JP2007053351A - Rare earth permanent magnet, its manufacturing method, and permanent magnet rotary machine - Google Patents
Rare earth permanent magnet, its manufacturing method, and permanent magnet rotary machine Download PDFInfo
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本発明は、焼結磁石体の残留磁束密度の低減を抑制しながら保磁力を増大させたＲ−Ｆｅ−Ｂ系希土類永久磁石、及びその製造方法、並びに高速回転を行う電気自動車用モータや発電機、ＦＡモータ等に最適な永久磁石回転機に関する。 The present invention relates to an R-Fe-B rare earth permanent magnet having an increased coercive force while suppressing a reduction in residual magnetic flux density of a sintered magnet body, a method for manufacturing the same, a motor for electric vehicles that performs high-speed rotation, and power generation. The present invention relates to a permanent magnet rotating machine suitable for a machine, FA motor and the like.
Ｎｄ−Ｆｅ−Ｂ系永久磁石は、その優れた磁気特性のために、ますます用途が広がってきている。近年、モータや発電機などの回転機の分野においても、機器の軽量短小化、高性能化、省エネルギー化に伴い、Ｎｄ−Ｆｅ−Ｂ系永久磁石を利用した永久磁石回転機が開発されている。回転機中の永久磁石は、巻き線や鉄心の発熱により高温に曝され、更に巻き線からの反磁界により極めて減磁しやすい状況下にある。このため、耐熱性、耐減磁性の指標となる保磁力が一定以上あり、磁力の大きさの指標となる残留磁束密度ができるだけ高いＮｄ−Ｆｅ−Ｂ系焼結磁石が要求されている。 Nd-Fe-B permanent magnets are increasingly used because of their excellent magnetic properties. In recent years, in the field of rotating machines such as motors and generators, permanent magnet rotating machines using Nd-Fe-B permanent magnets have been developed along with reductions in weight, size, performance, and energy saving of equipment. . The permanent magnet in the rotating machine is exposed to a high temperature due to the heat generated by the winding and the iron core, and is in a state where it is very easily demagnetized by the demagnetizing field from the winding. For this reason, there is a demand for Nd—Fe—B sintered magnets that have a coercive force that is an index of heat resistance and demagnetization resistance at a certain level and that has as high a residual magnetic flux density as possible that is an index of the magnitude of magnetic force.
Ｎｄ−Ｆｅ−Ｂ系焼結磁石の残留磁束密度増大は、Ｎｄ2Ｆｅ14Ｂ化合物の体積率増大と結晶配向度向上により達成され、これまでに種々のプロセスの改善が行われてきている。保磁力の増大に関しては、結晶粒の微細化を図る、Ｎｄ量を増やした組成合金を用いる、あるいは効果のある元素を添加する等、様々なアプローチがある中で、現在最も一般的な手法はＤｙやＴｂでＮｄの一部を置換した組成合金を用いることである。Ｎｄ2Ｆｅ14Ｂ化合物のＮｄをこれらの元素で置換することで、化合物の異方性磁界が増大し、保磁力も増大する。一方で、ＤｙやＴｂによる置換は化合物の飽和磁気分極を減少させる。従って、上記手法で保磁力の増大を図る限りでは残留磁束密度の低下は避けられない。 The increase in the residual magnetic flux density of the Nd—Fe—B based sintered magnet has been achieved by increasing the volume fraction of the Nd 2 Fe 14 B compound and improving the degree of crystal orientation, and various processes have been improved so far. Regarding the increase in coercive force, among the various approaches such as refinement of crystal grains, use of a composition alloy with an increased Nd amount, or addition of an effective element, the most common method at present is A composition alloy in which a part of Nd is substituted with Dy or Tb is used. By substituting Nd of the Nd 2 Fe 14 B compound with these elements, the anisotropic magnetic field of the compound increases and the coercive force also increases. On the other hand, substitution with Dy or Tb reduces the saturation magnetic polarization of the compound. Therefore, as long as the coercive force is increased by the above method, a decrease in residual magnetic flux density is inevitable.
Ｎｄ−Ｆｅ−Ｂ系焼結磁石は、結晶粒界面で逆磁区の核が生成する外部磁界の大きさが保磁力となる。逆磁区の核生成には結晶粒界面の構造が強く影響しており、界面近傍における結晶構造の乱れが磁気的な構造の乱れを招き、逆磁区の生成を助長する。一般的には、結晶界面から５ｎｍ程度の深さまでの磁気的構造が保磁力の増大に寄与していると考えられている（非特許文献１：Ｋ． −Ｄ． Ｄｕｒｓｔ ａｎｄ Ｈ． Ｋｒｏｎｍｕｌｌｅｒ， “ＴＨＥ ＣＯＥＲＣＩＶＥ ＦＩＥＬＤ ＯＦ ＳＩＮＴＥＲＥＤ ＡＮＤ ＭＥＬＴ−ＳＰＵＮ ＮｄＦｅＢ ＭＡＧＮＥＴＳ”， Ｊｏｕｒｎａｌ ｏｆ Ｍａｇｎｅｔｉｓｍ ａｎｄ Ｍａｇｎｅｔｉｃ Ｍａｔｅｒｉａｌｓ ６８ （１９８７） ６３−７５）。本発明者らは、結晶粒の界面近傍のみにわずかなＤｙやＴｂを濃化させ、界面近傍のみの異方性磁界を増大させることで、残留磁束密度の低下を抑制しつつ保磁力を増大できることを見出している（特許文献１：特公平５−３１８０７号公報）。更に、Ｎｄ2Ｆｅ14Ｂ化合物組成合金と、ＤｙあるいはＴｂに富む合金を別に作製した後に混合して焼結する製造方法を確立している（特許文献２：特開平５−２１２１８号公報）。この方法では、ＤｙあるいはＴｂに富む合金は焼結時に液相となり、Ｎｄ2Ｆｅ14Ｂ化合物を取り囲むように分布する。その結果、化合物の粒界近傍でのみＮｄとＤｙあるいはＴｂが置換され、残留磁束密度の低下を抑制しつつ効果的に保磁力を増大できる。 In the Nd—Fe—B based sintered magnet, the coercive force is the magnitude of the external magnetic field generated by the nucleus of the reverse magnetic domain at the crystal grain interface. The structure of the crystal grain interface strongly influences the nucleation of the reverse magnetic domain, and the disorder of the crystal structure in the vicinity of the interface causes the disorder of the magnetic structure and promotes the generation of the reverse magnetic domain. In general, it is considered that a magnetic structure from a crystal interface to a depth of about 5 nm contributes to an increase in coercive force (Non-Patent Document 1: K.-D. Durst and H. Kronmuller, “ THE COERCIVE FIELD OF SINTERED AND MELT-SPUN NdFeB MAGNETS ", Journal of Magnetics and Magnetic Materials 68 (1987) 63-75). The present inventors concentrated a small amount of Dy and Tb only in the vicinity of the crystal grain interface, and increased the anisotropy magnetic field only in the vicinity of the interface, thereby increasing the coercive force while suppressing the decrease in the residual magnetic flux density. (Patent Document 1: Japanese Patent Publication No. 5-31807). Furthermore, a manufacturing method has been established in which an Nd 2 Fe 14 B compound composition alloy and an alloy rich in Dy or Tb are separately manufactured and then mixed and sintered (Patent Document 2: JP-A-5-21218). In this method, an alloy rich in Dy or Tb becomes a liquid phase during sintering and is distributed so as to surround the Nd 2 Fe 14 B compound. As a result, Nd and Dy or Tb are replaced only near the grain boundary of the compound, and the coercive force can be effectively increased while suppressing a decrease in the residual magnetic flux density.
しかし、上記方法では２種の合金微粉末を混合した状態で１，０００〜１，１００℃という高温で焼結するために、ＤｙあるいはＴｂがＮｄ2Ｆｅ14Ｂ結晶粒の界面のみでなく内部まで拡散しやすい。実際に得られる磁石の組織観察からは結晶粒界表層部で界面から深さ１〜２μｍ程度まで拡散しており、拡散した領域を体積分率に換算すると６０％以上となる。また、結晶粒内への拡散距離が長くなるほど界面近傍におけるＤｙあるいはＴｂの濃度は低下してしまう。結晶粒内への過度な拡散を極力抑えるには焼結温度を低下させることが有効であるが、これは同時に焼結による緻密化を阻害するため現実的な手法となり得ない。ホットプレスなどで応力を印加しながら低温で焼結する方法では、緻密化は可能であるが、生産性が極端に低くなるという問題がある。 However, in the above method, since two kinds of alloy fine powders are mixed and sintered at a high temperature of 1,000 to 1,100 ° C., Dy or Tb is not only the interface of Nd 2 Fe 14 B crystal grains but also the inside. Easy to diffuse. From the observation of the structure of the actually obtained magnet, it is diffused from the interface to a depth of about 1 to 2 μm at the grain boundary surface layer portion, and when the diffused region is converted into a volume fraction, it becomes 60% or more. Further, the longer the diffusion distance into the crystal grain, the lower the concentration of Dy or Tb in the vicinity of the interface. Although it is effective to lower the sintering temperature in order to suppress excessive diffusion into the crystal grains as much as possible, this cannot be a practical method because it simultaneously inhibits densification by sintering. In the method of sintering at a low temperature while applying stress by hot pressing or the like, densification is possible, but there is a problem that productivity becomes extremely low.
一方、焼結磁石を小型に加工した後、磁石表面にＤｙやＴｂをスパッタによって被着させ、磁石を焼結温度より低い温度で熱処理することにより粒界部にのみＤｙやＴｂを拡散させて保磁力を増大させる方法が報告されている（非特許文献２：Ｋ． Ｔ． Ｐａｒｋ， Ｋ． Ｈｉｒａｇａ ａｎｄ Ｍ． Ｓａｇａｗａ， “Ｅｆｆｅｃｔ ｏｆ Ｍｅｔａｌ−Ｃｏａｔｉｎｇ ａｎｄ Ｃｏｎｓｅｃｕｔｉｖｅ Ｈｅａｔ Ｔｒｅａｔｍｅｎｔ ｏｎ Ｃｏｅｒｃｉｖｉｔｙ ｏｆ Ｔｈｉｎ Ｎｄ−Ｆｅ−Ｂ Ｓｉｎｔｅｒｅｄ Ｍａｇｎｅｔｓ”， Ｐｒｏｃｅｅｄｉｎｇｓ ｏｆ ｔｈｅ Ｓｉｘｔｅｅｎ Ｉｎｔｅｒｎａｔｉｏｎａｌ Ｗｏｒｋｓｈｏｐ ｏｎ Ｒａｒｅ−Ｅａｒｔｈ Ｍａｇｎｅｔｓ ａｎｄ Ｔｈｅｉｒ Ａｐｐｌｉｃａｔｉｏｎｓ， Ｓｅｎｄａｉ， ｐ．２５７ （２０００）、非特許文献３：町田憲一、川嵜尚志、鈴木俊治、伊東正浩、堀川高志、“Ｎｄ−Ｆｅ−Ｂ系焼結磁石の粒界改質と磁気特性”、粉体粉末冶金協会講演概要集 平成１６年度春季大会、ｐ．２０２参照）。この方法では、更に効率的にＤｙやＴｂを粒界に濃化できるため、残留磁束密度の低下をほとんど伴わずに保磁力を増大させることが可能である。また、磁石の比表面積が大きい、即ち磁石体が小さいほど供給されるＤｙやＴｂの量が多くなるので、この方法は小型あるいは薄型の磁石へのみ適用可能である。しかし、スパッタ等による金属膜の被着には生産性が悪いという問題があった。 On the other hand, after processing the sintered magnet to a small size, Dy and Tb are deposited on the magnet surface by sputtering, and the magnet is heat-treated at a temperature lower than the sintering temperature to diffuse Dy and Tb only at the grain boundary part. A method for increasing the coercive force has been reported (Non-Patent Document 2: K. T. Park, K. Hiraga and M. Sagawa, "Effect of Metal-Coating and Conscientious Heat Treatment on Co-Circency of T Sintered Magnets ", Proceedings of the Sixteen International Works on Rare-Earth Magnets and Ther Application , Sendai, p. 257 (2000), Non-Patent Document 3: Kenichi Machida, Naoshi Kawamata, Toshiharu Suzuki, Masahiro Ito, Takashi Horikawa, “Granular boundary modification and magnetic properties of Nd—Fe—B based sintered magnet”, Summary of Powder and Powder Metallurgy Association, 2004 Spring Meeting, p. 202). In this method, since Dy and Tb can be concentrated more efficiently at the grain boundary, the coercive force can be increased with almost no decrease in the residual magnetic flux density. Moreover, since the amount of Dy and Tb supplied increases as the specific surface area of the magnet increases, that is, the magnet body decreases, this method is applicable only to small or thin magnets. However, there has been a problem that the productivity is poor when depositing a metal film by sputtering or the like.
また、近年１０ｋＷ以上の大容量の回転機にもＮｄ−Ｆｅ−Ｂ系焼結磁石が使用されるようになった。Ｎｄ−Ｆｅ−Ｂ系焼結磁石の電気抵抗は１００〜２００μΩ・ｃｍの導体であり、磁石に生じる渦電流やそれに伴う発熱が、磁石の大きさの２乗で大きくなるために大容量回転機においては問題となっている。渦電流低減のために有効な手段は、鉄心に使われる電磁鋼板のように薄板化して絶縁積層することであるが、細分化したセグメント磁石を接着固化して所要の大きさの磁石とする方法は、磁石の製造工程が増加し、製造コストの増加や磁石重量歩留まりの低下を招く。また、セグメント磁石を接着固化せず小磁石のまま用いることも考えられるが、磁石間の反発力に抗して小磁石をロータに組込み固着することは難しい。 In recent years, Nd—Fe—B based sintered magnets have also been used in large capacity rotating machines of 10 kW or more. The Nd-Fe-B sintered magnet has a resistance of 100 to 200 μΩ · cm, and the eddy current generated in the magnet and the accompanying heat generation increase with the square of the size of the magnet. Is a problem. An effective means for reducing eddy currents is to thin and insulate and laminate like a magnetic steel sheet used for iron cores, but a method of bonding and solidifying segmented segment magnets into a magnet of the required size. Increases the manufacturing process of the magnet, leading to an increase in manufacturing cost and a decrease in magnet weight yield. Although it is conceivable to use the segment magnet as it is without bonding and solidifying the segment magnet, it is difficult to incorporate and fix the small magnet into the rotor against the repulsive force between the magnets.
本発明は、上述した従来の問題点に鑑みなされたもので、永久磁石回転機に適した渦電流が小さく保磁力の大きなＲ−Ｆｅ−Ｂ系希土類永久磁石（ＲはＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）及びその製造方法、並びにこの磁石を用いた永久磁石回転機を提供することを目的とするものである。 The present invention has been made in view of the above-described conventional problems, and is an R—Fe—B rare earth permanent magnet having a small eddy current and a large coercive force suitable for a permanent magnet rotating machine (R is a rare earth containing Y and Sc). It is an object of the present invention to provide a permanent magnet rotating machine using one or two or more selected from elements), a method for producing the same, and this magnet.
本発明者らは、Ｎｄ−Ｆｅ−Ｂ系焼結磁石に代表されるＲ1−Ｆｅ−Ｂ系焼結磁石に対し、Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上を含有する粉末（なお、Ｒ1〜Ｒ4はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）を磁石表面に存在させた状態で加熱することで、粉末に含まれていたＲ2、Ｒ3又はＲ4が磁石体に吸収され、残留磁束密度の減少を著しく抑制しながら保磁力を増大し得ることを見出した。この場合、特にＲ3のフッ化物又はＲ4の酸フッ化物を用いた場合、Ｒ3又はＲ4がフッ素と共に磁石体に高効率に吸収され、残留磁束密度が高く、保磁力の大きな焼結磁石が得られること、更に、磁石体に複数のスリットを入れることで、実質的に磁石表面積を大きくしてＲ2、Ｒ3又はＲ4の吸収率を高めることができ、しかもスリットは、磁石体を永久磁石回転機に組み込んだ際の渦電流低減にも有効であることを知見したものである。 The inventors of the present invention have compared R 1 -Fe-B sintered magnets represented by Nd—Fe—B based sintered magnets with respect to R 2 oxides, R 3 fluorides, and R 4 oxyfluorides. The powder containing one or more selected from the above (wherein R 1 to R 4 are one or more selected from rare earth elements including Y and Sc) is heated in a state of being present on the magnet surface. Thus, it has been found that R 2 , R 3 or R 4 contained in the powder is absorbed by the magnet body, and the coercive force can be increased while significantly suppressing the decrease in the residual magnetic flux density. In this case, in particular, when R 3 fluoride or R 4 oxyfluoride is used, R 3 or R 4 is absorbed into the magnet body together with fluorine with high efficiency, the residual magnetic flux density is high, and the coercive force is large. The magnet can be obtained, and further, by inserting a plurality of slits in the magnet body, the surface area of the magnet can be substantially increased to increase the absorption rate of R 2 , R 3 or R 4. It has been found that it is also effective in reducing eddy currents when the body is incorporated into a permanent magnet rotating machine.
即ち、本発明は、以下の希土類永久磁石、その製造方法、並びに永久磁石回転機を提供する。
請求項１：
Ｒ1−Ｆｅ−Ｂ系組成（Ｒ1はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）からなる焼結磁石体に対し、当該磁石体の少なくとも１つの表面に複数のスリットを設け、Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上（Ｒ2、Ｒ3、Ｒ4はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）を含有する粉末を当該磁石体の表面に存在させた状態で、当該磁石体及び粉末を当該磁石の焼結温度以下の温度で真空又は不活性ガス中において熱処理を施すことを特徴とする希土類永久磁石の製造方法。
請求項２：
Ｒ1−Ｆｅ−Ｂ系組成（Ｒ1はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）からなる焼結磁石体に対し、Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上（Ｒ2、Ｒ3、Ｒ4はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）を含有する粉末を当該磁石体の表面に存在させた状態で、当該磁石体及び粉末を当該磁石体の焼結温度以下の温度で真空又は不活性ガス中において熱処理を施し、次いで当該磁石体の少なくとも１つの表面に複数のスリットを設けることを特徴とする希土類永久磁石の製造方法。
請求項３：
焼結磁石体のスリット形成面に形成された各スリット間の間隔がそれぞれ１０ｍｍ以下であり、各スリットの最深部とスリット形成面に対して反対側の面との間の距離がそれぞれ５ｍｍ以下である請求項１又は２記載の希土類永久磁石の製造方法。
請求項４：
熱処理される焼結磁石体が、最大部の寸法が１００ｍｍ以下で、かつ磁気異方性化した方向の寸法が１０ｍｍ以下の形状を有する請求項１，２又は３記載の希土類永久磁石の製造方法。
請求項５：
Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上を含有する粉末の磁石体表面に対する存在量が、この磁石体の表面から距離１ｍｍ以内の当該磁石体を取り囲む空間内における平均的な占有率で１０容積％以上である請求項１乃至４のいずれか１項記載の希土類永久磁石の製造方法。
請求項６：
Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上を含有する粉末の平均粒子径が１００μｍ以下である請求項１乃至５のいずれか１項記載の希土類永久磁石の製造方法。
請求項７：
Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上（Ｒ2、Ｒ3、Ｒ4はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）のＲ2、Ｒ3、Ｒ4に１０原子％以上のＤｙ及び／又はＴｂが含まれることを特徴とする請求項１乃至６のいずれか１項記載の希土類永久磁石の製造方法。
請求項８：
Ｒ3のフッ化物及び／又はＲ4の酸フッ化物を含有する粉末を用い、Ｒ3及び／又はＲ4と共にフッ素を焼結磁石体に吸収させた請求項１乃至７のいずれか１項記載の希土類永久磁石の製造方法。
請求項９：
前記Ｒ3のフッ化物及び／又はＲ4の酸フッ化物を含有する粉末において、Ｒ3及び／又はＲ4に１０原子％以上のＤｙ及び／又はＴｂが含まれ、かつＲ3及び／又はＲ4におけるＮｄとＰｒの合計濃度が前記Ｒ1におけるＮｄとＰｒの合計濃度より低いことを特徴とする請求項８記載の希土類永久磁石の製造方法。
請求項１０：
前記Ｒ3のフッ化物及び／又はＲ4の酸フッ化物を含有する粉末において、Ｒ3のフッ化物とＲ4の酸フッ化物が合計で１０質量％以上含まれ、残部にＲ5の炭化物、窒化物、酸化物、水酸化物、水素化物から選ばれる１種又は２種以上（Ｒ5はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）を含むことを特徴とする請求項８又は９記載の希土類永久磁石の製造方法。
請求項１１：
上記熱処理後、更に低温で時効処理を施すことを特徴とする請求項１乃至１０のいずれか１項記載の希土類永久磁石の製造方法。
請求項１２：
Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上（Ｒ2、Ｒ3、Ｒ4はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）からなる平均粒子径が１００μｍ以下の粉末を水系又は有機系の溶媒に分散させたスラリーとして前記磁石体表面に存在させることを特徴とする請求項１乃至１１のいずれか１項記載の希土類永久磁石の製造方法。
請求項１３：
上記焼結磁石体を、アルカリ、酸又は有機溶剤のいずれか１種以上により洗浄した後、上記粉末を磁石体表面に存在させて上記熱処理を行うことを特徴とする請求項１乃至１２のいずれか１項記載の希土類永久磁石の製造方法。
請求項１４：
上記焼結磁石体の表面層をショットブラストで除去した後、上記粉末を磁石体表面に存在させて上記熱処理を行うことを特徴とする請求項１乃至１２のいずれか１項記載の希土類永久磁石の製造方法。
請求項１５：
熱処理後の最終処理として、アルカリ、酸又は有機溶剤のいずれか１種以上による洗浄処理、研削処理、又はメッキもしくは塗装処理を行うことを特徴とする請求項１乃至１４のいずれか１項記載の希土類永久磁石の製造方法。
請求項１６：
請求項１乃至１５のいずれか１項記載の製造方法により得られた希土類永久磁石。
請求項１７：
請求項１乃至１５のいずれか１項記載の製造方法によって得られた希土類永久磁石を組み込んだ永久磁石回転機において、当該磁石体のスリットが磁気異方性化した方向に対し直角な面に設けられたことを特徴とする永久磁石回転機。
請求項１８：
希土類永久磁石の表面に設けたスリットに非導電性物質を充填してなる請求項１７記載の永久磁石回転機。
That is, the present invention provides the following rare earth permanent magnet, method for producing the same, and permanent magnet rotating machine.
Claim 1:
For a sintered magnet body having an R 1 -Fe-B composition (R 1 is one or more selected from rare earth elements including Y and Sc), a plurality of slits are formed on at least one surface of the magnet body One or more selected from oxides of R 2 , fluorides of R 3 , and oxyfluorides of R 4 (R 2 , R 3 , R 4 are selected from rare earth elements including Y and Sc) The magnet body and the powder are subjected to heat treatment in a vacuum or an inert gas at a temperature lower than the sintering temperature of the magnet in a state where the powder containing one or more kinds is present on the surface of the magnet body. A method for producing a rare earth permanent magnet.
Claim 2:
For a sintered magnet body having an R 1 -Fe-B composition (R 1 is one or more selected from rare earth elements including Y and Sc), an oxide of R 2 , a fluoride of R 3 , A magnet containing a powder containing one or more selected from oxyfluorides of R 4 (R 2 , R 3 , R 4 are one or more selected from rare earth elements including Y and Sc) The magnet body and the powder are heat-treated in a vacuum or an inert gas at a temperature lower than the sintering temperature of the magnet body, and then a plurality of slits are formed on at least one surface of the magnet body. A method for producing a rare earth permanent magnet.
Claim 3:
The interval between the slits formed on the slit forming surface of the sintered magnet body is 10 mm or less, and the distance between the deepest part of each slit and the surface opposite to the slit forming surface is 5 mm or less. The method for producing a rare earth permanent magnet according to claim 1 or 2.
Claim 4:
The method for producing a rare earth permanent magnet according to claim 1, 2 or 3, wherein the sintered magnet body to be heat-treated has a shape in which the dimension of the maximum part is 100 mm or less and the dimension in the direction of magnetic anisotropy is 10 mm or less. .
Claim 5:
The abundance of the powder containing one or more selected from R 2 oxide, R 3 fluoride, and R 4 oxyfluoride with respect to the surface of the magnet body is within a distance of 1 mm from the surface of the magnet body. The method for producing a rare earth permanent magnet according to any one of
Claim 6:
Oxide of R 2, fluoride of R 3, any one of
Claim 7:
One or more selected from R 2 oxide, R 3 fluoride, R 4 oxyfluoride (R 2 , R 3 , R 4 are one selected from rare earth elements including Y and Sc, or The method for producing a rare earth permanent magnet according to any one of
Claim 8:
The powder containing R 3 fluoride and / or R 4 oxyfluoride, and fluorine is absorbed into the sintered magnet body together with R 3 and / or R 4. Manufacturing method of rare earth permanent magnets.
Claim 9:
In powders containing fluoride and / or oxyfluoride of R 4 of the R 3, R 3 and / or R 4 to 10 atomic% or more Dy and / or Tb is included, and R 3 and / or R 9. The method for producing a rare earth permanent magnet according to claim 8, wherein the total concentration of Nd and Pr in 4 is lower than the total concentration of Nd and Pr in R 1 .
Claim 10:
Wherein in the powder comprising a fluoride and / or oxyfluoride of R 4 in R 3, oxyfluoride of fluoride and R 4 in R 3 are contained more than 10 wt% in total, carbide R 5 to the remainder, One or more selected from nitrides, oxides, hydroxides, and hydrides (R 5 is one or more selected from rare earth elements including Y and Sc). Item 10. A method for producing a rare earth permanent magnet according to Item 8 or 9.
Claim 11:
The method for producing a rare earth permanent magnet according to any one of
Claim 12:
One or more selected from R 2 oxide, R 3 fluoride, R 4 oxyfluoride (R 2 , R 3 , R 4 are one selected from rare earth elements including Y and Sc, or 12. The powder according to
Claim 13:
13. The sintered magnet body is washed with one or more of alkali, acid, or organic solvent, and then the heat treatment is performed with the powder being present on the surface of the magnet body. A method for producing a rare earth permanent magnet according to
Claim 14:
13. The rare earth permanent magnet according to
Claim 15:
The final treatment after the heat treatment is performed by a cleaning treatment, a grinding treatment, or a plating or coating treatment with at least one of an alkali, an acid, and an organic solvent. A method for producing a rare earth permanent magnet.
Claim 16:
A rare earth permanent magnet obtained by the production method according to any one of
Claim 17:
The permanent magnet rotating machine incorporating the rare earth permanent magnet obtained by the manufacturing method according to any one of
Claim 18:
The permanent magnet rotating machine according to claim 17, wherein a slit provided on the surface of the rare earth permanent magnet is filled with a nonconductive material.
本発明によれば、永久磁石回転機に適した渦電流が小さく高い残留磁束密度と高い保磁力を有するＲ−Ｆｅ−Ｂ系焼結磁石及びこの磁石を用いた永久磁石回転機を提供することができる。 According to the present invention, an R—Fe—B sintered magnet having a small eddy current and a high residual magnetic flux density and a high coercive force suitable for a permanent magnet rotating machine and a permanent magnet rotating machine using this magnet are provided. Can do.
本発明は、永久磁石回転機に適した渦電流が小さく高い残留磁束密度と高い保磁力を有するＲ−Ｆｅ−Ｂ系焼結磁石及びこの磁石を用いた永久磁石回転機に関するものである。本発明の希土類永久磁石は、Ｒ1−Ｆｅ−Ｂ系組成からなる焼結磁石体表面にスリットを入れ、後述する希土類元素の酸化物、フッ化物又は酸フッ化物を供給して熱処理を行うもの、及び希土類永久磁石はＲ1−Ｆｅ−Ｂ系組成からなる焼結磁石体表面に、後述する希土類元素の酸化物、フッ化物又は酸フッ化物を供給して熱処理したものにスリットを入れるものがある。 The present invention relates to an R—Fe—B sintered magnet having a small eddy current and high residual magnetic flux density and high coercive force suitable for a permanent magnet rotating machine, and a permanent magnet rotating machine using this magnet. The rare earth permanent magnet of the present invention has a slit formed on the surface of a sintered magnet body composed of an R 1 —Fe—B composition, and supplies a rare earth element oxide, fluoride or oxyfluoride described later to perform heat treatment. , And rare earth permanent magnets that have slits formed on the surface of a sintered magnet body having an R 1 —Fe—B composition and supplied with a rare earth element oxide, fluoride, or oxyfluoride, which will be described later, and heat-treated. is there.
ここで、Ｒ1−Ｆｅ−Ｂ系焼結磁石体は、常法に従い、母合金を粗粉砕、微粉砕、成形、焼結させることにより得ることができる。 Here, the R 1 —Fe—B based sintered magnet body can be obtained by roughly pulverizing, finely pulverizing, forming and sintering the mother alloy according to a conventional method.
なお、本発明において、Ｒ及びＲ1はいずれもＹ及びＳｃを含む希土類元素から選ばれるものを意味するが、Ｒは主に得られた磁石体に関して使用し、Ｒ1は主に出発原料に関して用いる。 In the present invention, R and R 1 are both selected from rare earth elements including Y and Sc. R is mainly used for the obtained magnet body, and R 1 is mainly used for the starting material. Use.
母合金は、Ｒ1、Ｆｅ、Ｂを含有する。Ｒ1はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上で、具体的にはＹ、Ｓｃ、Ｌａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｅｕ、Ｇｄ、Ｔｂ、Ｄｙ、Ｈｏ、Ｅｒ、Ｙｂ及びＬｕが挙げられ、好ましくはＮｄ、Ｐｒ、Ｄｙを主体とする。これらＹ及びＳｃを含む希土類元素は合金全体の１０〜１５原子％、特に１２〜１５原子％であることが好ましく、更に好ましくはＲ1中にＮｄとＰｒあるいはそのいずれか１種を１０原子％以上、特に５０原子％以上含有することが好適である。Ｂは３〜１５原子％、特に４〜８原子％含有することが好ましい。その他、Ａｌ、Ｃｕ、Ｚｎ、Ｉｎ、Ｓｉ、Ｐ、Ｓ、Ｔｉ、Ｖ、Ｃｒ、Ｍｎ、Ｎｉ、Ｇａ、Ｇｅ、Ｚｒ、Ｎｂ、Ｍｏ、Ｐｄ、Ａｇ、Ｃｄ、Ｓｎ、Ｓｂ、Ｈｆ、Ｔａ、Ｗの中から選ばれる１種又は２種以上を０〜１１原子％、特に０．１〜５原子％含有してもよい。残部はＦｅ及びＣ、Ｎ、Ｏ等の不可避的な不純物であるが、Ｆｅは５０原子％以上、特に６５原子％以上含有することが好ましい。また、Ｆｅの一部、例えばＦｅの０〜４０原子％、特に０〜１５原子％をＣｏで置換しても差支えない。 The mother alloy contains R 1 , Fe, and B. R 1 is one or more selected from rare earth elements including Y and Sc, specifically, Y, Sc, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er , Yb, and Lu, preferably Nd, Pr, and Dy. These rare earth elements including Y and Sc are preferably 10 to 15 atomic%, particularly 12 to 15 atomic% of the whole alloy, more preferably 10% by atom of Nd and Pr or any one of them in R 1. As mentioned above, it is suitable to contain especially 50 atomic% or more. B is preferably contained in an amount of 3 to 15 atomic%, particularly 4 to 8 atomic%. In addition, Al, Cu, Zn, In, Si, P, S, Ti, V, Cr, Mn, Ni, Ga, Ge, Zr, Nb, Mo, Pd, Ag, Cd, Sn, Sb, Hf, Ta, One or two or more kinds selected from W may be contained in an amount of 0 to 11 atomic%, particularly 0.1 to 5 atomic%. The balance is inevitable impurities such as Fe and C, N, and O, but Fe is preferably contained in an amount of 50 atomic% or more, particularly 65 atomic% or more. Further, a part of Fe, for example, 0 to 40 atomic%, particularly 0 to 15 atomic% of Fe may be substituted with Co.
母合金は原料金属あるいは合金を真空あるいは不活性ガス、好ましくはＡｒ雰囲気中で溶解したのち、平型やブックモールドに鋳込む、あるいはストリップキャストにより鋳造することで得られる。また、本系合金の主相であるＲ2Ｆｅ14Ｂ化合物組成に近い合金と焼結温度で液相助剤となるＲリッチな合金とを別々に作製し、粗粉砕後に秤量混合する、いわゆる２合金法も本発明には適用可能である。但し、主相組成に近い合金に対して、鋳造時の冷却速度や合金組成に依存してα−Ｆｅ相が残存しやすく、Ｒ2Ｆｅ14Ｂ化合物相の量を増やす目的で必要に応じて均質化処理を施す。その条件は真空あるいはＡｒ雰囲気中で７００〜１，２００℃で１時間以上熱処理する。この場合、主相組成に近い合金はストリップキャスト法にて得ることもできる。液相助剤となるＲリッチな合金については上記鋳造法のほかに、いわゆる液体急冷法やストリップキャスト法も適用できる。 The mother alloy can be obtained by melting a raw metal or alloy in a vacuum or an inert gas, preferably in an Ar atmosphere, and then casting it in a flat mold or a book mold, or by strip casting. Also, an alloy close to the R 2 Fe 14 B compound composition that is the main phase of this alloy and an R-rich alloy that becomes a liquid phase aid at the sintering temperature are separately prepared, and are weighed and mixed after coarse pulverization. A two alloy method is also applicable to the present invention. However, for an alloy close to the main phase composition, the α-Fe phase tends to remain depending on the cooling rate at the time of casting and the alloy composition, and as necessary for the purpose of increasing the amount of R 2 Fe 14 B compound phase. Apply homogenization. The conditions are heat treatment at 700 to 1,200 ° C. for 1 hour or more in vacuum or Ar atmosphere. In this case, an alloy close to the main phase composition can also be obtained by strip casting. In addition to the above casting method, a so-called liquid quenching method or strip casting method can be applied to the R-rich alloy serving as the liquid phase aid.
更に、以下に述べる粉砕工程において、Ｒ1の炭化物、窒化物、酸化物、水酸化物のうち少なくとも１種あるいはこれらの混合物又は複合物を０．００５〜５質量％の範囲で合金粉末と混合することも可能である。 Further, in the pulverization step described below, at least one of R 1 carbide, nitride, oxide and hydroxide, or a mixture or composite thereof is mixed with the alloy powder in the range of 0.005 to 5% by mass. It is also possible to do.
上記合金は、通常０．０５〜３ｍｍ、特に０．０５〜１．５ｍｍに粗粉砕される。粗粉砕工程にはブラウンミルあるいは水素粉砕が用いられ、ストリップキャストにより作製された合金の場合は水素粉砕が好ましい。粗粉は、例えば高圧窒素を用いたジェットミルにより通常０．２〜３０μｍ、特に０．５〜２０μｍに微粉砕される。微粉末は磁界中圧縮成形機で成形され、焼結炉に投入される。焼結は真空あるいは不活性ガス雰囲気中、通常９００〜１，２５０℃、特に１，０００〜１，１００℃で行われる。 The alloy is generally coarsely pulverized to 0.05 to 3 mm, particularly 0.05 to 1.5 mm. Brown mill or hydrogen pulverization is used for the coarse pulverization process, and hydrogen pulverization is preferable in the case of an alloy produced by strip casting. The coarse powder is usually finely pulverized to 0.2 to 30 μm, particularly 0.5 to 20 μm, for example, by a jet mill using high-pressure nitrogen. The fine powder is formed by a compression molding machine in a magnetic field and put into a sintering furnace. Sintering is usually performed at 900 to 1,250 ° C, particularly 1,000 to 1,100 ° C in a vacuum or an inert gas atmosphere.
ここで得られた焼結磁石は、正方晶Ｒ2Ｆｅ14Ｂ化合物を主相として６０〜９９体積％、特に好ましくは８０〜９８体積％含有し、残部は０．５〜２０体積％のＲに富む相、０〜１０体積％のＢに富む相及び不可避的不純物により生成した、あるいは添加による炭化物、窒化物、酸化物、水酸化物のうち少なくとも１種あるいはこれらの混合物又は複合物からなる。 The sintered magnet obtained here contains 60 to 99% by volume, particularly preferably 80 to 98% by volume of a tetragonal R 2 Fe 14 B compound as a main phase, and the balance is 0.5 to 20% by volume of R. A phase rich in 0, 10% by volume of B, and inevitable impurities, or at least one of carbides, nitrides, oxides and hydroxides, or a mixture or composite thereof. .
本発明において、磁石表面に存在させたＲ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上を含有する粉末から磁石体へのＲ2、Ｒ3又はＲ4の吸収を高めるために、得られた焼結ブロックを所定形状に研削する際に、表面に複数のスリットを入れて比表面積を大きくする。 In the present invention, R 2 , R from the powder containing one or more selected from the R 2 oxide, R 3 fluoride, and R 4 oxyfluoride present on the magnet surface to the magnet body. In order to increase the absorption of 3 or R 4 , when the obtained sintered block is ground into a predetermined shape, a plurality of slits are put on the surface to increase the specific surface area.
この場合、スリットの形成態様は特に限定されるものではなく、焼結磁石体の形成等に応じて種々選定することができる。例えば、焼結磁石体が直方体形状の場合は、図１（Ａ）〜（Ｃ）に示すように、図において焼結磁石体１のスリット形成面１ａの幅方向両側縁部に対しスリット２の長さ方向両端部を離間させて、又は離間させることなく側縁部から切り込み形成した態様を採用し得るが、勿論これに制限されるものではない。
なお、焼結磁石体のスリット形成面に図１（Ａ）〜（Ｄ）の如くスリットを形成した場合（但し、図１（Ａ）〜（Ｃ）はそれぞれ異なる態様でスリットが形成されたスリット形成面を示す平面図であり、図１（Ｄ）は縦断面図である）、スリット２最深部とスリット形成面１ａに対し、反対側の面１ｂとの間の距離Ｄ1及びスリット２の長さ方向端部とこれに対向する面１ｃ又は１ｄとの間の距離Ｄ2はいずれも５ｍｍ以下、より好ましくは３ｍｍ以下、特に好ましくは１ｍｍ以下であることがよく、また図においてスリット２と平行な面１ｅ，１ｆとこれに隣接するスリット２ａとの間隔Ｄ3及び互いに隣接するスリット２間の間隔Ｄ4は、いずれも１０ｍｍ以下、より好ましくは６ｍｍ以下、特に好ましくは２ｍｍ以下であることがよい。この場合、上記距離Ｄ1は通常０．４ｍｍ以上であることが好ましく、距離Ｄ2は０ｍｍであってもよい。また、間隔Ｄ3，Ｄ4はそれぞれ０．４ｍｍ以上であることが好ましい。
In this case, the formation mode of the slit is not particularly limited, and can be variously selected according to the formation of the sintered magnet body. For example, when the sintered magnet body has a rectangular parallelepiped shape, as shown in FIGS. 1 (A) to 1 (C), the
In addition, when slits are formed on the slit forming surface of the sintered magnet body as shown in FIGS. 1A to 1D (however, FIGS. 1A to 1C are slits in which slits are formed in different modes. FIG. 1D is a longitudinal sectional view), and the distance D 1 between the deepest part of the
このようにスリットを形成することにより、図１（Ｅ）に示したように、磁石の表面及びスリット部分から磁石内部に至る最大距離Ｌを５ｍｍ以下にすることができ、これによって磁石全体をＲ2の酸化物、Ｒ3のフッ化物又はＲ4の酸フッ化物で均一にかつ効率よく熱処理、浸透させることができる。なお、Ｌはより好ましくは３ｍｍ以下、特に好ましくは１ｍｍ以下である。 By forming the slit in this way, as shown in FIG. 1E, the maximum distance L from the surface of the magnet and the slit portion to the inside of the magnet can be reduced to 5 mm or less. Heat treatment and permeation can be performed uniformly and efficiently with 2 oxides, fluoride of R 3 or oxyfluoride of R 4 . Note that L is more preferably 3 mm or less, and particularly preferably 1 mm or less.
このように、スリットと磁石面との距離関係を設定することにより、スリットによる表面積も増えて、磁石全体において吸収処理が起きやすい領域になったものである。ここで、スリットが形成されない場合、図１（Ｆ）の焼結磁石体表面の各外縁部から５ｍｍ以上の中央領域３が吸収処理が起こり難い領域であるが、上記のようにスリットを形成することにより、表面からの吸収処理が起こる領域が増大したものである。
Thus, by setting the distance relationship between the slit and the magnet surface, the surface area due to the slit also increases, and the entire magnet is easily subjected to absorption treatment. Here, when the slit is not formed, the
なお、上述したスリットは、焼結前の成形体の段階で形成することができる。 In addition, the slit mentioned above can be formed in the stage of the molded object before sintering.
ここで、スリットのない状態での焼結ブロックの最大部の寸法が１００ｍｍ以下、好ましくは５０ｍｍ以下で、かつ磁気異方性化した方向の寸法が１０ｍｍ以下、好ましくは５ｍｍ以下である場合には、本発明の磁石表面に存在させたＲ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上を含有する粉末から磁石体にＲ2、Ｒ3又はＲ4を吸収させる熱処理を行った後で、磁石表面に複数のスリットを入れても、前述のスリットを入れた後に熱処理を行う方法と同様の効果を得ることができる。即ち、渦電流が小さく、高い残留磁束密度と高い保磁力を有することができる。なお上記最大部の寸法及び磁気異方性化した方向の寸法の下限は特に制限されず、適宜選定されるが、上記形状の最大部の寸法は１ｍｍ以上であり、磁気異方性化した方向の寸法は０．５ｍｍ以上とすることができるが、上記距離Ｄ1，Ｄ2、間隔Ｄ3，Ｄ4の下限値を与えるように、また上記距離Ｌを有するような大きさに選定し得る。 Here, when the dimension of the maximum part of the sintered block without a slit is 100 mm or less, preferably 50 mm or less, and the dimension in the direction of magnetic anisotropy is 10 mm or less, preferably 5 mm or less. oxide of R 2 to the magnet surface was present in the present invention, R 2 fluoride of R 3, a powder containing one or more kinds selected from an acid fluoride of R 4 to the magnet body, R 3 Alternatively, even if a plurality of slits are formed on the magnet surface after heat treatment for absorbing R 4 , the same effect as the method of performing heat treatment after inserting the slits can be obtained. That is, an eddy current is small, and it can have a high residual magnetic flux density and a high coercive force. The lower limit of the dimension of the maximum part and the direction of magnetic anisotropy is not particularly limited and is appropriately selected, but the dimension of the maximum part of the shape is 1 mm or more and the direction of magnetic anisotropy. Can be selected to a size that gives the lower limit of the distances D 1 and D 2 and the distances D 3 and D 4 and that has the distance L. .
本発明では、従来の渦電流を小さくするための方法である細分化した磁石を接着固化して所要の大きさの磁石にする（分割磁石）のではなく、セグメント磁石にスリットを入れるだけであり、分割磁石の接着、組立工程をなくして製造コストを抑えることができる。スリットの幅は、磁束をロスさせないために、１ｍｍ以下の狭い幅にするのが好ましい。焼結前の成形体や焼結体にスリットを入れる方法として内周又は外周切断機やワイヤーソーやウォータジェットなどで加工して溝を形成するため、切断歯の厚みを考慮すると、望ましくは０．８ｍｍ以下であり、一方、スリット幅の下限は幾らでもよいが、加工機の制約から０．０５ｍｍ以上が実際的である。 In the present invention, the conventional method for reducing eddy currents is not to bond and solidify a segmented magnet into a magnet of the required size (split magnet), but only to slit the segment magnet. The manufacturing cost can be reduced by eliminating the bonding and assembling steps of the split magnets. The width of the slit is preferably a narrow width of 1 mm or less so as not to lose the magnetic flux. As a method of forming a slit in a green body before sintering or a sintered body, a groove is formed by processing with an inner or outer peripheral cutting machine, a wire saw, a water jet, or the like. On the other hand, the lower limit of the slit width may be any number, but 0.05 mm or more is practical due to the limitations of the processing machine.
研削加工された磁石体表面にはＲ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上を含有する粉末を存在させる。なお、Ｒ2、Ｒ3、Ｒ4はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上で、それぞれＲ2、Ｒ3、Ｒ4中１０原子％以上、より好ましくは２０原子％以上、特に４０原子％以上のＤｙ又はＴｂを含むことが好ましい。この場合、前記Ｒ3のフッ化物及び／又はＲ4の酸フッ化物を含有する粉末において、Ｒ3及び／又はＲ4に１０原子％以上のＤｙ及び／又はＴｂが含まれ、かつＲ3及び／又はＲ4におけるＮｄとＰｒの合計濃度が前記Ｒ1におけるＮｄとＰｒの合計濃度より低いことが本発明の目的から好ましい。 A powder containing one or more selected from R 2 oxide, R 3 fluoride, and R 4 oxyfluoride is present on the surface of the ground magnet body. R 2 , R 3 , and R 4 are one or more selected from rare earth elements including Y and Sc, and each of R 2 , R 3 , and R 4 is 10 atom% or more, more preferably 20 atom%. As described above, it is particularly preferable to contain 40 atomic% or more of Dy or Tb. In this case, the powder containing fluoride and / or oxyfluoride of R 4 of the R 3, R 3 and / or R 4 to 10 atomic% or more Dy and / or Tb is included, and R 3 and It is preferable from the object of the present invention that the total concentration of Nd and Pr in R 4 is lower than the total concentration of Nd and Pr in R 1 .
磁石表面空間における粉末の存在率は高いほど吸収されるＲ2、Ｒ3又はＲ4量が多くなるので、本発明における効果を達成させるために、上記粉末の存在率は、磁石表面から距離１ｍｍ以内の磁石を取り囲む空間内での平均的な値で１０容積％以上が好ましく、更に好ましくは４０容積％以上である。 The higher the abundance ratio of the powder in the magnet surface space, the more R 2 , R 3, or R 4 is absorbed. Therefore, in order to achieve the effect of the present invention, the abundance ratio of the powder is 1 mm from the magnet surface. The average value in the space surrounding the inner magnet is preferably 10% by volume or more, and more preferably 40% by volume or more.
粉末を存在させる方法（粉末処理方法）としては、例えば、Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上を含有する微粉末を水あるいは有機溶剤に分散させ、このスラリーに磁石体を浸した後に熱風や真空により乾燥させる、あるいは自然乾燥させる方法が挙げられる。この他にスプレーによる塗布等も可能である。いずれの具体的手法にせよ、非常に簡便にかつ大量に処理できることが特徴といえる。上記微粉末の粒子径はＲ2、Ｒ3又はＲ4成分が磁石に吸収される際の反応性に影響を与え、粒子が小さいほど反応にあずかる接触面積が増大する。本発明における効果をより効果的に達成させるためには、存在させる粉末の平均粒子径は１００μｍ以下、好ましくは１０μｍ以下が望ましい。その下限は特に制限されないが１ｎｍ以上が好ましい。なお、この平均粒子径は、例えばレーザー回折法などによる粒度分布測定装置等を用いて質量平均値Ｄ50（即ち、累積質量が５０％となるときの粒子径又はメジアン径）などとして求めることができる。 As a method for making the powder exist (powder processing method), for example, a fine powder containing one or more selected from R 2 oxide, R 3 fluoride, and R 4 oxyfluoride is used as water or Examples include a method of dispersing in an organic solvent and immersing the magnet body in this slurry, followed by drying with hot air or vacuum, or natural drying. In addition, application by spraying is also possible. Whatever the specific method, it can be said that it can be processed very easily and in large quantities. The particle size of the fine powder affects the reactivity when the R 2 , R 3 or R 4 component is absorbed by the magnet, and the smaller the particle, the greater the contact area involved in the reaction. In order to achieve the effect of the present invention more effectively, the average particle size of the powder to be present is 100 μm or less, preferably 10 μm or less. The lower limit is not particularly limited, but is preferably 1 nm or more. The average particle diameter can be obtained as a mass average value D 50 (that is, a particle diameter or a median diameter when the cumulative mass is 50%) using a particle size distribution measuring device using a laser diffraction method, for example. it can.
本発明におけるＲ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物とは、好ましくはそれぞれＲ2 2Ｏ3、Ｒ3Ｆ3、Ｒ4ＯＦであるが、これ以外のＲ2Ｏn、Ｒ3Ｆn、Ｒ4ＯmＦn（ｍ、ｎは任意の正数）や、金属元素によりＲ2、Ｒ3、Ｒ4の一部を置換したあるいは安定化されたもの等、本発明の効果を達成することができるＲ2と酸素を含む酸化物、Ｒ3とフッ素を含むフッ化物、Ｒ4と酸素とフッ素を含む酸フッ化物を指す。
Oxide of R 2 in the present invention, fluoride of R 3, and oxyfluoride of R 4, preferably each R 2 2 O 3, R 3
この場合、磁石表面に存在させる粉末は、Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物、あるいはこれらの混合物を含有し、この他にＲ5（Ｒ5はＹ及びＳｃを含む希土類元素から選ばれる１種又は２種以上）の炭化物、窒化物、水酸化物、水素化物のうち少なくとも１種あるいはこれらの混合物又は複合物を含んでもよく、またＲ3のフッ化物及び／又はＲ4の酸フッ化物を用いる場合、Ｒ5の酸化物を含んでもよい。更に、粉末の分散性や化学的・物理的吸着を促進するために、ホウ素、窒化ホウ素、シリコン、炭素などの微粉末やステアリン酸などの有機化合物を含むこともできる。本発明の効果を高効率に達成するには、Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物、あるいはこれらの混合物が粉末全体に対して１０質量％以上、好ましくは２０質量％以上含まれる。特には、主成分として、Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物が、粉末全体に対して５０質量％以上、より好ましくは７０質量％以上、更に好ましくは９０質量％以上含有することが推奨される。 In this case, the powder to be present on the magnet surface contains an oxide of R 2 , a fluoride of R 3, an oxyfluoride of R 4 , or a mixture thereof, in addition to R 5 (R 5 is Y and Sc). 1 type or 2 or more types selected from rare earth elements containing), carbides, nitrides, hydroxides, hydrides, or a mixture or composite thereof, and R 3 fluoride and When the acid fluoride of R 4 is used, the oxide of R 5 may be included. Furthermore, in order to promote the dispersibility of the powder and chemical / physical adsorption, fine powders such as boron, boron nitride, silicon, and carbon, and organic compounds such as stearic acid can also be included. In order to achieve the effect of the present invention with high efficiency, the oxide of R 2 , the fluoride of R 3 , the oxyfluoride of R 4 , or a mixture thereof is 10 mass% or more, preferably 20 More than mass% is contained. In particular, R 2 oxide, R 3 fluoride, and R 4 oxyfluoride as main components are 50% by mass or more, more preferably 70% by mass or more, and still more preferably 90% by mass with respect to the whole powder. % Or more is recommended.
Ｒ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物、あるいはこれらの混合物からなる粉末を磁石表面に存在させた状態で、磁石と粉末は真空あるいはアルゴン（Ａｒ）、ヘリウム（Ｈｅ）等の不活性ガス雰囲気中で熱処理される（以後、この処理を吸収処理と称する）。吸収処理温度は磁石体の焼結温度以下である。処理温度の限定理由は以下のとおりである。 In a state where a powder composed of an oxide of R 2 , a fluoride of R 3, an oxyfluoride of R 4 , or a mixture thereof is present on the surface of the magnet, the magnet and the powder may be vacuum, argon (Ar), helium (He And the like (hereinafter, this treatment is referred to as absorption treatment). The absorption treatment temperature is lower than the sintering temperature of the magnet body. The reasons for limiting the treatment temperature are as follows.
即ち、当該焼結磁石の焼結温度（ＴS℃と称する）より高い温度で処理すると、（１）焼結磁石の組織が変質し、高い磁気特性が得られなくなる、（２）熱変形により加工寸法が維持できなくなる、（３）拡散させたＲが磁石の結晶粒界面だけでなく内部にまで拡散してしまい残留磁束密度が低下する、等の問題が生じるために、処理温度は焼結温度以下、好ましくは（ＴS−１０）℃以下とする。なお、温度の下限は適宜選定されるが、通常３５０℃以上である。吸収処理時間は１分〜１００時間である。１分未満では吸収処理が完了せず、１００時間を超えると、焼結磁石の組織が変質する、不可避的な酸化や成分の蒸発が磁気特性に悪い影響を与えるといった問題が生じやすい。より好ましくは５分〜８時間、特に１０分〜６時間である。 That is, if the sintered magnet is processed at a temperature higher than the sintering temperature (referred to as T S ° C), (1) the structure of the sintered magnet is altered and high magnetic properties cannot be obtained. The processing temperature cannot be maintained. (3) The diffused R diffuses not only into the crystal grain interface of the magnet but also into the interior, resulting in a decrease in residual magnetic flux density. Temperature or lower, preferably (T S −10) ° C. or lower. In addition, although the minimum of temperature is selected suitably, it is 350 degreeC or more normally. Absorption treatment time is 1 minute to 100 hours. If it is less than 1 minute, the absorption treatment is not completed, and if it exceeds 100 hours, the structure of the sintered magnet is altered, and problems such as inevitable oxidation and evaporation of components adversely affect the magnetic properties. More preferably, it is 5 minutes to 8 hours, particularly 10 minutes to 6 hours.
以上のような吸収処理により、磁石内の希土類に富む粒界相成分に、磁石表面に存在させた粉末に含まれていたＲ2、Ｒ3又はＲ4が濃化し、このＲ2、Ｒ3又はＲ4がＲ2Ｆｅ14Ｂ主相粒子の表層部付近で置換される。また、粉末にＲ3のフッ化物又はＲ4の酸フッ化物が含まれている場合、この粉末に含まれているフッ素は、その一部がＲ3又はＲ4と共に磁石内に吸収されることにより、Ｒ3又はＲ4の粉末からの供給と磁石の結晶粒界における拡散を著しく高める。 By the absorption treatment as described above, R 2 , R 3 or R 4 contained in the powder present on the magnet surface is concentrated in the rare earth-rich grain boundary phase component in the magnet, and this R 2 , R 3 is concentrated. Alternatively, R 4 is substituted in the vicinity of the surface layer portion of the R 2 Fe 14 B main phase particle. In addition, when the powder contains R 3 fluoride or R 4 oxyfluoride, a part of the fluorine contained in the powder is absorbed in the magnet together with R 3 or R 4. Significantly increases the supply from the R 3 or R 4 powder and the diffusion at the grain boundaries of the magnet.
Ｒ2の酸化物、Ｒ3のフッ化物及びＲ4の酸フッ化物に含まれる希土類元素は、Ｙ及びＳｃを含む希土類元素から選ばれる１種又は２種以上であるが、上記表層部に濃化して結晶磁気異方性を高める効果の特に大きい元素はＤｙ、Ｔｂであるので、粉末に含まれている希土類元素としてはＤｙ及びＴｂの割合が合計で１０原子％以上であることが好適である。更に好ましくは２０原子％以上である。また、Ｒ2、Ｒ3、Ｒ4におけるＮｄとＰｒの合計濃度が、Ｒ1のＮｄとＰｒの合計濃度より低いことが好ましい。 The rare earth element contained in the oxide of R 2 , the fluoride of R 3 and the oxyfluoride of R 4 is one or more selected from the rare earth elements including Y and Sc. Since elements that have a particularly large effect of increasing crystal magnetic anisotropy are Dy and Tb, the rare earth elements contained in the powder preferably have a total ratio of Dy and Tb of 10 atomic% or more. is there. More preferably, it is 20 atomic% or more. Further, the total concentration of Nd and Pr in R 2 , R 3 and R 4 is preferably lower than the total concentration of Nd and Pr in R 1 .
この吸収処理の結果、残留磁束密度の低減をほとんど伴わずにＲ−Ｆｅ−Ｂ系焼結磁石の保磁力が効率的に増大される。 As a result of this absorption treatment, the coercive force of the R—Fe—B based sintered magnet is efficiently increased with little reduction in residual magnetic flux density.
上記吸収処理は、例えば上記粉末を水や有機溶剤に分散させたスラリーに焼結磁石体を投入するなどして、該焼結磁石体表面に上記粉末を付着させた状態で熱処理させることによって行うことができ、この場合、上記吸収処理において、磁石は粉末に覆われ、磁石同士は離れて存在するので、高温での熱処理であるにもかかわらず、吸収処理後に磁石同士が溶着することがない。更に、粉末も熱処理後に磁石に固着することもないため、熱処理用容器に大量に磁石を投入して処理することが可能であり、本発明による製造方法は生産性にも優れていることがわかる。 The absorption treatment is performed by, for example, putting a sintered magnet body into a slurry in which the powder is dispersed in water or an organic solvent, and performing a heat treatment with the powder adhered to the surface of the sintered magnet body. In this case, in the above absorption treatment, the magnets are covered with powder, and the magnets are separated from each other, so that the magnets are not welded after the absorption treatment despite the heat treatment at a high temperature. . Furthermore, since the powder does not stick to the magnet after the heat treatment, it can be processed by putting a large amount of magnets in the heat treatment container, and it can be seen that the production method according to the present invention is excellent in productivity. .
また、吸収処理後、時効処理を施すことが好ましい。この時効処理としては、吸収処理温度未満、好ましくは２００℃以上で吸収処理温度より１０℃低い温度以下、更に好ましくは３５０℃以上で吸収処理温度より１０℃低い温度以下であることが望ましい。また、その雰囲気は真空あるいはＡｒ、Ｈｅ等の不活性ガス中であることが好ましい。時効処理の時間は１分〜１０時間、好ましくは１０分〜５時間、特に３０分〜２時間である。 Moreover, it is preferable to perform an aging treatment after the absorption treatment. The aging treatment is desirably less than the absorption treatment temperature, preferably 200 ° C. or more and 10 ° C. or less, more preferably 350 ° C. or more and 10 ° C. or less. The atmosphere is preferably in a vacuum or an inert gas such as Ar or He. The time for aging treatment is 1 minute to 10 hours, preferably 10 minutes to 5 hours, particularly 30 minutes to 2 hours.
なお、上記粉末を焼結磁石体に存在させる前の上述した焼結磁石体の研削加工時において、研削加工機の冷却液に水系のものを用いる、あるいは加工時に研削面が高温に曝される場合、被研削面に酸化膜が生じやすく、この酸化膜が粉末から磁石体へのＲ2、Ｒ3又はＲ4成分の吸収反応を妨げることがある。このような場合には、アルカリ、酸あるいは有機溶剤のいずれか１種以上を用いて洗浄する、あるいはショットブラストを施して、その酸化膜を除去することで適切な吸収処理ができる。 In addition, at the time of grinding of the above-described sintered magnet body before the powder is present in the sintered magnet body, a water-based one is used as the coolant of the grinding machine, or the grinding surface is exposed to a high temperature during processing. In this case, an oxide film is likely to be formed on the surface to be ground, and this oxide film may hinder the absorption reaction of the R 2 , R 3 or R 4 component from the powder to the magnet body. In such a case, an appropriate absorption treatment can be carried out by removing the oxide film by washing with one or more of alkali, acid or organic solvent, or by performing shot blasting.
アルカリとしては、ピロリン酸カリウム、ピロリン酸ナトリウム、クエン酸カリウム、クエン酸ナトリウム、酢酸カリウム、酢酸ナトリウム、シュウ酸カリウム、シュウ酸ナトリウム等、酸としては、塩酸、硝酸、硫酸、酢酸、クエン酸、酒石酸等、有機溶剤としては、アセトン、メタノール、エタノール、イソプロピルアルコールなどを使用することができる。この場合、上記アルカリや酸は、磁石体を浸食しない適宜濃度の水溶液として使用することができる。 As alkali, potassium pyrophosphate, sodium pyrophosphate, potassium citrate, sodium citrate, potassium acetate, sodium acetate, potassium oxalate, sodium oxalate, etc., acids include hydrochloric acid, nitric acid, sulfuric acid, acetic acid, citric acid, As the organic solvent such as tartaric acid, acetone, methanol, ethanol, isopropyl alcohol and the like can be used. In this case, the alkali or acid can be used as an aqueous solution having an appropriate concentration that does not erode the magnet body.
更には、上記焼結磁石体の表面層を上記粉末を焼結磁石体に存在させる前にショットブラストで除去することもできる。 Furthermore, the surface layer of the sintered magnet body can be removed by shot blasting before the powder is present in the sintered magnet body.
また、上記吸収処理あるいはそれに続く時効処理を施した磁石に対して、アルカリ、酸あるいは有機溶剤のいずれか１種以上により洗浄したり、実用形状に研削することもできる。更には、かかる吸収処理、時効処理、洗浄又は研削後にメッキ又は塗装を施すこともできる。 Further, the magnet subjected to the above-described absorption treatment or subsequent aging treatment can be washed with one or more of alkali, acid or organic solvent, or ground into a practical shape. Furthermore, plating or coating can be applied after such absorption treatment, aging treatment, washing or grinding.
本発明のスリットは、磁石表面に存在させたＲ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上を含有する粉末から磁石体へのＲ2、Ｒ3又はＲ4の吸収を高めるため以外に、永久磁石回転機に組み込まれた際には、永久磁石に生ずる渦電流を低減する働きがある。回転機において磁石に渦電流が生じる原因は、磁石と対向する電機子のスロットの相対位置が変化し、スロット部分で磁石内の磁束が時間変化することが１つの原因である。また、電機子で作る磁束の歪みが大きな場合も渦電流の原因である。渦電流は磁束変化を妨げる向きに導体上に発生する電流であり、磁石の磁束は磁気異方性化した方向に通り、渦電流は磁気異方性化した方向に対し直角な面に流れるので、スリットは渦電流経路を分断するために磁気異方性化した方向に対し直角な面に入れるのが効果的である。更に、渦電流経路が細長くなる方向にスリットを入れるとより効果が高まる。 Slits of the present invention, the oxide of R 2 which was present on the magnet surface, R 2 of a fluoride of R 3, a powder containing one or more kinds selected from an acid fluoride of R 4 to the magnet body In addition to increasing the absorption of R 3 or R 4 , when incorporated in a permanent magnet rotating machine, it functions to reduce eddy currents generated in the permanent magnet. One cause of the eddy current generated in the magnet in the rotating machine is that the relative position of the slot of the armature facing the magnet changes, and the magnetic flux in the magnet changes over time in the slot portion. In addition, when the distortion of magnetic flux generated by the armature is large, it is also a cause of eddy current. The eddy current is a current generated on the conductor in a direction that prevents the magnetic flux change. The magnetic flux of the magnet passes in the direction of magnetic anisotropy, and the eddy current flows in a plane perpendicular to the direction of magnetic anisotropy. In order to break the eddy current path, it is effective to put the slit in a plane perpendicular to the direction of magnetic anisotropy. Furthermore, if a slit is made in the direction in which the eddy current path becomes elongated, the effect is further enhanced.
スリットのない状態での焼結ブロックの最大部の寸法が１００ｍｍ以下、好ましくは５０ｍｍ以下で、かつ磁気異方性化した方向の寸法が１０ｍｍ以下、好ましくは５ｍｍ以下である場合には、スリットのない磁石体に対して本発明の磁石表面に存在させたＲ2の酸化物、Ｒ3のフッ化物、Ｒ4の酸フッ化物から選ばれる１種又は２種以上を含有する粉末から磁石体にＲ2、Ｒ3又はＲ4を吸収させることができる。この場合は吸収処理を行った後で磁石表面に複数のスリットを入れれば、永久磁石回転機に組み込まれた永久磁石に生ずる渦電流を低減することができる。 When the dimension of the maximum part of the sintered block without a slit is 100 mm or less, preferably 50 mm or less, and the dimension in the direction of magnetic anisotropy is 10 mm or less, preferably 5 mm or less, From a powder containing one or more selected from the R 2 oxide, R 3 fluoride, and R 4 oxyfluoride present on the magnet surface of the present invention to a non-magnetic body R 2 , R 3 or R 4 can be absorbed. In this case, if a plurality of slits are formed on the magnet surface after the absorption treatment, eddy currents generated in the permanent magnet incorporated in the permanent magnet rotating machine can be reduced.
スリットを設けることによりセグメント磁石の機械的強度が低下する。特に回転機にこの磁石を用いた場合は、高速回転で磁石に大きな遠心力が働くため、機械特性が良好でなければ磁石が破損して飛散してしまう。このような問題を解決するにはスリットに接着剤や樹脂等の非導電性物質を充填することにより機械強度の低下を補うのが好ましい。上記接着剤は耐熱性と接着強度を両立できるものが望ましく、例えばエポキシ系やアクリル系接着剤が挙げられる。 By providing the slit, the mechanical strength of the segment magnet is lowered. In particular, when this magnet is used in a rotating machine, a large centrifugal force acts on the magnet at high speed rotation, so that the magnet is damaged and scattered unless mechanical characteristics are good. In order to solve such a problem, it is preferable to compensate for a decrease in mechanical strength by filling the slit with a nonconductive material such as an adhesive or a resin. The adhesive preferably has both heat resistance and adhesive strength, and examples thereof include epoxy and acrylic adhesives.
以上のようにして得られた永久磁石材料は、永久磁石回転機に適した渦電流が小さく高い残留磁束密度と高い保磁力を有するＲ−Ｆｅ−Ｂ系焼結磁石及びこの磁石を用いた永久磁石回転機として利用できる。 The permanent magnet material obtained as described above is an R—Fe—B sintered magnet having a small eddy current suitable for a permanent magnet rotating machine, a high residual magnetic flux density and a high coercive force, and a permanent using this magnet. It can be used as a magnet rotating machine.
以下、本発明の具体的態様について実施例をもって詳述するが、本発明の内容はこれに限定されるものではない。なお、下記例で、酸化Ｄｙ又はフッ化Ｄｙによる磁石表面空間の占有率（存在率）は、粉末処理後の磁石質量増と粉末物質の真密度より算出した。 Hereinafter, specific embodiments of the present invention will be described in detail with reference to examples, but the content of the present invention is not limited thereto. In the following examples, the occupation ratio (existence ratio) of the magnet surface space by oxidation Dy or fluoride Dy was calculated from the increase in magnet mass after powder treatment and the true density of the powder substance.
［実施例１，２及び比較例１，２］
純度９９質量％以上のＮｄ、Ｃｏ、Ａｌ、Ｆｅメタルとフェロボロンを所定量秤量してＡｒ雰囲気中で高周波溶解し、この合金溶湯をＡｒ雰囲気中で銅製単ロールに注湯するいわゆるストリップキャスト法により薄板状の合金とした。得られた合金の組成はＮｄが１３．５原子％、Ｃｏが１．０原子％、Ａｌが０．５原子％、Ｂが５．８原子％、Ｆｅが残部であり、これを合金Ａと称する。合金Ａに水素を吸蔵させた後、真空排気を行いながら５００℃まで加熱して部分的に水素を放出させる、いわゆる水素粉砕により３０メッシュ以下の粗粉とした。更に純度９９質量％以上のＮｄ、Ｔｂ、Ｆｅ、Ｃｏ、Ａｌ、Ｃｕメタルとフェロボロンを所定量秤量し、Ａｒ雰囲気中で高周波溶解した後、鋳造した。得られた合金の組成はＮｄが２０原子％、Ｔｂが１０原子％、Ｆｅが２４原子％、Ｂが６原子％、Ａｌが１原子％、Ｃｕが２原子％、Ｃｏが残部であり、これを合金Ｂと称する。合金Ｂは窒素雰囲気中、ブラウンミルを用いて３０メッシュ以下に粗粉砕した。
[Examples 1 and 2 and Comparative Examples 1 and 2]
Nd, Co, Al, Fe metal having a purity of 99% by mass or more and ferroboron are weighed in predetermined amounts and melted at high frequency in an Ar atmosphere, and this molten alloy is poured into a single copper roll in an Ar atmosphere by a so-called strip casting method A thin plate-like alloy was used. The composition of the obtained alloy is 13.5 atomic% Nd, 1.0 atomic% Co, 0.5 atomic% Al, 5.8 atomic% B, and the balance Fe. Called. The alloy A was occluded with hydrogen and then heated to 500 ° C. while being evacuated to partially release hydrogen, so that a coarse powder of 30 mesh or less was obtained by so-called hydrogen pulverization. Further, Nd, Tb, Fe, Co, Al, Cu metal having a purity of 99% by mass or more and ferroboron were weighed in predetermined amounts, melted by high frequency in an Ar atmosphere, and then cast. The composition of the resulting alloy is Nd 20 atom%, Tb 10 atom%, Fe 24 atom%, B 6 atom%,
続いて、合金Ａ粉末を９０質量％、合金Ｂ粉末を１０質量％秤量して、窒素置換したＶブレンダー中で３０分間混合した。この混合粉末は高圧窒素ガスを用いたジェットミルにて、粉末の質量中位粒径４μｍに微粉砕された。得られた混合微粉末を窒素雰囲気下１５ｋＯｅの磁界中で配向させながら、約１ｔｏｎ／ｃｍ2の圧力で成形した。次いで、この成形体をＡｒ雰囲気の焼結炉内に投入し、１，０６０℃で２時間焼結し、７１ｍｍ×４６ｍｍ×厚み２１ｍｍ（磁気異方性化した方向）の磁石ブロックを作製した。磁石ブロックはダイヤモンドカッターにより７０ｍｍ×４５ｍｍ×２０ｍｍ（磁気異方性化した方向）に全面研削加工した。同時に磁気異方性化した方向に対し直角な７０ｍｍ×４５ｍｍの面に７０ｍｍ方向に幅０．５ｍｍ、深さ１５ｍｍのスリットを４．５ｍｍ間隔でつけた。研削加工された磁石体をアルカリ溶液で洗浄した後、酸洗浄して乾燥させた。各洗浄の前後には純水による洗浄工程が含まれている。 Subsequently, 90% by mass of the alloy A powder and 10% by mass of the alloy B powder were weighed and mixed for 30 minutes in a nitrogen-substituted V blender. This mixed powder was finely pulverized to a mass median particle size of 4 μm by a jet mill using high-pressure nitrogen gas. The obtained mixed fine powder was molded at a pressure of about 1 ton / cm 2 while being oriented in a magnetic field of 15 kOe under a nitrogen atmosphere. Next, this compact was put into a sintering furnace in an Ar atmosphere and sintered at 1,060 ° C. for 2 hours to produce a magnet block of 71 mm × 46 mm × thickness 21 mm (direction of magnetic anisotropy). The magnet block was ground to 70 mm × 45 mm × 20 mm (direction of magnetic anisotropy) with a diamond cutter. At the same time, slits having a width of 0.5 mm and a depth of 15 mm in the 70 mm direction were formed at intervals of 4.5 mm on a 70 mm × 45 mm surface perpendicular to the direction of magnetic anisotropy. The ground magnet body was washed with an alkaline solution, and then washed with an acid and dried. A cleaning process with pure water is included before and after each cleaning.
次に、平均粉末粒径が５μｍのフッ化ディスプロシウムを質量分率５０％でエタノールと混合し、これに超音波を印加しながら磁石体を１分間浸した。引き上げた磁石は直ちに熱風により乾燥させた。この時のフッ化ディスプロシウムによる磁石表面空間の占有率は４５％であった。これにＡｒ雰囲気中９００℃で１時間という条件で吸収処理を施し、更に５００℃で１時間時効処理して急冷することで、磁石体を得た。これを磁石体Ｍ１と称する。 Next, dysprosium fluoride having an average powder particle size of 5 μm was mixed with ethanol at a mass fraction of 50%, and the magnet body was immersed for 1 minute while applying ultrasonic waves thereto. The magnet pulled up was immediately dried with hot air. The occupation ratio of the magnet surface space by dysprosium fluoride at this time was 45%. This was subjected to an absorption treatment at 900 ° C. for 1 hour in an Ar atmosphere, and further subjected to an aging treatment at 500 ° C. for 1 hour, followed by rapid cooling to obtain a magnet body. This is referred to as a magnet body M1.
比較のためにスリットなしの磁石体に熱処理のみ施したもの、及びスリット入り磁石体に熱処理のみを施したものも作製した。これをＰ１、Ｐ２と称する。 For comparison, a magnet body without slits subjected only to heat treatment and a magnet body including slits subjected only to heat treatment were also produced. These are referred to as P1 and P2.
磁石体Ｍ１、Ｐ１、Ｐ２の磁気特性を表１に示した。ディスプロシウムの吸収処理を施していない磁石（Ｐ１とＰ２）の保磁力に対して本発明による磁石Ｍ１は４００ｋＡｍ-1の保磁力増大が認められる。また、残留磁束密度の低下は５ｍＴであった。比較のために、合金ＡのＮｄの一部をＤｙで置換した組成合金を用いて磁石を作製し、４００ｋＡｍ-1の保磁力増大を図ったところ、残留磁束密度は５０ｍＴ低下した。 Table 1 shows the magnetic characteristics of the magnet bodies M1, P1, and P2. The magnet M1 according to the present invention has an increase in coercive force of 400 kAm −1 with respect to the coercive force of the magnets (P1 and P2) not subjected to the dysprosium absorption treatment. The decrease in residual magnetic flux density was 5 mT. For comparison, when a magnet was prepared using a composition alloy in which a part of Nd of alloy A was replaced with Dy and the coercive force was increased by 400 kAm −1 , the residual magnetic flux density was reduced by 50 mT.
磁石体Ｍ１のＳＥＭによる反射電子像とＥＰＭＡにより、磁石にはＤｙ及びＦが観察された。処理前の磁石にはＤｙ及びＦは含まれていないので、磁性体Ｍ１におけるＤｙ及びＦの存在は、本発明の吸収処理によるものである。吸収されたＤｙは結晶粒界近傍にのみ濃化している。一方、フッ素（Ｆ）も粒界部に存在し、処理前から磁石内に含まれている不可避的不純物である酸化物と結合して酸フッ化物を形成している。このＤｙの分布により、残留磁束密度の低下を最小限に抑えながら保磁力を増大させることが可能となった。 Dy and F were observed in the magnet from the backscattered electron image and EPMA of the magnet body M1. Since the magnet before processing does not contain Dy and F, the presence of Dy and F in the magnetic body M1 is due to the absorption processing of the present invention. The absorbed Dy is concentrated only in the vicinity of the crystal grain boundary. On the other hand, fluorine (F) is also present in the grain boundary part, and forms an oxyfluoride by being combined with an oxide that is an inevitable impurity contained in the magnet before the treatment. This Dy distribution makes it possible to increase the coercive force while minimizing the decrease in residual magnetic flux density.
Ｍ１、Ｐ２と同じ形状のスリット入りの磁石体に対し、平均粉末粒径が５μｍのフッ化テルビウムを質量分率５０％でエタノールと混合し、これに超音波を印加しながら磁石体を１分間浸した。引き上げた磁石は直ちに熱風により乾燥させた。この時のフッ化テルビウムによる磁石表面空間の占有率は４５％であった。これにＡｒ雰囲気中９００℃で１時間という条件で吸収処理を施し、更に５００℃で１時間時効処理して急冷することで、磁石体を得た。これを磁石体Ｍ２と称する。 For a magnet body with slits having the same shape as M1 and P2, terbium fluoride with an average powder particle size of 5 μm is mixed with ethanol at a mass fraction of 50%, and the magnet body is held for 1 minute while applying ultrasonic waves thereto. Soaked. The magnet pulled up was immediately dried with hot air. At this time, the occupation ratio of the magnet surface space by terbium fluoride was 45%. This was subjected to an absorption treatment at 900 ° C. for 1 hour in an Ar atmosphere, and further subjected to an aging treatment at 500 ° C. for 1 hour, followed by rapid cooling to obtain a magnet body. This is referred to as a magnet body M2.
磁石体Ｍ２の磁気特性も表１に併記した。テルビウムの吸収処理を施していない磁石（Ｐ１とＰ２）の保磁力に対して本発明による磁石Ｍ２は６００ｋＡｍ-1の保磁力増大が認められる。また、残留磁束密度の低下は５ｍＴであった。 The magnetic properties of the magnet body M2 are also shown in Table 1. The magnet M2 according to the present invention has a coercive force increase of 600 kAm −1 with respect to the coercive force of the magnets (P1 and P2) not subjected to the terbium absorption treatment. The decrease in residual magnetic flux density was 5 mT.
［実施例１−１，２−１及び比較例１−１，２−１］
実施例１，２の磁石Ｍ１、Ｍ２及び比較例１，２の磁石Ｐ１、Ｐ２を永久磁石モータに組み込んだ時のモータ特性について説明する。永久磁石モータは図２に示す埋め込み磁石構造型モータである。ロータは、０．５ｍｍの電磁鋼板を積層したものに永久磁石が埋め込まれた４極構造で、ロータヨーク１１の寸法は外径３１２ｍｍ、高さ１８０ｍｍとなっている。永久磁石１２の寸法は、幅７０ｍｍ、磁気異方性化方向の寸法２０ｍｍ、軸方向の寸法１８０ｍｍである。焼結磁石で長さ１８０ｍｍの磁石は作製し難いので、今回は長さ４５ｍｍの磁石をエポキシ系接着剤で４個貼り合せた。ステータは、０．５ｍｍの電磁鋼板を積層した６スロット構造で、各ティースには集中巻きでコイルが６０ターン巻かれており、コイル１３はＵ相，Ｖ相，Ｗ相の３相Ｙ結線となっている。図２に示すＵ，Ｖ，Ｗの添え字の＋と−はコイルの巻き方向を示すもので、＋は紙面に対し出る方向、−は入る方向を意味する。ステータヨーク１４の寸法は外径５２０ｍｍ、内径３１５ｍｍ、高さ１８０ｍｍとなっている。ロータとステータの空隙は１．５ｍｍである。ロータとステータの位置関係が図２の状態で、Ｕ相に余弦波の交流電流、Ｖ相にＵ相より１２０°位相の進んだ交流電流、Ｗ相にＵ相より２４０°位相の進んだ交流電流を流すことで、永久磁石の磁束とコイルの磁束の相互作用でロータは反時計回りに回転する。埋め込み磁石構造型では、各相の電流の位相を制御することで更に大きなトルクを発生するという特徴をもつ。更に、残留磁束密度の大きいＲ−Ｆｅ−Ｂ系焼結磁石を用いるとモータは高出力高効率になるので家電用、産業用、自動車の駆動用など幅広い分野で使われている。図２のモータの場合、回転数２，４００ｒｐｍ、各相の実効値電流５０Ａで、電流の位相制御を行わない場合のトルクが３７０Ｎｍであったが、進み電流位相４０°で駆動すると４９０Ｎｍまでトルクが増加する。しかし、進み電流によってコイルから永久磁石に対向する磁束が増え、永久磁石は減磁しやすい状況に置かれ、減磁しないためにはある程度の保磁力が必要になる。また、永久磁石を通る磁束はロータの回転と共に時々刻々変化しており、この磁場変動により磁石内部に渦電流が発生する。渦電流損失は大きさの２乗に比例するので、今回のように断面が７０ｍｍ×４５ｍｍの磁石では問題になる。更に、進み電流によってコイルから永久磁石に対向する磁束が増えると磁石の渦電流損失が増えてしまう。このような理由から、永久磁石回転機に適した渦電流が小さく保磁力の大きなＲ−Ｆｅ−Ｂ系焼結磁石が望まれている。
[Examples 1-1 and 2-1 and Comparative Examples 1-1 and 2-1]
The motor characteristics when the magnets M1 and M2 of Examples 1 and 2 and the magnets P1 and P2 of Comparative Examples 1 and 2 are incorporated in a permanent magnet motor will be described. The permanent magnet motor is an embedded magnet structure type motor shown in FIG. The rotor has a quadrupole structure in which permanent magnets are embedded in a laminate of 0.5 mm electromagnetic steel plates. The rotor yoke 11 has an outer diameter of 312 mm and a height of 180 mm. The
磁石Ｍ１、Ｍ２、Ｐ１、Ｐ２の表面にエポキシ塗装を行い、４５ｍｍ方向をエポキシ系接着剤で４枚貼り合せてＭ１，Ｍ２，Ｐ２のスリットにエポキシ系接着剤を充填した後、着磁したものを図２のロータに組み込んだ。磁石Ｍ１，Ｍ２，Ｐ２それぞれを４枚貼り合せた状態の磁石を図３、磁石Ｐ１を４枚貼り合せた状態を図４に示す。図３と図４の寸法は本実施例と比較例では、幅Ｗ＝７０ｍｍ、厚さＴ＝２０ｍｍ、長さＬ＝１８０ｍｍ、スリットの深さＴＳ＝１５ｍｍ、スリット間の間隔ＬＳ＝４．５ｍｍである。磁石Ｍ１、Ｍ２、Ｐ１、Ｐ２を組み込んだモータをそれぞれＭＭ１、ＭＭ２、ＭＰ１、ＭＰ２とする。各相に実効値電流５０Ａ、電流位相４０°、２，４００ｒｐｍで１時間連続運転し、運転直後のトルクと連続運転の後、十分冷えた状態で再度運転した時のトルクの比から、永久磁石の減磁量を評価した。結果を表２にまとめた。実施例のＭＭ１とＭＭ２については減磁が起こっていない。しかし、比較例のＭＰ１とＭＰ２は永久磁石の保磁力が低く減磁してしまっている。ＭＰ１については渦電流による発熱の影響が加わって更に大きく減磁してしまった。 The magnets M1, M2, P1, and P2 are coated with epoxy, 45mm direction is bonded with epoxy adhesive, the slits of M1, M2, and P2 are filled with epoxy adhesive, and then magnetized Was incorporated into the rotor of FIG. FIG. 3 shows a state where four magnets M1, M2 and P2 are bonded together, and FIG. 4 shows a state where four magnets P1 are bonded together. 3 and 4 show the width W = 70 mm, the thickness T = 20 mm, the length L = 180 mm, the slit depth TS = 15 mm, and the interval LS between slits LS = 4.5 mm in the present embodiment and the comparative example. It is. Motors incorporating magnets M1, M2, P1, and P2 are designated as MM1, MM2, MP1, and MP2, respectively. Permanent magnet based on the ratio of torque immediately after operation for 1 hour at RMS current 50A, current phase 40 °, 2,400 rpm for each phase, and torque when it is restarted in a sufficiently cooled state after continuous operation The amount of demagnetization was evaluated. The results are summarized in Table 2. No demagnetization has occurred in the MM1 and MM2 of the example. However, MP1 and MP2 of the comparative example are demagnetized because the coercive force of the permanent magnet is low. MP1 was further demagnetized due to the effect of heat generation by eddy current.
［実施例３，４及び比較例３，４］
実施例１、２と同様な方法で図５に示すような幅８０ｍｍ、高さ４５ｍｍ、磁気異方性方向の最大厚み１０ｍｍのＣ形磁石を半分にした形状の磁石体を作製し、図６のようにクシ歯状に幅０．５ｍｍ、深さ７０ｍｍのスリット２を４．５ｍｍ間隔で設けた。
次に、平均粉末粒径が５μｍのフッ化ディスプロシウムを質量分率５０％でエタノールと混合し、これに超音波を印加しながら磁石体を１分間浸した。引き上げた磁石は直ちに熱風により乾燥させた。この時のフッ化ディスプロシウムによる磁石表面空間の占有率は４５％であった。これにＡｒ雰囲気中９００℃で１時間という条件で吸収処理を施し、更に５００℃で１時間時効処理して急冷することで、磁石体を得た。これを磁石体Ｍ３と称する。また、フッ化ディスプロシウムの代わりにフッ化テルビウムを用いて同様の熱処理をしたものをＭ４とした。比較のためにスリット加工前の磁石体に熱処理のみ施したもの、及びスリット入り磁石体に熱処理のみを施したものも作製した。これをＰ３、Ｐ４と称する。
[Examples 3 and 4 and Comparative Examples 3 and 4]
A magnet body having a shape obtained by halving a C-shaped magnet having a width of 80 mm, a height of 45 mm, and a maximum thickness of 10 mm in the magnetic anisotropy direction as shown in FIG. Like this, slits 2 having a width of 0.5 mm and a depth of 70 mm were provided in a comb-like shape at intervals of 4.5 mm.
Next, dysprosium fluoride having an average powder particle size of 5 μm was mixed with ethanol at a mass fraction of 50%, and the magnet body was immersed for 1 minute while applying ultrasonic waves thereto. The magnet pulled up was immediately dried with hot air. The occupation ratio of the magnet surface space by dysprosium fluoride at this time was 45%. This was subjected to an absorption treatment at 900 ° C. for 1 hour in an Ar atmosphere, and further subjected to an aging treatment at 500 ° C. for 1 hour to rapidly cool, thereby obtaining a magnet body. This is referred to as a magnet body M3. Moreover, what carried out the same heat processing using terbium fluoride instead of dysprosium fluoride was set to M4. For comparison, a magnet body that had been subjected only to heat treatment on the magnet body before slit processing and a magnet body that had been subjected to only heat treatment were also produced. These are referred to as P3 and P4.
磁石体Ｍ３、Ｍ４、Ｐ３、Ｐ４の磁気特性を表３に示した。ディスプロシウムの吸収処理を施した本発明による磁石Ｍ３は、処理していない磁石（Ｐ３とＰ４）の保磁力に対して４５０ｋＡｍ-1の保磁力増大が認められる。また、残留磁束密度の低下は５ｍＴであった。テルビウムの吸収処理を施した本発明による磁石Ｍ４は、６５０ｋＡｍ-1の保磁力増大が認められる。また、残留磁束密度の低下は５ｍＴであった。 Table 3 shows the magnetic characteristics of the magnet bodies M3, M4, P3, and P4. In the magnet M3 according to the present invention subjected to the dysprosium absorption treatment, a coercive force increase of 450 kAm −1 is recognized with respect to the coercivity of the untreated magnets (P3 and P4). The decrease in residual magnetic flux density was 5 mT. In the magnet M4 according to the present invention subjected to the terbium absorption treatment, an increase in coercive force of 650 kAm −1 is recognized. The decrease in residual magnetic flux density was 5 mT.
［実施例３−１，４−１及び比較例３−１，４−１］
実施例３，４の磁石Ｍ３、Ｍ４及び比較例３，４の磁石Ｐ３、Ｐ４を永久磁石モータに組み込んだ時のモータ特性について説明する。永久磁石モータは図７に示す表面磁石構造型モータである。ロータは、０．５ｍｍの電磁鋼板を積層したロータヨーク２１の表面にＣ形の永久磁石２２が置かれた４極構造で、ロータ寸法は外径３１２ｍｍ、高さ１８０ｍｍとなっている。永久磁石２２の寸法は、幅１６０ｍｍ、磁気異方性化した方向の寸法は中央部分で１０ｍｍ、端部で３ｍｍ、軸方向の寸法１８０ｍｍである。焼結磁石で幅１６０ｍｍや長さ１８０ｍｍの磁石は作製し難いので、今回は幅方向に２個、長さ方向に４個、合計８個のセグメントをエポキシ系接着剤で貼り合せた。ステータは実施例１−１で説明したものと同じ物であり、詳細の説明は省略する。実効値電流５０Ａ、電流位相０°、２，４００ｒｐｍで３９０Ｎｍのトルクを発生させた。表面磁石構造型モータは、入力電流に対しトルクが線形に変化しトルクや回転数の制御性が非常に良いので、高精度制御を求められる家電用、産業用、自動車用など幅広い分野で使われている。しかし、表面磁石構造型では、永久磁石にはコイルからの反磁界が直接入るので減磁しやすい状況に置かれ、減磁しないためにはある程度の保磁力が必要になる。また、磁石内部の磁束がロータが回転すると対向するステータのスロット部分で急激な変化を起こすので、磁石内部に大きな渦電流が発生する。渦電流損失は大きさの２乗に比例するので、今回のように断面が８０ｍｍ×４５ｍｍの磁石では問題になる。このような理由から、渦電流が小さく保磁力の大きなＲ−Ｆｅ−Ｂ系焼結磁石が望まれている。
[Examples 3-1, 4-1 and Comparative examples 3-1, 4-1]
The motor characteristics when the magnets M3 and M4 of Examples 3 and 4 and the magnets P3 and P4 of Comparative Examples 3 and 4 are incorporated in a permanent magnet motor will be described. The permanent magnet motor is a surface magnet structure type motor shown in FIG. The rotor has a quadrupole structure in which a C-shaped permanent magnet 22 is placed on the surface of a rotor yoke 21 in which 0.5 mm electromagnetic steel plates are laminated. The rotor has an outer diameter of 312 mm and a height of 180 mm. The dimensions of the permanent magnet 22 are 160 mm in width, the dimension in the direction of magnetic anisotropy is 10 mm at the center, 3 mm at the end, and 180 mm in the axial direction. Since it is difficult to produce a magnet having a width of 160 mm and a length of 180 mm with a sintered magnet, this time, two segments in the width direction and four in the length direction were bonded together with an epoxy adhesive. The stator is the same as that described in Example 1-1, and detailed description thereof is omitted. A torque of 390 Nm was generated at an effective current of 50 A, a current phase of 0 °, and 2,400 rpm. Surface magnet structured motors are used in a wide range of fields such as home appliances, industrial applications, and automobiles where high-precision control is required because the torque varies linearly with the input current and the controllability of torque and rotation speed is very good. ing. However, in the surface magnet structure type, since the demagnetizing field from the coil directly enters the permanent magnet, the permanent magnet is easily demagnetized. In order not to demagnetize, some coercive force is required. In addition, when the magnetic flux inside the magnet rotates, the abrupt change occurs in the slot portion of the facing stator, so that a large eddy current is generated inside the magnet. Since the eddy current loss is proportional to the square of the size, a problem arises with a magnet having a cross section of 80 mm × 45 mm as in this case. For these reasons, an R—Fe—B based sintered magnet having a small eddy current and a large coercive force is desired.
磁石Ｍ３、Ｍ４、Ｐ３、Ｐ４の表面にエポキシ塗装を行い、エポキシ系接着剤で８枚貼り合せて図８，図９に示すようなＣ形磁石を作った。更にＭ３，Ｍ４，Ｐ４のスリットにはエポキシ系接着剤を充填した。これを着磁し、図７のロータに組み込んだ。なお、図８は磁石Ｍ３，Ｍ４，Ｐ４それぞれを８枚貼り合せた状態で、図９は磁石Ｐ３を８枚貼り合せた状態である。本実施例では磁石の幅が１６０ｍｍと大きかったので幅方向が２分割された構造であるが、１００ｍｍ以下のものであれば幅方向に分割のないＣ形磁石にスリットを入れたものでもよい。図８と図９の寸法は本実施例と比較例では、Ｗ＝１６０ｍｍ、Ｔ＝１０ｍｍ、Ｌ＝１８０ｍｍ、スリットＷＳ＝１４０ｍｍ、スリット間の間隔ＬＳ＝４．５ｍｍである。磁石Ｍ３、Ｍ４、Ｐ３、Ｐ４を組み込んだモータをそれぞれＭＭ３、ＭＭ４、ＭＰ３、ＭＰ４とする。実効値電流５０Ａ、電流位相０°、２，４００ｒｐｍで１時間連続運転し、運転直後のトルクと連続運転の後、十分冷えた状態で再度運転した時のトルクの比から、永久磁石の減磁量を評価した。結果を表４にまとめた。比較例のＭＰ３とＭＰ４は永久磁石の保磁力が低く、大きな減磁が起こってしまった。ＭＰ３については渦電流による発熱の影響が加わって更に大きく減磁してしまった。これに対し、実施例のＭＭ３で約８％の減磁が起こった。このモータで減磁を起こさないためには更に保磁力が大きな材料が必要であることが分かる。そこで実施例のＭＭ３より大きな保磁力を得ているＭＭ４を用いると、全く減磁が起こっていない。 Epoxy coating was performed on the surfaces of the magnets M3, M4, P3, and P4, and eight sheets were bonded with an epoxy adhesive to form a C-shaped magnet as shown in FIGS. Further, the M3, M4, and P4 slits were filled with an epoxy adhesive. This was magnetized and incorporated into the rotor of FIG. 8 shows a state in which eight magnets M3, M4, and P4 are bonded, and FIG. 9 shows a state in which eight magnets P3 are bonded. In the present embodiment, the width of the magnet is as large as 160 mm, so that the width direction is divided into two. However, if it is 100 mm or less, a C-shaped magnet that is not divided in the width direction may be slit. The dimensions of FIGS. 8 and 9 are W = 160 mm, T = 10 mm, L = 180 mm, slit WS = 140 mm, and the interval LS between slits LS = 4.5 mm in this embodiment and the comparative example. The motors incorporating the magnets M3, M4, P3, and P4 are referred to as MM3, MM4, MP3, and MP4, respectively. The permanent magnet is demagnetized from the ratio of the torque immediately after operation for 1 hour at an effective current of 50 A, current phase of 0 °, 2,400 rpm, and the torque at the time of continuous operation after the operation is sufficiently cooled. The amount was evaluated. The results are summarized in Table 4. In the comparative examples MP3 and MP4, the coercive force of the permanent magnet was low, and a large demagnetization occurred. MP3 was further demagnetized due to the effect of heat generation by eddy current. On the other hand, about 8% demagnetization occurred in the MM3 of the example. It can be seen that a material having a larger coercive force is necessary to prevent demagnetization by this motor. Therefore, when MM4 having a coercive force larger than that of MM3 of the embodiment is used, no demagnetization occurs.
なお、上記実施例は永久磁石モータであるが、永久磁石発電機も同じ構造であり、本発明の効果は同様である。 In addition, although the said Example is a permanent magnet motor, a permanent magnet generator is also the same structure and the effect of this invention is the same.
１ 焼結磁石体
１ａ スリット形成面
１ｂ スリット形成面と反対の面
２ スリット
３ 吸収処理が起こり難い領域
１１、２１ ロータヨーク
１２、２２ 永久磁石
１３ コイル
１４ ステータヨーク
DESCRIPTION OF
Claims (18)
The permanent magnet rotating machine according to claim 17, wherein a slit provided on the surface of the rare earth permanent magnet is filled with a non-conductive substance.
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