JP2006299402A5 - - Google Patents
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- JP2006299402A5 JP2006299402A5 JP2006020062A JP2006020062A JP2006299402A5 JP 2006299402 A5 JP2006299402 A5 JP 2006299402A5 JP 2006020062 A JP2006020062 A JP 2006020062A JP 2006020062 A JP2006020062 A JP 2006020062A JP 2006299402 A5 JP2006299402 A5 JP 2006299402A5
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- 239000000956 alloy Substances 0.000 claims description 41
- 229910045601 alloy Inorganic materials 0.000 claims description 41
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical class [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 claims description 40
- 239000002994 raw material Substances 0.000 claims description 30
- 238000005245 sintering Methods 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000005266 casting Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- 229910052803 cobalt Inorganic materials 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 229910052723 transition metal Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 description 13
- 239000002184 metal Substances 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- -1 rare earth alloy Chemical class 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 210000001519 tissues Anatomy 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000003247 decreasing Effects 0.000 description 1
- 230000004059 degradation Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
Description
ストリップキャスト法による原料合金の組織を均一にするためには、ストリップキャスト法で作製される薄帯がより均一に冷却される必要がある。つまり、ロールに供給される溶湯の厚さが厚ければ、その厚さ方向における冷却能が相違して、均一な冷却、換言すれば均一な組織を得ることが容易でなくなる。溶湯をより薄くしてロールに供給するために、溶湯状態の合金の粘度が重要と考えた。つまり、溶湯の粘度が低ければロールに供給される合金を薄くすることが可能となり、その結果として組織の均一なストリップキャストによる原料合金を提供することができる。そして、溶湯の粘度低下のためには、Ｐ（燐）及びＳ（硫黄）が有効である。そしてさらに、Ｐ（燐）及びＳ（硫黄）は、原料合金の時点で相当量含有していても、焼結の過程で磁気特性に悪影響を与えない程度に減少できることが判明した。このように、Ｐ及びＳは、本発明の目的達成にとって有効な元素である。 In order to make the structure of the raw material alloy uniform by the strip casting method, the ribbon produced by the strip casting method needs to be cooled more uniformly. That is, if the thickness of the molten metal supplied to the roll is large, the cooling ability in the thickness direction is different, so that it is not easy to obtain uniform cooling, in other words, a uniform structure. In order to make the molten metal thinner and supply it to the roll, the viscosity of the molten alloy was considered important. That is, when the viscosity of the molten metal is low, the alloy supplied to the roll can be made thin, and as a result, a raw material alloy by strip casting having a uniform structure can be provided. And P (phosphorus) and S (sulfur) are effective for the viscosity fall of a molten metal. Further, it has been found that even if P (phosphorus) and S (sulfur) are contained in a considerable amount at the time of the raw material alloy, they can be reduced to such an extent that the magnetic properties are not adversely affected during the sintering process. Thus, P及Beauty S is an element effective for achievement of the object of the present invention.
すなわち本発明のＲ−Ｔ−Ｂ系焼結磁石用原料合金（以下、単に原料合金）は、Ｒ２Ｔ１４Ｂ化合物からなる結晶粒を有し、Ｐ及びＳの含有量が１００〜９５０ｐｐｍであることを特徴としている。ここで、Ｒは希土類元素から選択される１種又は２種以上の元素、ＴはＦｅ又はＦｅ及びＣｏを含む遷移金属元素から選択される１種又は２種以上の元素である。なお、Ｒ及びＴの内訳は以下も同様とする。
本発明の原料合金において、Ｐ及びＳの含有量は２００〜７５０ｐｐｍであること、さらに３００〜７００ｐｐｍであることが好ましい。
本発明の原料合金において、Ｒ：２５〜３５ｗｔ％、Ｂ：０．５〜４ｗｔ％、Ａｌ及びＣｕの１種又は２種を０．０２〜０．６ｗｔ％、Ｃｏ：５ｗｔ％以下、残部Ｆｅ及び不可避的不純物からなる組成とすることが好ましい。また、この組成にさらにＺｒ、Ｎｂ及びＨｆの１種又は２種以上：２ｗｔ％以下を含有させることも好ましい。
That R-T-B based sintered magnet material alloy of the present invention (hereinafter, simply starting alloy) has a crystal grain consisting of R 2 T 14 B compound, 100～950Ppm P content及beauty S It is characterized by being. Here, R is one or more elements selected from rare earth elements, and T is one or more elements selected from transition metal elements including Fe or Fe and Co. The breakdown of R and T is the same in the following.
In the raw material alloy of the present invention, the content of P及beauty S it is 200～750Ppm, is preferably further 300～700Ppm.
In the raw material alloy of the present invention, R: 25 to 35 wt%, B: 0.5 to 4 wt%, one or two of Al and Cu are 0.02 to 0.6 wt%, Co: 5 wt% or less, and the balance is Fe And a composition comprising inevitable impurities. Moreover, it is also preferable that this composition further contains one or more of Zr, Nb and Hf: 2 wt% or less.
本発明によるＲ−Ｔ−Ｂ系焼結磁石は、Ｒ２Ｔ１４Ｂ化合物からなる結晶粒を主相とする焼結体からなり、この焼結体中にＰ及びＳが１０〜２２０ｐｐｍ含有することを特徴とする。焼結体中に含有されるＰ及びＳは、５０〜２００ｐｐｍであることが好ましく、５０〜１８０ｐｐｍであることがさらに好ましい。
本発明によるＲ−Ｔ−Ｂ系焼結磁石の組成は、基本的には、原料合金と同様となるが、焼結体中に含有されるＯ（酸素）は、３０００ｐｐｍ以下であることが高い磁気特性を得る上で好ましい。Ｏを３０００ｐｐｍ以下とする場合には、Ｚｒ、Ｎｂ及びＨｆの１種又は２種以上：２ｗｔ％以下を含有させることが好ましい。
R-T-B based sintered magnet according to the present invention comprises crystal grains composed of R 2 T 14 B compound sintered body as a main phase, P及Beauty S in the sintered body containing 10~220ppm It is characterized by doing. P及beauty S contained in the sintered body is preferably from 50 to 200 ppm, more preferably from 50～180Ppm.
The composition of the RTB-based sintered magnet according to the present invention is basically the same as that of the raw material alloy, but O (oxygen) contained in the sintered body is preferably 3000 ppm or less. It is preferable for obtaining magnetic characteristics. When O is 3000 ppm or less, it is preferable to contain one or more of Zr, Nb, and Hf: 2 wt% or less.
以上の本発明の原料合金を用いることにより、Ｒ２Ｔ１４Ｂ化合物からなる結晶粒を主相とする焼結体からなるＲ−Ｔ−Ｂ系焼結磁石の製造方法であって、Ｐ及びＳの含有量が１００〜９５０ｐｐｍであって、かつストリップキャスト法により作製された原料合金を所定粒度の粉末まで粉砕する工程と、得られた粉末を磁場中で成形して成形体を作製する工程と、この成形体を焼結することによりＰ及びＳの含有量が１０〜２２０ｐｐｍの焼結体を得る工程と、を備えるＲ−Ｔ−Ｂ系焼結磁石の製造方法が提供される。
このＲ−Ｔ−Ｂ系焼結磁石において、原料合金における好ましいＰ及びＳの含有量、焼結体における好ましいＰ及びＳの含有量は、上述の通りである。また、焼結体中に含有されるＯ（酸素）は、３０００ｐｐｍ以下であることが高い磁気特性を得る上で好ましいことも同様である。
By using the raw material alloy of the present invention as described above, there is provided a method for producing an RTB-based sintered magnet comprising a sintered body having a crystal phase comprising an R 2 T 14 B compound as a main phase, comprising P and And a step of pulverizing the raw material alloy produced by the strip casting method to a powder having a predetermined particle size, and molding the obtained powder in a magnetic field to produce a compact. and method of manufacturing an R-T-B based sintered magnet is provided comprising the steps of: the content of P及beauty S to obtain a sintered body of 10～220Ppm, a by sintering the molded body .
In this R-T-B based sintered magnet, the content of the preferred P及beauty S in the raw material alloy, the content of the preferred P及beauty S in the sintered body is as described above. Similarly, O (oxygen) contained in the sintered body is preferably 3000 ppm or less in order to obtain high magnetic properties.
本発明によれば、ストリップキャストによる原料合金に含有されるＰ及びＳの量を１００〜９５０ｐｐｍとすることにより、当該原料合金の組織が均一かつ微細になり、ひいては磁場中成形の対象となる微粉砕粉を微細かつシャープな粒度分布とすることができる。その結果として、得られるＲ−Ｔ−Ｂ系焼結磁石の磁気特性、特に保磁力を向上することができる。また、Ｐ及びＳは、焼結によりその含有量が減少して１０〜２２０ｐｐｍとなり、高い残留磁束密度を得ることもできる。 According to the present invention, by making the amount of P及beauty S contained in the raw material alloy according to a strip casting and 100～950Ppm, tissue of the material alloy is uniform and fine, is subject to turn the magnetic field during the molding Finely pulverized powder can have a fine and sharp particle size distribution. As a result, the magnetic properties, particularly the coercive force, of the obtained RTB-based sintered magnet can be improved. Further, the content of P and S decreases by sintering to 10 to 220 ppm, and a high residual magnetic flux density can be obtained.
本発明による原料合金は、Ｒ２Ｔ１４Ｂ化合物からなる結晶粒を有し、Ｐ及びＳの含有量が１００〜９５０ｐｐｍである。本発明においてＰ及びＳは、溶湯の粘度を低下させることにより得られる原料合金の組織を均一かつ微細にする効果を奏する。そのため、その後の微粉砕で得られる微粉砕粉の粒径が小さく、かつ粒度分布がシャープとなる。この結果、この微粉砕粉を用いて得られたＲ−Ｔ−Ｂ系焼結磁石の磁気特性、特に保磁力を増大させ、またＲ−Ｔ−Ｂ系焼結磁石の保磁力のばらつきを抑えることができる。 Material alloy according to the present invention has a crystal grain consisting of R 2 T 14 B compound, the content of P及beauty S is 100～950Ppm. P及beauty S in the present invention exhibits tissue uniform and effective to refine the raw material alloy obtained by reducing the viscosity of the molten metal. Therefore, the finely pulverized powder obtained by subsequent fine pulverization has a small particle size and a sharp particle size distribution. As a result, the magnetic properties of the RTB-based sintered magnet obtained using this finely pulverized powder, particularly the coercive force, is increased, and variations in the coercive force of the RTB-based sintered magnet are suppressed. be able to.
本発明において、原料合金のＰ及びＳの含有量が１００ｐｐｍ未満では溶湯の粘度低下の効果が十分に発揮されないために保磁力向上の効果を得ることができない。一方、Ｐ及びＳの含有量が多くなりすぎると原料合金の組織が微細になりすぎて、微粉砕後の粒径がそれに応じたものとなる。その結果、磁場中成形時の配向が不十分となり、残留磁束密度劣化が懸念される。したがって、本発明の原料合金はＰ及びＳの含有量を１００〜９５０ｐｐｍとする。原料合金に含まれるＰ及びＳの好ましい含有量は２００〜７５０ｐｐｍ、さらに好ましい含有量は３００〜７００ｐｐｍである。 In the present invention, the content of P及beauty S material alloy can not be obtained an effect of improving the coercive force in order to effect a viscosity reduction of the molten metal is not sufficiently exhibited less than 100 ppm. On the other hand, too the organization of P及beauty content number becomes too the material alloy of S fine, and that particle size after milling is accordingly. As a result, the orientation during molding in a magnetic field becomes insufficient, and there is a concern about residual magnetic flux density degradation. Therefore, the raw material alloy of the present invention is to 100~950ppm content of P及beauty S. The preferred content of P及beauty S contained in the raw material alloy 200～750Ppm, more preferred content is 300～700Ppm.
本発明の原料合金を用いて作製されるＲ−Ｔ−Ｂ系焼結磁石は、Ｒ２Ｔ１４Ｂ化合物からなる結晶粒を主相とし、その他に粒界相を備えている。この粒界相は、主相よりもＮｄ量がリッチであるためにＮｄリッチ相と呼ばれる相、ＢがリッチであるためにＢリッチ相と呼ばれる相、Ｒと酸素との化合物からなる酸化物相等のいくつかの相を含んでいる。そして、本発明の原料合金を用いて作製されるＲ−Ｔ−Ｂ系焼結磁石は、Ｐ及びＳを１０〜２２０ｐｐｍ含有することが好ましい。前述したように、原料合金に含まれるＰ及びＳは焼結により減少するものの、原料合金において１００ｐｐｍ以上含有していると焼結体のＰ及びＳを１０ｐｐｍ未満に減少することは困難である。一方、Ｒ−Ｔ−Ｂ系焼結磁石において２２０ｐｐｍを超えるＰ及びＳを含有していると残留磁束密度の低下が著しい。好ましいＲ−Ｔ−Ｂ系焼結磁石におけるＰ及びＳの含有量は５０〜２００ｐｐｍ、より好ましいＲ−Ｔ−Ｂ系焼結磁石におけるＰ及びＳの含有量は５０〜１８０ｐｐｍである。 The RTB-based sintered magnet produced using the raw material alloy of the present invention has crystal grains made of the R 2 T 14 B compound as a main phase and additionally has a grain boundary phase. This grain boundary phase includes a phase called an Nd-rich phase because the amount of Nd is richer than the main phase, a phase called a B-rich phase because B is rich, an oxide phase composed of a compound of R and oxygen, etc. Contains several phases. Then, R-T-B based sintered magnet prepared using a raw material alloy of the present invention preferably contains 10~220ppm the P及beauty S. As described above, P及beauty S contained in the raw material alloy although decreased by sintering, reducing the P及beauty S of a sintered body containing more than 100ppm in material alloy to less than 10ppm is difficult is there. On the other hand, lowering of the residual magnetic flux density contains a P及beauty S exceeding 220ppm in the R-T-B based sintered magnet is remarkable. The content of P及beauty S in the preferred R-T-B based sintered magnet 50 to 200 ppm, the content of P及beauty S in a more preferred R-T-B based sintered magnet is 50～180Ppm.
次に、本発明による原料合金を用いたＲ−Ｔ−Ｂ系焼結磁石の製造方法の好ましい形態について説明する。
原料金属を真空又は不活性ガス、好ましくはＡｒ雰囲気中でストリップキャスティングすることにより、原料合金を得ることができる。原料合金を得るための原料金属としては、希土類金属あるいは希土類合金、純鉄、フェロボロン、さらにはこれらの合金等を使用することができる。この際、得られる原料合金のＰ及びＳの含有量が１００〜９５０ｐｐｍとなるように原料金属を選定する必要がある。Ｐ及びＳは、原料金属、例えば純鉄中に不純物として含有される元素であるため、原料金属の不純物レベルを選定することにより本発明の原料合金を得ることができる。原料金属の不純物レベルを選定することなく、適宜、Ｐ及びＳを添加することにより本発明のＰ及びＳの含有量を得ることもできる。要するに、溶湯として必要な量のＰ及びＳを含有していればよい。
Next, the preferable form of the manufacturing method of the RTB type | system | group sintered magnet using the raw material alloy by this invention is demonstrated.
A raw material alloy can be obtained by strip casting the raw metal in a vacuum or an inert gas, preferably in an Ar atmosphere. As a raw material metal for obtaining a raw material alloy, a rare earth metal or a rare earth alloy, pure iron, ferroboron, or an alloy thereof can be used. In this case, it is necessary the content of P及beauty S of the resulting material alloy is selected raw material metal so that 100～950Ppm. P及beauty S, since the raw material metal is an element contained as an impurity, for example, in pure iron, can be obtained raw material alloy of the present invention by selecting the impurity level of the raw material metal. Without selecting the impurity level of the raw material metal, suitably, it is possible to obtain the content of P及beauty S of the present invention by the addition of P及beauty S. In short, it is sufficient to contain the P及beauty S required amount of a molten metal.
磁場中成形後、その成形体を真空又は不活性ガス雰囲気中で焼結する。焼結温度は、組成、粉砕方法、粒度と粒度分布の違い等、諸条件により調整する必要があるが、１０００〜１２００℃で１〜１０時間程度焼結すればよい。この焼結工程で原料合金に含まれていたＰ及びＳは低減する。この低減する量の制御は明らかでないところがあるが、焼結温度が高いほど、また焼結時間が長いほど、Ｐ及びＳの低減量が増える傾向にあることを確認している。
焼結後、得られた焼結体に時効処理を施すことができる。時効処理は、保磁力を制御する上で重要である。時効処理を２段に分けて行なう場合には、８００〜９００℃近傍、６００〜７００℃近傍での所定時間の保持が有効である。
After molding in a magnetic field, the compact is sintered in a vacuum or an inert gas atmosphere. Although it is necessary to adjust sintering temperature by various conditions, such as a composition, a grinding | pulverization method, a particle size, and a particle size distribution difference, what is necessary is just to sinter at 1000-1200 degreeC for about 1 to 10 hours. The P及beauty S contained in the raw material alloy in the sintering process is reduced. Although control of the amount of this reduction there is something not clear, it has been confirmed that the sintering temperature is higher, also the longer the sintering time tends to reduce the amount of P及beauty S increases.
After sintering, the obtained sintered body can be subjected to an aging treatment. The aging treatment is important for controlling the coercive force. In the case where the aging treatment is performed in two stages, it is effective to maintain a predetermined time in the vicinity of 800 to 900 ° C. and in the vicinity of 600 to 700 ° C.
Claims (10)
Ｐ及びＳの含有量が１００〜９５０ｐｐｍであることを特徴とするＲ−Ｔ−Ｂ系焼結磁石用原料合金。
ただし、Ｒは希土類元素から選択される１種又は２種以上の元素、ＴはＦｅ又はＦｅ及びＣｏを含む遷移金属元素から選択される１種又は２種以上の元素である。 Having crystal grains made of R 2 T 14 B compound,
P及beauty S R-T-B based sintered magnet material alloy that content is characterized by a 100~950ppm of.
Here, R is one or more elements selected from rare earth elements, and T is one or more elements selected from transition metal elements including Fe or Fe and Co.
前記粉末を磁場中で成形して成形体を作製し、
前記成形体を焼結して得られる焼結体を有するＲ−Ｔ−Ｂ系焼結磁石であり、
前記焼結体は、Ｒ２Ｔ１４Ｂ化合物からなる結晶粒を主相とし、
前記焼結体中にＰ及びＳが１０〜２２０ｐｐｍ含有することを特徴とするＲ−Ｔ−Ｂ系焼結磁石。
ただし、Ｒは希土類元素から選択される１種又は２種以上の元素、ＴはＦｅ又はＦｅ及びＣｏを含む遷移金属元素から選択される１種又は２種以上の元素である。 Grinding the raw material alloy according to any one of claims 1 to 4 to a powder of a predetermined particle size,
Molding the powder in a magnetic field to produce a molded body,
An RTB-based sintered magnet having a sintered body obtained by sintering the molded body;
The sintered body, the crystal grains composed of R 2 T 14 B compound as a main phase,
R-T-B based sintered magnet, characterized in that P及beauty S contains 10~220ppm in the sintered body.
Here, R is one or more elements selected from rare earth elements, and T is one or more elements selected from transition metal elements including Fe or Fe and Co.
ストリップキャスト法により作製された請求項１〜４のいずれかに記載の原料合金を所定粒度の粉末まで粉砕する工程と、
前記粉末を磁場中で成形して成形体を作製する工程と、
前記成形体を焼結することによりＰ及びＳの含有量が１０〜２２０ｐｐｍの前記焼結体を得る工程と、
を備えることを特徴とするＲ−Ｔ−Ｂ系焼結磁石の製造方法。
ただし、Ｒは希土類元素から選択される１種又は２種以上の元素、ＴはＦｅ又はＦｅ及びＣｏを含む遷移金属元素から選択される１種又は２種以上の元素である。 A method for producing an RTB-based sintered magnet comprising a sintered body having a crystal phase comprising an R 2 T 14 B compound as a main phase ,
A step of pulverizing the raw material alloy according to any one of claims 1 to 4 produced by a strip casting method to a powder having a predetermined particle size;
Forming the powder in a magnetic field to produce a molded body;
A step in which the content of P及beauty S to obtain the sintered body of 10~220ppm by sintering the molded body,
The manufacturing method of the RTB system sintered magnet characterized by including these.
Here, R is one or more elements selected from rare earth elements, and T is one or more elements selected from transition metal elements including Fe or Fe and Co.
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| JP2006020062A JP4753024B2 (en) | 2005-03-24 | 2006-01-30 | Raw material alloy for RTB-based sintered magnet, RTB-based sintered magnet, and manufacturing method thereof |
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| JP2005086100 | 2005-03-24 | ||
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| JP2006020062A JP4753024B2 (en) | 2005-03-24 | 2006-01-30 | Raw material alloy for RTB-based sintered magnet, RTB-based sintered magnet, and manufacturing method thereof |
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| JP2006299402A JP2006299402A (en) | 2006-11-02 |
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| CN103377820B (en) | 2013-07-17 | 2015-11-25 | 烟台首钢磁性材料股份有限公司 | A kind of R-T-B-M based sintered magnet and manufacture method thereof |
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| JP4332982B2 (en) * | 2000-03-24 | 2009-09-16 | 日立金属株式会社 | Manufacturing method of iron-based alloy magnet |
| JP2002161302A (en) * | 2000-09-18 | 2002-06-04 | Sumitomo Special Metals Co Ltd | Alloyed magnetic powder for permanent magnet and manufacturing method for the same |
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