうのが良い。例えば、（ １，１８０℃×５０分間
）＋ （ １，２１０℃×２時間）の２段階焼結とする
。本発明の合金組成物は２段階以上の多段填結をしなけ
れば、焼結体の密度が充分でなく、また、充分な角型性
が得られないためである。焼結時間が３０分間より短い
と密度上昇が充分でなく５時間以上になると長時間とな
り実用上困難となる。The molded product obtained in this way has a particle size of 1.100 to 1.
, 250° C., but it is preferable to perform the sintering in multiple stages, and the total sintering time for each stage is preferably 30 minutes to 5 hours. For example, two-stage sintering is performed: (1,180°C x 50 minutes) + (1,210°C x 2 hours). This is because, unless the alloy composition of the present invention is subjected to multistage packing in two or more stages, the density of the sintered body will not be sufficient and sufficient squareness will not be obtained. If the sintering time is shorter than 30 minutes, the density will not increase sufficiently, and if the sintering time exceeds 5 hours, it will take a long time and will be difficult in practice.
次いで、溶体化処理に入る。その条件は１，０００〜１
，２００℃の範囲内で２０分間〜３時間処理するが、前
述の焼結時間および該溶体化時間の合計を５０分間〜８
時間以内とすることが良い。該溶体化時間が２０分間よ
り短いと溶体化効果がなく、３時間以上になると長時間
となり、実用性がなくなるからである。Next, solution treatment begins. The condition is 1,000 to 1
, 200°C for 20 minutes to 3 hours, but the total of the above-mentioned sintering time and the solution time is 50 minutes to 8 hours.
It is best to do so within an hour. This is because if the solution treatment time is shorter than 20 minutes, there will be no solution treatment effect, and if it is 3 hours or more, it will be a long time and will be impractical.
次に時効工程に入るが、時効は４００〜１，０００℃で
２回以上行なう。最初の時効は８００℃以下で１０分間
〜１０時間保持後、１℃／分以下の速度で４００℃以下
まで降下させ、引き続き２回目以降の時効は８００℃以
上でｌＯ分間〜１０時間保持後、０．５℃／分以下の速
度で１００℃以下まで降下させる。時効を２回以上行な
わないと、充分な保持力が得られず、最初の時効および
２回目以降の時効も上記の条件を満たさない場合は、本
発明の組成において充分な保持力を得ることが出来ない
。１回目時効と２回目時効で保持時間、保持速度を変え
るのは、それにより良好な角型性を持つヒステリシスカ
ーブが得られ、磁気特性が向上するためである。Next, an aging process is started, and aging is performed at 400 to 1,000°C two or more times. The first aging is held at 800°C or lower for 10 minutes to 10 hours, then lowered to 400°C or lower at a rate of 1°C/min or less, and the second and subsequent aging is held at 800°C or higher for 10 minutes to 10 hours. The temperature is lowered to 100°C or less at a rate of 0.5°C/min or less. If aging is not performed two or more times, sufficient holding power cannot be obtained, and if the first aging and subsequent aging do not satisfy the above conditions, it is not possible to obtain sufficient holding power with the composition of the present invention. Can not. The reason why the holding time and holding speed are changed between the first aging and the second aging is that a hysteresis curve with good squareness can be obtained thereby improving the magnetic properties.
以上の各工゛程は、成型物が酸化されることがないよう
に真空中またはアルゴン等の不活性ガス中で行なわれる
。以上述べた様に上記組成の成型体を各工程で熱処理す
ることによって充分な保持力と良好な角型を確保し、磁
化の温度特性に優れた希土類永久磁石材料が得られる。Each of the above steps is carried out in vacuum or in an inert gas such as argon to prevent the molded product from being oxidized. As described above, by heat-treating the molded body having the above composition in each step, it is possible to obtain a rare earth permanent magnet material that ensures sufficient holding force and good squareness, and has excellent temperature characteristics of magnetization.
以下、本発明の具体的実施態様を実施例を挙げて説明す
るが、本発明はこれらに限定されるものではない。例中
部および％は全で重量に拠る。Hereinafter, specific embodiments of the present invention will be described with reference to Examples, but the present invention is not limited thereto. All percentages and percentages are by weight.
（実施例１）
Ｓｍｏ７Ｇｄｏ． ｓ （Ｇｏ。，ＩｎＦｅｂ． ｔｏ
ｃｔｌｏ． ｏｓＺｒａ． ｏｓｓ）ｔ． ｓ上記組或
のインゴットを１気圧のＡｒ雰囲気中で高周波溶解炉を
用い、アーク溶解を行ない、磁石インゴットを作製した
。このインゴットを使い、粉末冶金法にて磁石を製造し
た。先ず、粗砕機（ジョークラッシャーおよびブラウン
ミル）を用いて粗粉砕し、この粗粉をジェットミルを用
いて窒素中で平均微粉粒径３μｍまで微粉砕した。この
微粉を磁場中配向させ、２ ｔ／ｃｍ”のプレス圧でプ
レスした。この成型体を２００ＴｏｒｒのＡｒ雰囲気中
で焼結炉を用い、１，１８０℃で３０分間、１， １８
８℃で６０分間２段焼結した後、１， １７５℃で３０
分間の溶体化処理を行なった。この後、１気圧のＡｒ雰
囲気中で７８０℃でｌ時間時効処理を行ない、１℃／分
の速度で室温まで冷却した。次に、これを再び８３０℃
で３時間時効処理を行ない、０．５℃／分の速度で室温
まで冷却し、表−１に示す磁気特性および温度特性の磁
石を得た。(Example 1) Smo7Gdo. s (Go., InFeb. to
ctlo. osZra. oss)t. s A certain ingot of the above set was subjected to arc melting in an Ar atmosphere of 1 atmosphere using a high frequency melting furnace to produce a magnet ingot. Using this ingot, a magnet was manufactured using a powder metallurgy method. First, it was coarsely crushed using a coarse crusher (jaw crusher and Braun mill), and this coarse powder was finely crushed in nitrogen using a jet mill to an average fine particle diameter of 3 μm. This fine powder was oriented in a magnetic field and pressed at a pressing pressure of 2 t/cm. This molded body was heated at 1,180°C for 30 minutes using a sintering furnace in an Ar atmosphere of 200 Torr.
After two stages of sintering at 8°C for 60 minutes, sintering was performed at 1,175°C for 30 minutes.
Solution treatment was carried out for 1 minute. Thereafter, an aging treatment was performed at 780° C. for 1 hour in an Ar atmosphere of 1 atm, followed by cooling to room temperature at a rate of 1° C./min. Next, heat this again at 830℃
The magnet was aged for 3 hours and cooled to room temperature at a rate of 0.5° C./min to obtain a magnet with the magnetic properties and temperature characteristics shown in Table 1.
（実施例２）
Ｓｌｌｏ． ｓｓＧｄｏ． ４４ （ｆｌ：ｏｏ． ｙ
＋ｓＦｅａ． ｚｏｃｕｏ． ｏｓＺｒｏ． ｏｓｓ）
７． ｔ＋この組成の合金を用いて実施例１と同様の方
法で磁石を製造した。焼結は１，１８５℃で４０分間、
１，１９２℃で５０分間、２段焼結した後、１， １８
２℃で３０分間の溶体化処理を行なった。時効はｌ回目
の時効を７９０℃で２時間行ない、１’Ｃ／分の速度で
室温まで冷却した。２段目の時効は８３０℃で３時間行
ない、０．５℃／分の速度で室温まで冷却し、表−１に
示す磁気特性および温度特性を得た。(Example 2) Sllo. ssGdo. 44 (fl:oo.y
+sFea. zocuo. osZro. oss)
7. t+ A magnet was manufactured in the same manner as in Example 1 using an alloy having this composition. Sintering was performed at 1,185℃ for 40 minutes.
After two stages of sintering at 1,192°C for 50 minutes, 1,18
Solution treatment was performed at 2°C for 30 minutes. The first aging was carried out at 790° C. for 2 hours, followed by cooling to room temperature at a rate of 1′C/min. The second stage aging was carried out at 830°C for 3 hours and cooled to room temperature at a rate of 0.5°C/min to obtain the magnetic properties and temperature characteristics shown in Table 1.
（実施例３）
実施例２と同じ組或の合金を用いて実施例１と同様の方
法で磁石を製造した。填結は１， １８３℃で２０分間
、１， １９０℃で７０分間２段填結した後、１，１８
０℃で４０分間の溶体化処理を行なった。時効処理は１
回目の時効を７８０℃で２時間行ない、１℃／分の速度
で室温まで冷却した。２回目の時効は８４０℃で２時間
行ない、０，５℃／分の速度で室温まで冷却し、表−１
に示す磁気特性および温度特性を得た。(Example 3) A magnet was manufactured in the same manner as in Example 1 using the same set of alloys as in Example 2. The packing was carried out in two stages: at 1,183°C for 20 minutes and at 1,190°C for 70 minutes, and then at 1,183°C for 70 minutes.
Solution treatment was performed at 0°C for 40 minutes. Aging treatment is 1
The second aging was carried out at 780°C for 2 hours and cooled to room temperature at a rate of 1°C/min. The second aging was carried out at 840°C for 2 hours, and then cooled to room temperature at a rate of 0.5°C/min.
The magnetic and temperature characteristics shown in are obtained.
（実施例４）
Ｓｍｏ． ｙＧｄｏ． ｓ （Ｃｏｏ． ｔ４Ｆｅｏ．
＋ｓＣｕｏ． ｏａＴＬｏ． ａｓ）ｔ． ？この組
成の合金を用いて実施例１と同様の方法で磁石を製造し
た。焼結は１，１８２℃で４０分間、１，１９２℃で８
０分間２段焼結した後、１．１７７℃で５０分間の溶体
化処理を行なった。時効処理は１回目を７６０℃で３時
間行ない、１℃／分の速度で室温まで冷却した。２回目
は８３０℃で２時間行なル）、０．５℃／分の速度で室
温まで冷却し、表−１に示す磁気特性および温度特性を
得た。(Example 4) Smo. yGdo. s (Coo. t4Feo.
+sCuo. oaTLo. as) t. ? A magnet was manufactured in the same manner as in Example 1 using an alloy having this composition. Sintering was performed at 1,182°C for 40 minutes and at 1,192°C for 8 minutes.
After sintering in two stages for 0 minutes, solution treatment was performed at 1.177°C for 50 minutes. The first aging treatment was carried out at 760°C for 3 hours, and then cooled to room temperature at a rate of 1°C/min. The second time was carried out at 830° C. for 2 hours) and then cooled to room temperature at a rate of 0.5° C./min to obtain the magnetic properties and temperature characteristics shown in Table 1.
（比較例１）
実施例２と比較するために、実施例２の組成の合金を使
用して実施例ｌと同様の方法で磁石を製造した。焼結は
１，１９０℃で２時間の１段焼結とした。時効は１段の
みで８２０℃で３時間行ない、０．５℃／分の速度で室
温まで冷却し、表−１に示す磁気特性および温度特性を
得た。これを実施例２と比較すると、角型比およびｉＨ
ｃが小さくなっているため、磁気特性および温度特性が
落ちているのが解る。(Comparative Example 1) In order to compare with Example 2, a magnet was manufactured using the alloy having the composition of Example 2 in the same manner as in Example 1. Sintering was carried out in one stage at 1,190°C for 2 hours. Aging was performed in only one stage at 820° C. for 3 hours, and cooling was performed at a rate of 0.5° C./min to room temperature to obtain the magnetic properties and temperature characteristics shown in Table 1. Comparing this with Example 2, the squareness ratio and iH
It can be seen that because c is smaller, the magnetic properties and temperature characteristics are degraded.
（比較例２）
実施例３と比較するために実施例２の組成の合金を使用
して実施例１と同様の方法で磁石を製造した。焼結は１
，１８８℃で８０分間の１回焼結とした．時効は１回の
みで８２０℃で２時間行ない、０．５℃／分の速度で室
温まで冷却し、表−１に示す磁気特性、および温度特性
を得た。これを実施例３と比較すると、角型比およびｉ
Ｈｃが小さくなっているため、磁気特性および温度特性
が落ちているのが解る。(Comparative Example 2) For comparison with Example 3, a magnet was manufactured in the same manner as in Example 1 using an alloy having the composition of Example 2. Sintering is 1
, sintering was carried out once at 188°C for 80 minutes. Aging was performed only once at 820°C for 2 hours, and cooling was performed at a rate of 0.5°C/min to room temperature to obtain the magnetic properties and temperature properties shown in Table 1. Comparing this with Example 3, the squareness ratio and i
It can be seen that the magnetic properties and temperature characteristics have deteriorated because Hc has become smaller.
（発明の効果）
本発明により，従来の組成、磁化方法では得られなかっ
た磁化の温度特性に優れ、かつ、角型性の良い希土類永
久磁石の提供が可能となり、産業上極めて利用価値が高
い。(Effect of the invention) The present invention makes it possible to provide a rare earth permanent magnet that has excellent temperature characteristics of magnetization that could not be obtained with conventional compositions and magnetization methods, and has good squareness, and has extremely high utility value in industry. .
Claims (2)
＿−＿Ｖ＿−＿ＹＦｅ＿ＵＣｕ＿ＶＭ＿Ｙ）＿Ｚ（ここ
にＲはＧｄ、Ｔｂ、Ｄｙ、Ｈｏ、Ｅｒ、Ｔｍから選ばれ
る少なくとも１種以上、ＭはＴｉ、Ｚｒ、Ｈｆ、Ｎｂ、
Ｔａ、Ｗから選ばれる少なくとも１種以上、０．２≦Ｘ
≦０．６、０．１≦Ｕ≦０．３、０．０２≦Ｖ≦０．０
６、０．００３≦Ｙ≦０．０５、６．５≦Ｚ≦８．０）
で表わされる合金組成物からなる希土類永久磁石。1. General formula Sm_1_-_XR_X(Co_1_-_U
___V_-_YFe_UCu_VM_Y)_Z (herein, R is at least one selected from Gd, Tb, Dy, Ho, Er, and Tm, and M is Ti, Zr, Hf, Nb,
At least one selected from Ta, W, 0.2≦X
≦0.6, 0.1≦U≦0.3, 0.02≦V≦0.0
6, 0.003≦Y≦0.05, 6.5≦Z≦8.0)
A rare earth permanent magnet consisting of an alloy composition represented by:
を磁界中で所定形状に圧縮成形した後、焼結、溶体化お
よび時効処理する永久磁石の製造方法において、ａ）１
，１００〜１，２５０℃の範囲内で２段階以上の多段焼
結を合計３０分間〜５時間行なった後、ｂ）１，０００
〜１，２００℃の範囲内で２０分間〜３時間溶体化処理
するが、ｃ）ａ）の焼結時間およびｂ）の溶体化時間の
合計を５０分間〜８時間内とし、次いでｄ）４００〜１
，０００℃の範囲内で２回以上の時効処理を行なうこと
を特徴とする希土類永久磁石の製造方法。2. A method for producing a permanent magnet, which comprises finely pulverizing the alloy composition according to claim 1, compression molding the fine powder into a predetermined shape in a magnetic field, and then sintering, solutionizing and aging treatment, comprising: a)1.
, 2 or more stages of multi-stage sintering within the range of 100 to 1,250°C for a total of 30 minutes to 5 hours, b) 1,000
Solution treatment is carried out within the range of ~1,200°C for 20 minutes to 3 hours, but c) the total of the sintering time in a) and the solution treatment time in b) is within 50 minutes to 8 hours, and then d) 400°C ~1
A method for producing a rare earth permanent magnet, characterized by performing aging treatment two or more times within a range of ,000°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1190168A JPH0354805A (en) | 1989-07-21 | 1989-07-21 | Rare-earth permanent magnet and manufacture thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1190168A JPH0354805A (en) | 1989-07-21 | 1989-07-21 | Rare-earth permanent magnet and manufacture thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0354805A true JPH0354805A (en) | 1991-03-08 |
Family
ID=16253568
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1190168A Pending JPH0354805A (en) | 1989-07-21 | 1989-07-21 | Rare-earth permanent magnet and manufacture thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0354805A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101882494A (en) * | 2010-05-17 | 2010-11-10 | 中国科学院宁波材料技术与工程研究所 | Samarium-cobalt sintered magnet material and preparation method thereof |
| CN103021621A (en) * | 2011-09-27 | 2013-04-03 | 株式会社东芝 | Permanent magnet and manufacturing method thereof, and motor and generator using the same |
| CN103036323A (en) * | 2011-09-29 | 2013-04-10 | 株式会社东芝 | Permanent magnet and motor and generator using the same |
| US20130241333A1 (en) * | 2010-03-30 | 2013-09-19 | Kabushiki Kaisha Toshiba | Permanent magnet and method for manufacturing the same, and motor and power generator using the same |
| CN103839639A (en) * | 2012-11-20 | 2014-06-04 | 株式会社东芝 | Permanent magnet, and motor and power generator using the same |
| JP2016157952A (en) * | 2016-03-18 | 2016-09-01 | 株式会社東芝 | Motor, generator, and motor car |
| JP2017168847A (en) * | 2017-04-04 | 2017-09-21 | 株式会社東芝 | Permanent magnet, motor, power generator, and vehicle |
| CN111243804A (en) * | 2019-11-29 | 2020-06-05 | 南京安德海睿智能科技有限公司 | Rare earth permanent magnet with hydrogen resistance and preparation method thereof |
| CN111313571A (en) * | 2019-11-29 | 2020-06-19 | 南京安德海睿智能科技有限公司 | Hydrogen-resistant motor based on rare earth permanent magnet |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57161044A (en) * | 1981-03-31 | 1982-10-04 | Shin Etsu Chem Co Ltd | Permanent magnet containing rare earth element and its manufacture |
| JPS59204208A (en) * | 1983-05-07 | 1984-11-19 | Hitachi Metals Ltd | Manufacture of rare earth cobalt magnet |
-
1989
- 1989-07-21 JP JP1190168A patent/JPH0354805A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57161044A (en) * | 1981-03-31 | 1982-10-04 | Shin Etsu Chem Co Ltd | Permanent magnet containing rare earth element and its manufacture |
| JPS59204208A (en) * | 1983-05-07 | 1984-11-19 | Hitachi Metals Ltd | Manufacture of rare earth cobalt magnet |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130241333A1 (en) * | 2010-03-30 | 2013-09-19 | Kabushiki Kaisha Toshiba | Permanent magnet and method for manufacturing the same, and motor and power generator using the same |
| US9774234B2 (en) * | 2010-03-30 | 2017-09-26 | Kabushiki Kaisha Toshiba | Permanent magnet and method for manufacturing the same, and motor and power generator using the same |
| CN101882494A (en) * | 2010-05-17 | 2010-11-10 | 中国科学院宁波材料技术与工程研究所 | Samarium-cobalt sintered magnet material and preparation method thereof |
| CN103021621A (en) * | 2011-09-27 | 2013-04-03 | 株式会社东芝 | Permanent magnet and manufacturing method thereof, and motor and generator using the same |
| JP2013074235A (en) * | 2011-09-29 | 2013-04-22 | Toshiba Corp | Permanent magnet, and motor and dynamo including the same |
| CN103036323A (en) * | 2011-09-29 | 2013-04-10 | 株式会社东芝 | Permanent magnet and motor and generator using the same |
| CN103839639A (en) * | 2012-11-20 | 2014-06-04 | 株式会社东芝 | Permanent magnet, and motor and power generator using the same |
| CN103839639B (en) * | 2012-11-20 | 2017-01-04 | 株式会社东芝 | Permanent magnet and use motor and the electromotor of this permanent magnet |
| JP2016157952A (en) * | 2016-03-18 | 2016-09-01 | 株式会社東芝 | Motor, generator, and motor car |
| JP2017168847A (en) * | 2017-04-04 | 2017-09-21 | 株式会社東芝 | Permanent magnet, motor, power generator, and vehicle |
| CN111243804A (en) * | 2019-11-29 | 2020-06-05 | 南京安德海睿智能科技有限公司 | Rare earth permanent magnet with hydrogen resistance and preparation method thereof |
| CN111313571A (en) * | 2019-11-29 | 2020-06-19 | 南京安德海睿智能科技有限公司 | Hydrogen-resistant motor based on rare earth permanent magnet |
| CN111243804B (en) * | 2019-11-29 | 2023-10-17 | 南京安德海睿智能科技有限公司 | Rare earth permanent magnet with hydrogen resistance and preparation method thereof |
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