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JP2005163066A - Apparatus for manufacturing alloy powder for permanent magnet and method therefor - Google Patents

Apparatus for manufacturing alloy powder for permanent magnet and method therefor Download PDF

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JP2005163066A
JP2005163066A JP2003400413A JP2003400413A JP2005163066A JP 2005163066 A JP2005163066 A JP 2005163066A JP 2003400413 A JP2003400413 A JP 2003400413A JP 2003400413 A JP2003400413 A JP 2003400413A JP 2005163066 A JP2005163066 A JP 2005163066A
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alloy powder
heat treatment
hydrogen
alloy
inert gas
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JP4101737B2 (en
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Motoaki Hosako
元彰 宝迫
Masaatsu Hatta
誠厚 八田
Takashi Inoue
隆 井上
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TDK Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To efficiently realize dehydrogenation in a heat-treating portion. <P>SOLUTION: A method for manufacturing an alloy powder for a permanent magnet comprises the steps of: making an alloy slug of a raw material containing a rare earth element, a metallic element and boron occlude hydrogen; and pulverizing it into the alloy powder. The apparatus is provided with a rotatable heat-treating portion for dehydrogenating the alloy powder having occluded hydrogen by heating. The heat-treating portion has an inert-gas-feeding mechanism for introducing an inert gas to the inside during treatment. The apparatus dehydrogenates the alloy powder having occluded hydrogen by heating while rotating the heat-treating portion and introducing an inert gas into the heat-treating portion. Since hydrogen released from the alloy powder is immediately exhausted together with the inert gas, dehydrogenation is efficiently realized. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は、希土類焼結磁石等の永久磁石を製造する際に用いられる合金粉末の製造装置及び製造方法に関するものであり、特に、水素吸蔵による粉砕に際し、効率的且つ確実に脱水素を行うための技術に関する。   The present invention relates to an apparatus and method for producing an alloy powder used when producing a permanent magnet such as a rare earth sintered magnet, and in particular, for performing dehydrogenation efficiently and reliably at the time of pulverization by hydrogen storage. Related to technology.

例えばNd−Fe−B磁石等のR−B−M系(Rは、Yを含む希土類元素の1種以上である。Mは、Feを必須とし、その他金属元素を含む。)焼結磁石は、磁気特性に優れていること、主成分であるNdが資源的に豊富で比較的安価であること等の利点を有することから、近年、その需要は益々拡大する傾向にある。このような状況から、R−B−M系焼結磁石の磁気特性を向上するための研究開発や、品質の高い希土類焼結磁石を製造するための製造方法の改良等が各方面において進められている。   For example, an R—B—M system such as an Nd—Fe—B magnet (R is one or more of rare earth elements including Y. M is essential for Fe and contains other metal elements). In recent years, the demand has tended to increase more and more because it has advantages such as excellent magnetic properties and Nd as a main component, which is abundant in resources and relatively inexpensive. Under these circumstances, research and development for improving the magnetic properties of RBM type sintered magnets and improvement of manufacturing methods for producing high-quality rare earth sintered magnets have been promoted in various directions. ing.

希土類焼結磁石の製造方法としては、焼結法が一般的であり、溶解→鋳造→合金塊粗粉砕→微粉砕→プレス→焼結の各工程からなるプロセスが広く適用され、ある程度高い磁石特性が得られている(例えば、特許文献1等を参照)。ただし、前述のようなプロセスにより焼結磁石を製造する場合、合金塊粉砕に手間がかかるため生産性が低いという問題がある。   As a manufacturing method of rare earth sintered magnets, the sintering method is generally used, and a process consisting of melting, casting, alloy lump coarse pulverization, fine pulverization, press, and sintering is widely applied, and a certain degree of magnet characteristics is obtained. (See, for example, Patent Document 1). However, when a sintered magnet is manufactured by the process as described above, there is a problem that productivity is low because it takes time to grind the alloy lump.

すなわち、合金塊の粉砕を容易に行なうために、従来、水素吸蔵粉砕が利用されている。水素吸蔵粉砕では、水素を吸蔵した合金にクラックが生じて自己崩壊的に粉末化が進行する。また、水素吸蔵は、合金の耐酸化性を向上する上でも有効である。しかしながら、静止した容器中において原料合金塊に水素を吸蔵させ、次いで熱処理を施した場合、表面付近は粉末化するものの、中心部付近まで粉末化することは難しい。このため塊状の合金が残ってしまうという不都合がある。   That is, hydrogen storage and pulverization has been conventionally used to easily pulverize the alloy lump. In hydrogen occlusion and pulverization, cracks occur in the alloy that occludes hydrogen, and powdering proceeds in a self-destructive manner. Hydrogen storage is also effective in improving the oxidation resistance of the alloy. However, when hydrogen is occluded in the raw material alloy lump in a stationary container and then subjected to heat treatment, the vicinity of the surface is pulverized, but it is difficult to pulverize to the vicinity of the center. For this reason, there is an inconvenience that a massive alloy remains.

また、特に複数の合金塊を同時に処理する場合、水素吸蔵工程及び熱処理工程において合金塊を均等に加熱することが難しく、合金の処理温度にばらつきが生じ易い。これら塊状の合金の残存や処理温度のばらつきは、焼結磁石を効率的に製造する上で大きな障害となり、得られる焼結磁石の特性を損なう原因ともなる。   In particular, when a plurality of alloy ingots are processed at the same time, it is difficult to uniformly heat the alloy ingots in the hydrogen storage step and the heat treatment step, and the alloy processing temperature tends to vary. Residues of these massive alloys and variations in processing temperatures are a major obstacle to the efficient production of sintered magnets, and the characteristics of the obtained sintered magnets are impaired.

さらに、従来の装置では、処理用の容器への合金塊の投入、合金粉末の払い出しが必要であるため、自動化ライン内へのこれらの処理の組み込みが難しいという問題もある。   Furthermore, the conventional apparatus requires the introduction of the alloy lump into the processing container and the discharge of the alloy powder, which makes it difficult to incorporate these processes into the automated line.

そこで、これらの課題を解決する方法として、本願出願人は、容器に運動を加えることで効率的な水素吸蔵粉砕工程を実現することを既に提案している(特許文献2参照)。特許文献2記載の方法では、水素吸蔵工程及び熱処理工程において、合金塊が封入された容器に回転、揺動、振動等の運動を与えることにより、合金塊同士や合金塊の容器の内壁とを衝突させ、合金塊の破砕や粉砕を行うようにしている。
特開昭59−46008号公報 特開平4−147908号公報
Thus, as a method for solving these problems, the applicant of the present application has already proposed that an efficient hydrogen storage and pulverization process is realized by applying motion to the container (see Patent Document 2). In the method described in Patent Document 2, in the hydrogen occlusion process and the heat treatment process, by giving motions such as rotation, swinging, and vibration to the container in which the alloy lump is enclosed, the alloy lumps and the inner wall of the alloy lump container are formed. It is made to collide and crush and crush the alloy lump.
JP 59-46008 A JP-A-4-147908

ところで、先の特許文献2記載の技術では、水素吸蔵後の熱処理工程を、真空中、あるいは不活性雰囲気中で行うとある。ここで、例えば熱処理工程を真空中で行おうとすると、熱処理部内に周囲の空気が浸入する可能性が高く、合金粉末を酸化して特性を劣化する原因になる。また、放出される水素に空気が混入することは、安全性の観点からも好ましいものではない。一方、熱処理部内を不活性ガスで置換して脱水素を行う場合、放出される水素により、熱処理部内の水素濃度が次第に高くなり、効率的な脱水素の妨げとなる。   By the way, in the technique of previous patent document 2, it is said that the heat treatment process after hydrogen occlusion is performed in a vacuum or in an inert atmosphere. Here, for example, if the heat treatment step is performed in a vacuum, there is a high possibility that ambient air will enter the heat treatment portion, which causes the alloy powder to be oxidized and deteriorate the characteristics. Moreover, it is not preferable from the viewpoint of safety that air is mixed into the released hydrogen. On the other hand, when dehydrogenation is performed by substituting the inside of the heat treatment part with an inert gas, the hydrogen concentration in the heat treatment part gradually increases due to the released hydrogen, thereby preventing efficient dehydrogenation.

本発明は、このような従来の実情に鑑みて提案されたものであり、酸化による特性劣化を回避することができ、しかも効率的な脱水素を実現することが可能な永久磁石用合金粉末の製造装置及び製造方法を提供することを目的とする。   The present invention has been proposed in view of such a conventional situation, and it is possible to avoid deterioration of characteristics due to oxidation and to achieve efficient dehydrogenation of permanent magnet alloy powder. An object is to provide a manufacturing apparatus and a manufacturing method.

上述の目的を達成するために、本発明の永久磁石用合金粉末の製造装置は、希土類元素、金属元素及びホウ素を含む原料合金塊に水素を吸蔵させ、これを粉砕して合金粉末とする永久磁石用合金粉末の製造装置であって、水素吸蔵した合金粉末を加熱し脱水素する回転可能な熱処理部を備え、当該熱処理部は、処理時に内部に不活性ガスを導入するための不活性ガス供給機構を有することを特徴とする。   In order to achieve the above-described object, the permanent magnet alloy powder manufacturing apparatus of the present invention has a permanent alloy powder containing hydrogen stored in a raw material alloy lump containing a rare earth element, a metal element, and boron, and pulverized. A magnet alloy powder manufacturing apparatus comprising a rotatable heat treatment part for heating and dehydrogenating a hydrogen-occluded alloy powder, the heat treatment part for introducing an inert gas into the interior at the time of treatment. It has a supply mechanism.

また、本発明の永久磁石用合金粉末の製造方法は、希土類元素、金属元素及びホウ素を含む原料合金塊に水素を吸蔵させ、これを粉砕して合金粉末とする永久磁石用合金粉末の製造方法において、熱処理部を回転させるとともに、熱処理部内に不活性ガスを導入しながら水素吸蔵した合金粉末を加熱し脱水素することを特徴とする。   The method for producing an alloy powder for permanent magnets according to the present invention is a method for producing an alloy powder for permanent magnets in which hydrogen is occluded in a raw material alloy block containing rare earth elements, metal elements and boron, and pulverized into alloy powders. The heat treatment part is rotated, and the alloy powder stored with hydrogen is heated and dehydrogenated while introducing an inert gas into the heat treatment part.

水素吸蔵による粗粉砕において、合金塊は、水素ガスと接触することにより表面付近にクラックを生じ、表面付近が次々に粉末化する。このとき、粉末化した部分が表面から次々に崩落し、合金塊の破砕ないし粉砕が進む。そして、水素吸蔵後には、合金粉末に含まれる水素を脱水素するための熱処理を行うが、この熱処理を真空中で行うと、空気の浸入による合金粉末の酸化や、水素に空気が混入することによる安全面での課題が問題となる。また、雰囲気を不活性ガスで置換しただけでは、効率的な脱水素は難しい。   In coarse pulverization by hydrogen storage, the alloy lump is cracked near the surface by contact with hydrogen gas, and the vicinity of the surface is pulverized one after another. At this time, the powdered portion collapses from the surface one after another, and the alloy lump is crushed or crushed. After the hydrogen storage, a heat treatment for dehydrogenating the hydrogen contained in the alloy powder is performed. If this heat treatment is performed in a vacuum, the alloy powder is oxidized by the intrusion of air and air is mixed into the hydrogen. Safety issues due to Moreover, efficient dehydrogenation is difficult only by replacing the atmosphere with an inert gas.

本発明においては、熱処理部に不活性ガス供給機構を設け、熱処理部内に不活性ガスを流しながら熱処理を行うようにしているので、放出された水素は不活性ガスとともに速やかに排出され、効率的な脱水素が実現される。また、熱処理部には常に新たな不活性ガスが導入されるので、熱処理部内に空気が浸入することはない。   In the present invention, an inert gas supply mechanism is provided in the heat treatment section so that the heat treatment is performed while flowing the inert gas in the heat treatment section. Therefore, the released hydrogen is quickly discharged together with the inert gas, and is efficient. Dehydrogenation is realized. Moreover, since a new inert gas is always introduced into the heat treatment part, air does not enter the heat treatment part.

したがって、装置の大きさに対して処理能力が大幅に改善され、熱処理部を通過させることで、合金粉末の脱水素が円滑に進行し、合金粉末からほぼ完全に水素が除去される。連続処理を行う自動化ラインへの組み込みも容易である。   Therefore, the processing capacity is greatly improved with respect to the size of the apparatus, and the dehydrogenation of the alloy powder proceeds smoothly by passing through the heat treatment section, and hydrogen is almost completely removed from the alloy powder. It is easy to incorporate into an automated line for continuous processing.

本発明によれば、効率的な脱水素を実現し得る永久磁石用合金粉末の製造装置及び製造方法を提供することが可能である。また、本発明によれば、合金粉末の酸化による特性劣化を抑えることができ、安全性の確保も可能である。さらに、装置の大きさに対して処理能力を大幅に向上させることが可能であり、自動化も容易である。   ADVANTAGE OF THE INVENTION According to this invention, it is possible to provide the manufacturing apparatus and manufacturing method of the alloy powder for permanent magnets which can implement | achieve efficient dehydrogenation. Further, according to the present invention, characteristic deterioration due to oxidation of the alloy powder can be suppressed, and safety can be ensured. Furthermore, the processing capability can be greatly improved with respect to the size of the apparatus, and automation is easy.

以下、本発明を適用した永久磁石用合金粉末の製造装置及び製造方法について、図面を参照して詳細に説明する。   Hereinafter, the manufacturing apparatus and manufacturing method of the permanent magnet alloy powder to which this invention is applied are demonstrated in detail with reference to drawings.

本発明の製造装置、製造方法において、製造対象となる永久磁石用合金粉末は、希土類焼結磁石の製造に用いられるものである。そこで、先ず、この希土類焼結磁石及びその製造方法について概略説明する。   In the production apparatus and production method of the present invention, the alloy powder for permanent magnets to be produced is used for the production of rare earth sintered magnets. First, the rare earth sintered magnet and the manufacturing method thereof will be outlined.

希土類焼結磁石は、希土類元素、遷移金属元素及びホウ素を主成分とするものである。ここで、磁石組成(合金組成)は、目的に応じて任意に選択すればよい。例えば、R−T−B(Rは希土類元素の1種又は2種以上、但し希土類元素はYを含む概念である。TはFeまたはFe及びCoを必須とする遷移金属元素の1種または2種以上であり、Bはホウ素である。)系希土類焼結磁石とする場合、磁気特性に優れた希土類焼結磁石を得るためには、焼結後の磁石組成において、希土類元素Rが20〜40重量%、ホウ素Bが0.5〜4.5重量%、残部が遷移金属元素Tとなるような配合組成とすることが好ましい。ここで、Rは、希土類元素、すなわちY、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Yb及びLuから選ばれる1種、または2種以上である。中でも、Ndは、資源的に豊富で比較的安価であることから、主成分をNdとすることが好ましい。また、Dyの含有は異方性磁界を増加させるため、保磁力Hcjを向上させる上で有効である。   The rare earth sintered magnet is mainly composed of rare earth elements, transition metal elements and boron. Here, the magnet composition (alloy composition) may be arbitrarily selected according to the purpose. For example, R-T-B (R is a concept including one or more rare earth elements, where the rare earth element includes Y. T is one or two of transition metal elements essential for Fe or Fe and Co. In order to obtain a rare earth sintered magnet having excellent magnetic properties, the rare earth element R is 20 to 20 in the magnet composition after sintering. It is preferable that the composition be such that 40% by weight, boron B is 0.5 to 4.5% by weight, and the balance is the transition metal element T. Here, R is one or more selected from rare earth elements, that is, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb, and Lu. Especially, since Nd is abundant in resources and relatively inexpensive, the main component is preferably Nd. Further, the inclusion of Dy is effective in improving the coercive force Hcj because it increases the anisotropic magnetic field.

あるいは、添加元素Mを加えて、R−T−B−M系希土類焼結磁石とすることも可能である。この場合、添加元素Mとしては、Al、Cr、Mn、Mg、Si、Cu、C、Nb、Sn、W、V、Zr、Ti、Mo、Bi、Ga等を挙げることができ、これらの1種または2種以上を選択して添加することができる。これら添加元素Mの添加量は、残留磁束密度等の磁気特性を考慮して、3重量%以下とすることが好ましい。添加元素Mの添加量が多すぎると、磁気特性が劣化するおそれがある。   Alternatively, the additive element M can be added to form an R-T-B-M rare earth sintered magnet. In this case, examples of the additive element M include Al, Cr, Mn, Mg, Si, Cu, C, Nb, Sn, W, V, Zr, Ti, Mo, Bi, and Ga. A seed | species or 2 or more types can be selected and added. The addition amount of these additional elements M is preferably 3% by weight or less in consideration of magnetic characteristics such as residual magnetic flux density. If the amount of additive element M added is too large, the magnetic properties may be deteriorated.

勿論、これら組成に限らず、希土類焼結磁石として従来公知の組成全般に適用可能であることは言うまでもない。   Of course, it is needless to say that the present invention is not limited to these compositions, and can be applied to all known compositions as rare earth sintered magnets.

上述の希土類焼結磁石を製造するには、粉末冶金法が採用される。以下、希土類焼結磁石の粉末冶金法による製造方法について説明する。   Powder metallurgy is employed to produce the rare earth sintered magnet described above. Hereinafter, a method for producing a rare earth sintered magnet by powder metallurgy will be described.

図1は、粉末冶金法による希土類焼結磁石の製造プロセスの一例を示すものである。この製造プロセスは、基本的には、合金化工程1、粗粉砕工程2、微粉砕工程3、磁場中成形工程4、焼結工程5、時効工程6、加工工程7、及び表面処理工程8とにより構成される。なお、酸化防止のために、時効後までの各工程は、ほとんどの工程を真空中、あるいは不活性ガス雰囲気中(窒素雰囲気中、Ar雰囲気中等)で行う。   FIG. 1 shows an example of a process for producing a rare earth sintered magnet by powder metallurgy. This manufacturing process basically includes an alloying step 1, a coarse pulverizing step 2, a fine pulverizing step 3, a magnetic field forming step 4, a sintering step 5, an aging step 6, a processing step 7, and a surface treatment step 8. Consists of. In order to prevent oxidation, most of the steps until aging are performed in vacuum or in an inert gas atmosphere (in a nitrogen atmosphere, an Ar atmosphere, etc.).

合金化工程1では、原料となる金属、あるいは合金を磁石組成に応じて配合し、真空あるいは不活性ガス、例えばAr雰囲気中で溶解し、鋳造することにより合金化する。鋳造法としては、溶融した高温の液体金属を回転ロール上に供給し、合金薄板を連続的に鋳造するストリップキャスト法(連続鋳造法)が生産性等の観点から好適であるが、本発明はそれに限ったものではない。原料金属(合金)としては、純希土類元素、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。凝固偏析を解消すること等を目的に、必要に応じて溶体化処理を行ってもよい。溶体化処理の条件としては、例えば真空またはAr雰囲気下、700〜1500℃領域で1時間以上保持する。   In the alloying step 1, a metal or alloy as a raw material is blended according to the magnet composition, melted in a vacuum or an inert gas, for example, Ar atmosphere, and cast into an alloy. As a casting method, a strip casting method (continuous casting method) in which molten high-temperature liquid metal is supplied onto a rotating roll and an alloy thin plate is continuously cast is preferable from the viewpoint of productivity and the like. It is not limited to that. As the raw material metal (alloy), pure rare earth elements, rare earth alloys, pure iron, ferroboron, and alloys thereof can be used. A solution treatment may be performed as necessary for the purpose of eliminating solidification segregation. As a condition for the solution treatment, for example, it is held in a 700 to 1500 ° C. region for 1 hour or more under vacuum or Ar atmosphere.

合金は、ほぼ最終磁石組成である単一の合金を用いても良いし、最終磁石組成になるように、組成の異なる複数種類の合金を混合しても良い。混合は、合金・原料粗粉・原料微粉のどの工程でもよいが、混合性を考慮すると合金での混合が望ましい。   As the alloy, a single alloy having almost the final magnet composition may be used, or a plurality of types of alloys having different compositions may be mixed so as to have the final magnet composition. Mixing may be performed in any process of alloy, raw material coarse powder, and raw material fine powder, but in consideration of mixing properties, mixing with an alloy is desirable.

粗粉砕工程2では、先ず、鋳造した原料合金の薄板、あるいはインゴット等をある程度粉砕して、合金塊とし、水素吸蔵に供する。合金塊の寸法、形状に特に制限はないが、5〜100mm角程度とすることが好ましい。この粉砕は、例えばジョークラッシャ等により行えばよい。   In the coarse pulverization step 2, first, the cast raw alloy sheet or ingot is pulverized to some extent to form an alloy lump and used for hydrogen storage. Although there is no restriction | limiting in particular in the dimension and shape of an alloy lump, It is preferable to set it as about 5-100 mm square. This pulverization may be performed by, for example, a jaw crusher.

粗粉砕工程2では、前記合金塊に対して水素吸蔵させ、粉砕を行う。原料合金塊に水素を吸蔵させると、相によって水素吸蔵量が異なり、これにより表面から自己崩壊的に粉砕が進行する。粗粉砕工程2では、前記水素吸蔵処理の後、熱処理により合金粉末の脱水素を行い、脱水素後の合金粉末を冷却して取り出す。   In the coarse pulverization step 2, the alloy lump is occluded with hydrogen and pulverized. When hydrogen is occluded in the raw material alloy lump, the hydrogen occlusion amount differs depending on the phase, and pulverization proceeds from the surface in a self-destructive manner. In the coarse pulverization step 2, after the hydrogen storage treatment, the alloy powder is dehydrogenated by heat treatment, and the dehydrogenated alloy powder is cooled and taken out.

前述の粗粉砕工程2が終了した後、通常、粗粉砕した原料合金粉末に粉砕助剤を添加する。粉砕助剤としては、例えば脂肪酸系化合物等を使用することができるが、特に、脂肪酸アミドを粉砕助剤として用いることで、良好な磁気特性を有する希土類焼結磁石を得ることができる。粉砕助剤の添加量としては、0.03〜0.4重量%とすることが好ましい。この範囲内で粉砕助剤を添加した場合、焼結後の残留炭素の量を低減することができ、希土類焼結磁石の磁気特性を向上させる上で有効である。   After the coarse pulverization step 2 is completed, a pulverization aid is usually added to the coarsely pulverized raw material alloy powder. As the grinding aid, for example, a fatty acid compound or the like can be used. In particular, by using a fatty acid amide as the grinding aid, a rare earth sintered magnet having good magnetic properties can be obtained. The addition amount of the grinding aid is preferably 0.03 to 0.4% by weight. When the grinding aid is added within this range, the amount of residual carbon after sintering can be reduced, which is effective in improving the magnetic properties of the rare earth sintered magnet.

粗粉砕工程2の後、微粉砕工程3を行うが、この微粉砕工程3は、例えばジェットミルを使用して行われる。微粉砕の際の条件は、用いる気流式粉砕機に応じて適宜設定すればよく、原料合金粉末を平均粒径が1〜10μm程度、例えば3〜6μmとなるまで微粉砕する。ジェットミルは、高圧の不活性ガス(例えば窒素ガス)を狭いノズルより開放して高速のガス流を発生させ、この高速のガス流により粉体の粒子を加速し、粉体の粒子同士の衝突や、衝突板あるいは容器壁との衝突を発生させて粉砕する方法である。ジェットミルは、一般的に、流動層を利用するジェットミル、渦流を利用するジェットミル、衝突板を用いるジェットミル等に分類される。   After the coarse pulverization step 2, a fine pulverization step 3 is performed. The fine pulverization step 3 is performed using, for example, a jet mill. The conditions at the time of fine pulverization may be appropriately set according to the airflow pulverizer to be used, and the raw material alloy powder is finely pulverized until the average particle size becomes about 1 to 10 μm, for example, 3 to 6 μm. A jet mill opens a high-pressure inert gas (for example, nitrogen gas) from a narrow nozzle to generate a high-speed gas flow, accelerates powder particles by this high-speed gas flow, and collides powder particles with each other. Or, it is a method of crushing by generating a collision with a collision plate or a container wall. Jet mills are generally classified into jet mills that use fluidized beds, jet mills that use vortex flow, jet mills that use impingement plates, and the like.

微粉砕工程3の後、磁場中成形工程4において、原料合金微粉を磁場中にて成形する。具体的には、微粉砕工程3にて得られた原料合金微粉を電磁石を配置した金型内に充填し、磁場印加によって結晶軸を配向させた状態で磁場中成形する。磁場中成形は、縦磁場成形、横磁場成形のいずれであってもよい。この磁場中成形は、例えば800〜1500kA/mの磁場中で、130〜160MPa前後の圧力で行えばよい。   After the pulverizing step 3, in the forming step 4 in the magnetic field, the raw material alloy fine powder is formed in the magnetic field. Specifically, the raw material alloy fine powder obtained in the fine pulverization step 3 is filled in a mold in which an electromagnet is arranged, and is molded in a magnetic field with a crystal axis oriented by applying a magnetic field. Forming in the magnetic field may be either longitudinal magnetic field shaping or transverse magnetic field shaping. The forming in the magnetic field may be performed at a pressure of about 130 to 160 MPa in a magnetic field of 800 to 1500 kA / m, for example.

次に焼結工程5・時効工程6において、焼結及び時効処理を実施する。すなわち、焼結工程5として原料合金微粉を磁場中成形後、成形体を真空また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、例えば1000〜1150℃で5時間程度焼結すればよく、焼結後、急冷することが好ましい。焼結後、得られた焼結体に時効処理を施すことが好ましい。時効工程6は、得られる希土類焼結磁石の保磁力Hcjを制御する上で重要な工程であり、例えば不活性ガス雰囲気中あるいは真空中で時効処理を施す。時効処理としては、2段時効処理が好ましく、1段目の時効処理工程では、800℃前後の温度で1〜3時間保持する。次いで、室温〜200℃の範囲内にまで急冷する第1急冷工程を設ける。2段目の時効処理工程では、550℃前後の温度で1〜3時間保持する。次いで、室温まで急冷する第2急冷工程を設ける。600℃近傍の熱処理で保磁力Hcjが大きく増加するため、時効処理を一段で行う場合には、600℃近傍の時効処理を施すとよい。   Next, in the sintering process 5 and the aging process 6, sintering and an aging treatment are performed. That is, as the sintering step 5, after the raw material alloy fine powder is formed in a magnetic field, the compact is sintered in a vacuum or an inert gas atmosphere. The sintering temperature needs to be adjusted according to various conditions such as composition, pulverization method, difference in particle size and particle size distribution, etc. For example, sintering may be performed at 1000 to 1150 ° C. for about 5 hours, and rapid cooling after sintering. Is preferred. After sintering, the obtained sintered body is preferably subjected to aging treatment. The aging step 6 is an important step in controlling the coercive force Hcj of the obtained rare earth sintered magnet. For example, the aging step is performed in an inert gas atmosphere or in a vacuum. As the aging treatment, a two-stage aging treatment is preferable, and in the first aging treatment step, the temperature is maintained at a temperature of about 800 ° C. for 1 to 3 hours. Next, a first quenching step is provided for quenching to room temperature to 200 ° C. In the second stage aging treatment step, the temperature is maintained at about 550 ° C. for 1 to 3 hours. Next, a second quenching step for quenching to room temperature is provided. Since the coercive force Hcj is greatly increased by heat treatment at around 600 ° C., when aging treatment is performed in a single stage, it is preferable to perform aging treatment at around 600 ° C.

前記焼結工程5・時効工程6の後、加工工程7及び表面処理工程8を行う。加工工程7は、所望の形状に機械的に成形する工程である。表面処理工程8は、得られた希土類焼結磁石の酸化を抑えるために行う工程であり、例えばメッキ被膜や樹脂被膜を希土類焼結磁石の表面に形成する。   After the sintering step 5 and the aging step 6, a processing step 7 and a surface treatment step 8 are performed. The processing step 7 is a step of mechanically forming into a desired shape. The surface treatment step 8 is a step performed to suppress oxidation of the obtained rare earth sintered magnet. For example, a plating film or a resin film is formed on the surface of the rare earth sintered magnet.

以上の希土類焼結磁石の製造プロセスにおいて、本発明では、次のような製造装置、製造方法を用いて粗粉砕(水素吸蔵粉砕)を行い、永久磁石用合金粉末を得る。以下、本発明を適用した永久磁石用合金粉末の製造装置及び製造方法の実施形態について説明する。   In the manufacturing process of the rare earth sintered magnet described above, in the present invention, coarse pulverization (hydrogen storage pulverization) is performed using the following manufacturing apparatus and manufacturing method to obtain an alloy powder for permanent magnets. Embodiments of a manufacturing apparatus and a manufacturing method for permanent magnet alloy powder to which the present invention is applied will be described below.

本実施形態の永久磁石用合金粉末の製造装置は、図2に示すように、合金塊に水素を吸蔵させ破砕もしくは粉砕し合金粉末とする水素吸蔵部11と、水素吸蔵した合金粉末を加熱し脱水素する熱処理部12と、脱水素した合金粉末を除熱する冷却部13とを備えている。そして、これら水素吸蔵部11、熱処理部12、冷却部13は、同一の容器の中心円筒軸に沿って配置されている。   As shown in FIG. 2, the apparatus for producing a permanent magnet alloy powder according to the present embodiment heats the hydrogen occlusion unit 11 that occludes hydrogen into an alloy lump and crushes or grinds the alloy powder, and heats the hydrogen occluded alloy powder. A heat treatment part 12 for dehydrogenation and a cooling part 13 for removing heat from the dehydrogenated alloy powder are provided. And these hydrogen storage part 11, the heat processing part 12, and the cooling part 13 are arrange | positioned along the center cylindrical axis | shaft of the same container.

これら水素吸蔵部11、熱処理部12及び冷却部13を一体化した容器は、その中心軸が概ね水平となるように架台(図示は省略する。)上に支持されている。そして、中心軸を軸とする回転運動する構造となっている。また、容器を支持する架台には、水素吸蔵部11側をジャッキアップする機構が取り付けられている。これにより、各部間(水素吸蔵部11から熱処理部12、熱処理部12から冷却部13)における合金粉末の移動補助をすることができる。   The container in which the hydrogen storage unit 11, the heat treatment unit 12, and the cooling unit 13 are integrated is supported on a gantry (not shown) so that the central axis thereof is substantially horizontal. And it is the structure which carries out the rotational motion centering on a central axis. Moreover, the mechanism which jacks up the hydrogen storage part 11 side is attached to the mount frame which supports a container. Thereby, the movement assistance of the alloy powder in each part (the hydrogen storage part 11 to the heat processing part 12 and the heat processing part 12 to the cooling part 13) can be supported.

水素吸蔵部11、熱処理部12及び冷却部13を一体化した容器には、入口側にガス導入管14が接続され、水素導入管15及び不活性ガス導入機構となるAr導入管16が挿入されている。一方、出口側には、排気管17が接続されており、容器内の空気、水素ガス、不活性ガス(窒素ガス)等の排気を行うようにしてある。また、水素吸蔵部11、熱処理部12及び冷却部13を一体化した容器は、図3に示すように、モータ24及びチェーン25により正逆双方向に回転可能とされている。モータ24は、例えばインバータにより回転方向、回転数が制御される。   A gas introduction pipe 14 is connected to the inlet side of the container in which the hydrogen storage part 11, the heat treatment part 12, and the cooling part 13 are integrated, and a hydrogen introduction pipe 15 and an Ar introduction pipe 16 serving as an inert gas introduction mechanism are inserted. ing. On the other hand, an exhaust pipe 17 is connected to the outlet side to exhaust air, hydrogen gas, inert gas (nitrogen gas), etc. in the container. In addition, the container in which the hydrogen storage unit 11, the heat treatment unit 12, and the cooling unit 13 are integrated is rotatable in both forward and reverse directions by a motor 24 and a chain 25 as shown in FIG. The motor 24 has its rotation direction and rotation speed controlled by, for example, an inverter.

水素吸蔵部11は、合金塊に水素を吸蔵させる領域であり、その内周面に容器中心軸を軸とする溝状若しくはフィン状の螺旋部18が形成されている。したがって、回転方向により、螺旋部18の作用で合金塊を滞留させたり、払い出しすることが可能である。また、水素吸蔵部11には、水素吸蔵に伴う発熱を抑えることを目的に、上部に冷却水を散布するシャワー19が設けられていてもよい。   The hydrogen storage portion 11 is a region for storing hydrogen in the alloy lump, and a groove-shaped or fin-shaped spiral portion 18 having the container central axis as an axis is formed on the inner peripheral surface thereof. Therefore, the alloy lump can be retained or dispensed by the action of the spiral portion 18 depending on the rotation direction. In addition, the hydrogen storage unit 11 may be provided with a shower 19 for spraying cooling water on the top for the purpose of suppressing heat generation associated with hydrogen storage.

熱処理部12は、加熱により合金粉末の脱水素を行う領域であり、外側に電熱体21が複数配置されており、容器外側から合金粉末を加熱する構造となっている。本例では、電熱体21として、熱処理部12の両側面、並びに上面に加熱する手段としてパネル状の抵抗加熱ヒータが3組配置され、容器内が均一な温度になるように制御されている。   The heat treatment part 12 is a region where the alloy powder is dehydrogenated by heating, and a plurality of electric heaters 21 are arranged on the outside, and the alloy powder is heated from the outside of the container. In this example, three sets of panel-like resistance heaters are arranged as means for heating the both sides and the upper surface of the heat treatment section 12 as the electric heating element 21 and are controlled so that the inside of the container has a uniform temperature.

また、熱処理部12においては、容器内周面に容器の中心軸に向かい突出する複数の突出部20が形成されている。これら複数の突出部20は、任意の配置関係であってよく、例えば図4に示すように、それぞれが90度づつずらした関係にある4枚の突出部20を形成したり、図2のように中心軸方向に千鳥状に複数組配置しても良い。突出部20の形状も、棚状のもの等、合金粉末が撹拌されるような形状であれば任意形状でよい。   Moreover, in the heat processing part 12, the some protrusion part 20 which protrudes toward the center axis | shaft of a container is formed in the container internal peripheral surface. The plurality of protrusions 20 may be in any arrangement relationship. For example, as shown in FIG. 4, four protrusions 20 that are shifted by 90 degrees are formed as shown in FIG. A plurality of sets may be arranged in a zigzag pattern in the central axis direction. The shape of the protruding portion 20 may be any shape as long as the alloy powder is stirred, such as a shelf shape.

冷却部13は、脱水素後の合金粉末を冷却して払い出すための領域であり、先の水素吸蔵部11と同様、容器内周面に容器中心軸を軸とする溝状若しくはフィン状の螺旋部22が形成されている。ただし、この螺旋部22の螺旋の方向は、水素吸蔵部11の螺旋部18の螺旋の方向とは逆である。   The cooling unit 13 is a region for cooling and discharging the alloy powder after dehydrogenation, and, like the hydrogen storage unit 11 described above, a groove-like or fin-like shape with the vessel central axis as an axis on the vessel inner peripheral surface. A spiral portion 22 is formed. However, the spiral direction of the spiral portion 22 is opposite to the spiral direction of the spiral portion 18 of the hydrogen storage unit 11.

今回使用した容器の冷却部13には、図示していないが中心軸の円周上に配置した中心軸を公転する(自転はしない。)6本の小円筒が設置されており、熱処理部12から合金粉末が分割供給されるように溝状若しくはフィン状の螺旋部22が形成されている。各々の小円筒内に設けられた溝状若しくはフィン状の螺旋部22によって、合金粉末は撹拌移動しながら冷却される。さらに、各小円筒の外周には放熱フィンが複数設けられるとともに、この部分の冷却部13上に冷却水を散布するシャワー23が設置されている。   The container cooling unit 13 used this time is provided with six small cylinders that revolve (not rotate) the center axis arranged on the circumference of the center axis (not shown). A groove-shaped or fin-shaped spiral portion 22 is formed so that the alloy powder is supplied in a divided manner. The alloy powder is cooled while being stirred and moved by the groove-shaped or fin-shaped spiral portion 22 provided in each small cylinder. Furthermore, a plurality of heat radiating fins are provided on the outer periphery of each small cylinder, and a shower 23 for spraying cooling water is installed on the cooling portion 13 in this portion.

次に、上述の製造装置を用いた合金粉末の粗粉砕工程について説明する。図5に、図2に示す装置を用いた一連の工程を示す。   Next, the rough pulverization process of the alloy powder using the above manufacturing apparatus will be described. FIG. 5 shows a series of steps using the apparatus shown in FIG.

粗粉砕に際しては、先ず、合金塊を円筒形状のステンレス製容器である水素吸蔵部11に封入する(原料投入工程:ステップS1)。ここでは、重量百分率でNd31.5%、Dy1.5%、B1.1%、Al0.3%、残部Feなる組成を有する合金塊を粉砕し、約30mm角の合金塊を作製した。   In the coarse pulverization, first, the alloy lump is sealed in the hydrogen storage unit 11 which is a cylindrical stainless steel container (raw material charging step: step S1). Here, an alloy lump having a composition of Nd 31.5%, Dy 1.5%, B 1.1%, Al 0.3% and the balance Fe in weight percentage was pulverized to prepare an alloy lump of about 30 mm square.

原料投入後、ほぼ真空にまで排気(真空引き工程:ステップS2)した後、次いで、水素ガスを導入する(水素導入工程:ステップS3)。このとき、水素吸蔵部11内の圧力は、大気圧より若干高めに設定する。   After the raw materials are charged, after evacuating to a substantially vacuum (evacuation step: step S2), hydrogen gas is then introduced (hydrogen introduction step: step S3). At this time, the pressure in the hydrogen storage unit 11 is set slightly higher than the atmospheric pressure.

そして、この雰囲気を維持しながら容器の中心軸(円筒軸)を軸とする回転運動をさせ、合金塊に水素を吸蔵させながら破砕ないし粉砕を進める。水素吸蔵部11の内周面には、容器の中心軸を軸とする溝状若しくはフィン状の螺旋部18が形成されており、水素導入中は水素吸蔵部11に合金塊もしくは合金粉末を滞留(貯留)させるべく逆回転させる(ステップS4)。   Then, while maintaining this atmosphere, the container is rotated about the central axis (cylindrical axis) of the container, and crushing or pulverizing is performed while storing hydrogen in the alloy lump. A groove-shaped or fin-shaped spiral portion 18 with the central axis of the container as an axis is formed on the inner peripheral surface of the hydrogen storage portion 11, and an alloy lump or alloy powder stays in the hydrogen storage portion 11 during hydrogen introduction. Reverse rotation is performed to store (step S4).

なお、水素吸蔵工程における合金塊の保持温度は、0〜200℃とすることが好ましい。したがって、温度が上昇し過ぎた場合には、シャワー19から冷却水を散布する。また、水素吸蔵工程の処理時間は、特に限定されないが、通常、0.5〜5時間程度とすることが好ましい。   In addition, it is preferable that the retention temperature of the alloy lump in a hydrogen storage process shall be 0-200 degreeC. Therefore, when the temperature rises too much, cooling water is sprayed from the shower 19. Further, the treatment time of the hydrogen storage step is not particularly limited, but it is usually preferable to set it to about 0.5 to 5 hours.

その後、水素吸蔵部11を正回転させることにより、水素吸蔵部11中の合金粉末Mを溝状若しくはフィン状の螺旋部18の作用により熱処理部12へ移動させる(ステップS5)。このとき、容器を支持する架台を傾斜させる(熱処理部12側の容器を下降させる)ことにより、合金粉末Mの移動補助をすると良い。   Thereafter, by rotating the hydrogen storage unit 11 in the forward direction, the alloy powder M in the hydrogen storage unit 11 is moved to the heat treatment unit 12 by the action of the groove-shaped or fin-shaped spiral unit 18 (step S5). At this time, it is preferable to assist the movement of the alloy powder M by tilting the gantry supporting the container (lowering the container on the heat treatment unit 12 side).

水素吸蔵の後、熱処理部12では、容器内の水素ガスを排気するようにAr(この他の不活性ガスでもよい。)を導入しつつ(ステップS6)、熱処理部12内の合金粉末Mの温度が600℃程度になるようにヒータ21で加熱して、この温度を維持しながら合金粉末から水素ガスを放出させる(ステップS7)。   After the hydrogen occlusion, the heat treatment unit 12 introduces Ar (other inert gas may be used) so as to exhaust the hydrogen gas in the container (step S6), and the alloy powder M in the heat treatment unit 12 is heated. Heating is performed by the heater 21 so that the temperature is about 600 ° C., and hydrogen gas is released from the alloy powder while maintaining this temperature (step S7).

前記Arガスの導入は、不活性ガス供給機構であるAr導入管16により行い、熱処理部12内に大気圧以上の圧力でArガスを流す。供給するArガスを大気圧以上とすることで、熱処理部12内に周囲の空気が浸入することを防止することができる。また、Arガスを流し、冷却部を介して排気管17から順次排気することで、合金粉末から放出される水素も順次排出され、効率的な脱水素が可能となる。   The Ar gas is introduced by an Ar introduction pipe 16 which is an inert gas supply mechanism, and Ar gas is caused to flow into the heat treatment portion 12 at a pressure equal to or higher than atmospheric pressure. By setting the supplied Ar gas to atmospheric pressure or higher, ambient air can be prevented from entering the heat treatment section 12. In addition, by flowing Ar gas and exhausting sequentially from the exhaust pipe 17 through the cooling unit, hydrogen released from the alloy powder is also sequentially discharged, and efficient dehydrogenation is possible.

熱処理工程は、合金粉末Mから水素を放出させる工程であり、吸蔵した水素の50%〜90%程度を放出するような熱処理を行うことが好ましい。熱処理工程は、本実施形態のように、水素吸蔵工程に引き続いて連続的に行うことが好ましい。熱処理条件に特に制限はないが、合金粉末からの水素除去を効率的に行うためには、200〜800℃にて0.5〜5時間の熱処理を行うことが好ましい。   The heat treatment step is a step of releasing hydrogen from the alloy powder M, and it is preferable to perform a heat treatment that releases about 50% to 90% of the stored hydrogen. The heat treatment step is preferably performed continuously following the hydrogen storage step as in this embodiment. Although there is no restriction | limiting in particular in heat processing conditions, In order to perform the hydrogen removal from an alloy powder efficiently, it is preferable to perform the heat processing for 0.5 to 5 hours at 200-800 degreeC.

熱処理工程中は、水素吸蔵部11、熱処理部12及び冷却部13を一体化した容器を正回転させる。水素吸蔵部11の螺旋部18と冷却部13の螺旋部22の螺旋の方向が逆であるので、正回転させると、水素吸蔵部11の螺旋部18は、合金粉末を図2中左方向に移動させるように作用し、一方、冷却部13の螺旋部22は、合金粉末を図2中右方向に滞留させるように作用する。したがって、これらの作用によって、合金粉末は熱処理工程中は熱処理部12に滞留する。   During the heat treatment step, the container in which the hydrogen storage unit 11, the heat treatment unit 12, and the cooling unit 13 are integrated is rotated forward. Since the spiral direction of the spiral part 18 of the hydrogen storage part 11 and the spiral part 22 of the cooling part 13 are opposite, when the forward rotation is performed, the spiral part 18 of the hydrogen storage part 11 causes the alloy powder to move leftward in FIG. On the other hand, the spiral portion 22 of the cooling portion 13 acts to cause the alloy powder to stay in the right direction in FIG. Therefore, due to these actions, the alloy powder stays in the heat treatment section 12 during the heat treatment process.

ここで、本実施形態では、熱処理部12に棚板状の突出部20が形成されているので、粉砕が促進され、水素の放出が促進される。すなわち、熱処理部12に合金粉末が滞留している間、円筒形状の容器である熱処理部12は回転しており、熱処理部12内の合金粉末は複数の突出部20により破砕ないし粉砕させながら脱水素が行われる。このとき、残存する合金塊や崩落した合金粉末には突出部20により加速度が与えられるので、これらは熱処理部12内において頻繁に移動して相互に接触ないし衝突し、また熱処理部12の内壁とも接触ないし衝突する。その結果、熱処理部12内への合金粉末の投入量が多く、熱処理部12内における合金粉末の占める割合が高くても、合金粉末は均一に加熱される。このため、装置の大きさに対して処理能力を大幅に向上させることができる。また、熱処理部12においても合金粉末の破砕ないし粉砕はさらに進行し、合金塊をほぼ完全に粉末化することが可能である。その後、熱処理部12内の温度が100℃程度になるように冷却させる。このとき合金粉末Mは200℃程度まで冷却すればよい。   Here, in this embodiment, since the shelf-like protrusion 20 is formed in the heat treatment part 12, pulverization is promoted and hydrogen release is promoted. That is, while the alloy powder stays in the heat treatment section 12, the heat treatment section 12 that is a cylindrical container rotates, and the alloy powder in the heat treatment section 12 is dehydrated while being crushed or pulverized by the plurality of protrusions 20. Elementary is done. At this time, since the remaining alloy lump and the collapsed alloy powder are accelerated by the protrusions 20, they frequently move in the heat treatment part 12 and contact or collide with each other, and the inner wall of the heat treatment part 12 also Contact or collide. As a result, even if the amount of the alloy powder input into the heat treatment part 12 is large and the proportion of the alloy powder in the heat treatment part 12 is high, the alloy powder is heated uniformly. For this reason, the processing capability can be greatly improved with respect to the size of the apparatus. Further, in the heat treatment section 12, the pulverization or pulverization of the alloy powder further proceeds, and the alloy lump can be pulverized almost completely. Then, it cools so that the temperature in the heat processing part 12 may be set to about 100 degreeC. At this time, the alloy powder M may be cooled to about 200 ° C.

前記熱処理部12における熱処理後、最後に、水素吸蔵部11、熱処理部12及び冷却部13を一体化した容器を逆回転させ、脱水素を行った合金粉末を熱処理部12から冷却部13に移動させる(ステップS8)。冷却部13では、空冷、水冷、油冷、冷却ガスの何れか、もしくはこれらの組み合わせにより合金粉末を冷却して、次工程(微粉砕工程)へ移動させる(ステップS9)。合金粉末は、50℃以下まで冷却することにより安定化させることが好ましい。   After the heat treatment in the heat treatment part 12, finally, the container in which the hydrogen storage part 11, the heat treatment part 12 and the cooling part 13 are integrated is reversely rotated, and the dehydrogenated alloy powder is moved from the heat treatment part 12 to the cooling part 13. (Step S8). In the cooling unit 13, the alloy powder is cooled by any one of air cooling, water cooling, oil cooling, cooling gas, or a combination thereof, and moved to the next process (fine pulverization process) (step S9). The alloy powder is preferably stabilized by cooling to 50 ° C. or lower.

冷却部13には、溝状若しくはフィン状の螺旋部22を水素吸蔵部11とは逆方向に形成してある。したがって、逆回転させることにより、冷却部12中の溝状若しくはフィン状の螺旋部22により、合金粉末は冷却部13を通過し、温度を下げられた後、排気管17側の排出部から払い出される。このとき、容器を支持する架台を傾斜させる(排気管17側へ容器を下降させる)ことにより、合金粉末の移動補助をすると良い。   A groove-shaped or fin-shaped spiral portion 22 is formed in the cooling portion 13 in the opposite direction to the hydrogen storage portion 11. Therefore, by rotating in reverse, the alloy powder passes through the cooling unit 13 by the groove-shaped or fin-shaped spiral unit 22 in the cooling unit 12 and is discharged from the discharge unit on the exhaust pipe 17 side after the temperature is lowered. It is. At this time, it is preferable to assist movement of the alloy powder by inclining a gantry supporting the container (lowering the container to the exhaust pipe 17 side).

以上の装置及び方法においては、同一の容器で各工程を処理することができるため、高収率、短時間で効率が良く、且つ合金粉末の発火等も無く安全に微粉砕工程へ供給することができる。冷却工程後の合金は、例えば粒径1〜500μm程度の粒子から構成される粉末となる。   In the above apparatus and method, since each process can be processed in the same container, it can be efficiently supplied in a high yield, in a short time, and can be safely supplied to the pulverization process without ignition of the alloy powder. Can do. The alloy after the cooling step is, for example, a powder composed of particles having a particle size of about 1 to 500 μm.

以上、水素吸蔵による粗粉砕について説明したが、本発明がこの例に限られるものではなく、種々の変更が可能であることは言うまでもない。例えば、先の例では、水素吸蔵工程や熱処理工程において、回転運動を与えることで破砕や粉砕を促進するようにしているが、例えば各工程において、回転、揺動、振動の2種類以上を含む複合運動を運動付与手段によって与え、粉砕を促進するようにしてもよい。   The coarse pulverization by hydrogen storage has been described above, but the present invention is not limited to this example, and it goes without saying that various modifications are possible. For example, in the previous example, crushing and crushing are promoted by applying a rotational motion in the hydrogen storage process and the heat treatment process. For example, each process includes two or more types of rotation, oscillation, and vibration. Compound motion may be applied by the motion imparting means to promote crushing.

揺動や振動を運動付与手段によって与える場合、加速度の向きはいずれの方向であってもよく、例えば、鉛直方向の加速度を有する運動や水平方向の加速度を有する運動、あるいはこれらが複合された運動等のいずれであってもよい。超音波により振動させる場合には、ホーンを容器(水素吸蔵部11や熱処理部12)に密着させて振動を与えればよい。   When swinging or vibration is applied by the motion applying means, the direction of the acceleration may be any direction, for example, a motion having a vertical acceleration, a motion having a horizontal acceleration, or a motion in which these are combined. Any of these may be used. In the case of vibrating by ultrasonic waves, the horn may be brought into close contact with the container (hydrogen storage unit 11 or heat treatment unit 12) to apply vibration.

容器に与える運動が回転運動を含むとき、回転数は0.1〜10回転/分であることが好ましい。容器に与える運動が揺動運動や振動運動を含むとき、周期は0.05ミリ秒〜1分、振幅は10μm〜1mであることが好ましい。   When the motion applied to the container includes a rotational motion, the rotational speed is preferably 0.1 to 10 revolutions / minute. When the motion given to the container includes a rocking motion or a vibrating motion, the period is preferably 0.05 milliseconds to 1 minute, and the amplitude is preferably 10 μm to 1 m.

希土類焼結磁石の製造プロセスの一例を示すフロー図である。It is a flowchart which shows an example of the manufacturing process of a rare earth sintered magnet. 本発明を適用した永久磁石用合金粉末製造装置の一構成例を模式的に示す側面図である。It is a side view which shows typically one structural example of the alloy powder manufacturing apparatus for permanent magnets to which this invention is applied. 水素吸蔵部の内部構造を示す断面図である。It is sectional drawing which shows the internal structure of a hydrogen storage part. 熱処理部の内部構造を示す断面図である。It is sectional drawing which shows the internal structure of a heat processing part. 本発明装置及び方法による粗粉砕工程を工程順に示すフロー図である。It is a flowchart which shows the rough crushing process by this invention apparatus and method in process order.

符号の説明Explanation of symbols

11 水素吸蔵部、12 熱処理部、13 冷却部、15 水素導入管、16 Ar導入管、18 螺旋部、20 突出部、21 電熱体、22 螺旋部 DESCRIPTION OF SYMBOLS 11 Hydrogen storage part, 12 Heat processing part, 13 Cooling part, 15 Hydrogen introduction pipe, 16 Ar introduction pipe, 18 Spiral part, 20 Protrusion part, 21 Electric heating body, 22 Spiral part

この問題を解決し、合金塊の粉砕を容易に行なうために、従来、水素吸蔵粉砕が利用されている。水素吸蔵粉砕では、水素を吸蔵した合金にクラックが生じて自己崩壊的に粉末化が進行する。また、水素吸蔵は、合金の耐酸化性を向上する上でも有効である。しかしながら、静止した容器中において原料合金塊に水素を吸蔵させ、次いで熱処理を施した場合、表面付近は粉末化するものの、中心部付近まで粉末化することは難しい。このため塊状の合金が残ってしまうという不都合がある。 Conventionally, hydrogen occlusion pulverization has been used to solve this problem and to easily pulverize the alloy lump. In the hydrogen occlusion pulverization, a crack is generated in the alloy that occludes hydrogen, and powdering proceeds in a self-destructive manner. Hydrogen storage is also effective in improving the oxidation resistance of the alloy. However, when hydrogen is occluded in the raw material alloy lump in a stationary container and then subjected to heat treatment, the vicinity of the surface is pulverized, but it is difficult to pulverize to the vicinity of the center. For this reason, there is an inconvenience that a massive alloy remains.

上述の目的を達成するために、本発明の永久磁石用合金粉末の製造装置は、希土類元素、金属元素及びホウ素を含む原料合金塊に水素を吸蔵させ、これを粉砕して合金粉末とする永久磁石用合金粉末の製造装置であって、中心軸に沿って、水素吸蔵部と、水素吸蔵した合金粉末を加熱し脱水素する熱処理部と、冷却部とが順次配置されるとともに、これら各部が一体容器とされてなり、前記一体容器の入口側には、内部に不活性ガスを導入するための不活性ガス導入管及び水素ガスを導入するための水素ガス導入管が設けられ、出口側には、内部のガスを排気する排気管が設けられていることを特徴とする。 In order to achieve the above-described object, the permanent magnet alloy powder manufacturing apparatus of the present invention has a permanent alloy powder containing hydrogen stored in a raw material alloy lump containing a rare earth element, a metal element, and boron, and pulverized. An apparatus for producing magnet alloy powder for magnets , wherein a hydrogen storage part, a heat treatment part for heating and dehydrogenating the alloy powder stored with hydrogen, and a cooling part are sequentially arranged along the central axis. The integrated container is provided with an inert gas introduction pipe for introducing an inert gas therein and a hydrogen gas introduction pipe for introducing hydrogen gas inside the integral container. Is characterized in that an exhaust pipe for exhausting the internal gas is provided .

また、本発明の永久磁石用合金粉末の製造方法は、希土類元素、金属元素及びホウ素を含む原料合金塊に水素を吸蔵させ、これを粉砕して合金粉末とする永久磁石用合金粉末の製造方法において、水素吸蔵部において水素ガスを導入しながら原料合金塊に水素を吸蔵させた後、水素吸蔵部から熱処理部へと合金粉末を移動させ、熱処理部内に不活性ガスを導入するとともに排気しながら水素吸蔵した合金粉末を加熱して脱水素を行い、前記熱処理部で脱水素を行った合金粉末を冷却部で冷却することを特徴とする。 The method for producing an alloy powder for permanent magnets according to the present invention is a method for producing an alloy powder for permanent magnets in which hydrogen is occluded in a raw material alloy block containing rare earth elements, metal elements and boron, and pulverized into alloy powders. In the hydrogen storage portion, hydrogen gas is introduced into the raw material alloy lump while introducing hydrogen gas, and then the alloy powder is moved from the hydrogen storage portion to the heat treatment portion, and an inert gas is introduced into the heat treatment portion and exhausted. The hydrogen-absorbed alloy powder is heated for dehydrogenation, and the alloy powder dehydrogenated in the heat treatment part is cooled in a cooling part.

上述の目的を達成するために、本発明の永久磁石用合金粉末の製造装置は、希土類元素、金属元素及びホウ素を含む原料合金塊に水素を吸蔵させ、これを粉砕して合金粉末とする永久磁石用合金粉末の製造装置であって、中心軸に沿って、水素吸蔵部と、水素吸蔵した合金粉末を加熱し脱水素する熱処理部と、冷却部とが順次配置されるとともに、これら各部が回転運動する構造の一体容器とされてなり、前記一体容器の入口側には、内部に不活性ガスを導入するための不活性ガス導入管及び水素ガスを導入するための水素ガス導入管が設けられ、出口側には、内部のガスを排気する排気管が設けられていることを特徴とする。 In order to achieve the above-described object, the permanent magnet alloy powder manufacturing apparatus of the present invention has a permanent alloy powder containing hydrogen stored in a raw material alloy lump containing a rare earth element, a metal element, and boron, and pulverized. An apparatus for producing magnet alloy powder for magnets, wherein a hydrogen storage part, a heat treatment part for heating and dehydrogenating the alloy powder stored with hydrogen, and a cooling part are sequentially arranged along the central axis. The integrated container is structured to rotate , and an inert gas introduction pipe for introducing an inert gas and a hydrogen gas introduction pipe for introducing hydrogen gas are provided inside the integral container. An exhaust pipe for exhausting the internal gas is provided on the outlet side.

また、本発明の永久磁石用合金粉末の製造方法は、希土類元素、金属元素及びホウ素を含む原料合金塊に水素を吸蔵させ、これを粉砕して合金粉末とする永久磁石用合金粉末の製造方法において、中心軸に沿って、水素吸蔵部と、水素吸蔵した合金粉末を加熱し脱水素する熱処理部と、冷却部とが順次配置されるとともに、これら各部が回転運動する構造の一体容器を用い、前記一体容器の入口側に、内部に不活性ガスを導入するための不活性ガス導入管及び水素ガスを導入するための水素ガス導入管を設けるとともに、出口側に、内部のガスを排気する排気管を設け、前記水素ガス導入管より水素ガスを導入しながら水素吸蔵部において原料合金塊に水素を吸蔵させた後、水素吸蔵部から熱処理部へと合金粉末を移動させ、前記不活性ガス導入管から不活性ガスを導入するとともに前記排気管により排気しながら熱処理部内において水素吸蔵した合金粉末を加熱して脱水素を行い、前記熱処理部で脱水素を行った合金粉末を冷却部で冷却することを特徴とする。 The method for producing an alloy powder for permanent magnets according to the present invention is a method for producing an alloy powder for permanent magnets in which hydrogen is occluded in a raw material alloy block containing rare earth elements, metal elements and boron, and pulverized into alloy powders. In this example, a hydrogen storage part, a heat treatment part for heating and dehydrogenating the hydrogen-occluded alloy powder, and a cooling part are sequentially arranged along the central axis, and an integrated container having a structure in which these parts rotate. In addition, an inert gas introduction pipe for introducing an inert gas and a hydrogen gas introduction pipe for introducing hydrogen gas are provided on the inlet side of the integrated container, and the internal gas is exhausted on the outlet side. the exhaust pipe is provided, after the raw material alloy ingot in to occlude hydrogen in the hydrogen storage unit while introducing hydrogen gas from the hydrogen gas inlet pipe, move the alloy powder to a heat treatment unit from the hydrogen storage unit, the inert gas Perform hydrogen occluded alloy powder is heated to dehydrogenation in the thermal processing while exhausting by the exhaust pipe with an inert gas is introduced from the pipe, to cool the alloy powder subjected to dehydrogenation in the heat treatment unit in the cooling unit It is characterized by that.

Claims (12)

希土類元素、金属元素及びホウ素を含む原料合金塊に水素を吸蔵させ、これを粉砕して合金粉末とする永久磁石用合金粉末の製造装置であって、
水素吸蔵した合金粉末を加熱し脱水素する回転可能な熱処理部を備え、当該熱処理部は、処理時に内部に不活性ガスを導入するための不活性ガス供給機構を有することを特徴とする永久磁石用合金粉末の製造装置。
An apparatus for producing an alloy powder for permanent magnets that stores hydrogen in a raw material alloy lump containing a rare earth element, a metal element and boron, and pulverizes this into an alloy powder,
A permanent magnet comprising a rotatable heat treatment part for heating and dehydrogenating an alloy powder stored with hydrogen, the heat treatment part having an inert gas supply mechanism for introducing an inert gas into the interior during the treatment. Alloy powder manufacturing equipment.
前記不活性ガス供給機構により導入される不活性ガスは、Arガスであることを特徴とする請求項1記載の永久磁石用合金粉末の製造装置。   The apparatus for producing an alloy powder for a permanent magnet according to claim 1, wherein the inert gas introduced by the inert gas supply mechanism is Ar gas. 前記熱処理部は冷却部を介して排気管を有し、導入された不活性ガスが前記排気管から順次排気されることを特徴とする請求項1記載の永久磁石用合金粉末の製造装置。   The said heat processing part has an exhaust pipe through a cooling part, The introduced inert gas is exhausted sequentially from the said exhaust pipe, The manufacturing apparatus of the alloy powder for permanent magnets of Claim 1 characterized by the above-mentioned. 前記熱処理部は円筒形状を有し、その中心軸が傾斜可能に設置されていることを特徴とする請求項1記載の永久磁石用合金粉末の製造装置。   The said heat processing part has a cylindrical shape, The center axis | shaft is installed so that inclination is possible, The manufacturing apparatus of the alloy powder for permanent magnets of Claim 1 characterized by the above-mentioned. 前記熱処理部を加熱する手段を備えることを特徴とする請求項1記載の永久磁石用合金粉末の製造装置。   The apparatus for producing alloy powder for permanent magnets according to claim 1, further comprising means for heating the heat treatment section. 前記加熱する手段が抵抗加熱ヒータであり、熱処理部の周囲に配置されていることを特徴とする請求項5記載の永久磁石用合金粉末の製造装置。   6. The apparatus for producing a permanent magnet alloy powder according to claim 5, wherein the heating means is a resistance heater and is disposed around the heat treatment section. 前記熱処理部に揺動、振動から選択される少なくとも1種を与える運動付与手段が設けられていることを特徴とする請求項1記載の永久磁石用合金粉末の製造装置。   The apparatus for producing alloy powder for permanent magnets according to claim 1, wherein the heat treatment section is provided with a motion imparting means for imparting at least one selected from oscillation and vibration. 希土類元素、金属元素及びホウ素を含む原料合金塊に水素を吸蔵させ、これを粉砕して合金粉末とする永久磁石用合金粉末の製造方法において、
熱処理部を回転させるとともに、熱処理部内に不活性ガスを導入しながら水素吸蔵した合金粉末を加熱し脱水素することを特徴とする永久磁石用合金粉末の製造方法。
In the manufacturing method of alloy powder for permanent magnets, hydrogen is occluded in a raw material alloy lump containing rare earth elements, metal elements and boron, and pulverized into alloy powder.
A method for producing a permanent magnet alloy powder, comprising rotating a heat treatment section and heating and dehydrogenating an alloy powder occluded with hydrogen while introducing an inert gas into the heat treatment section.
導入される不活性ガスの圧力を、大気圧以上とすることを特徴とする請求項8記載の永久磁石用合金粉末の製造方法。   The method for producing a permanent magnet alloy powder according to claim 8, wherein the pressure of the inert gas introduced is set to atmospheric pressure or higher. 導入される不活性ガスを合金粉末から放出された水素ガスとともに排気することを特徴とする請求項8記載の永久磁石用合金粉末の製造方法。   9. The method for producing a permanent magnet alloy powder according to claim 8, wherein the introduced inert gas is exhausted together with the hydrogen gas released from the alloy powder. 前記熱処理部において、合金粉末の温度を200℃〜800℃に保持することを特徴とする請求項8記載の永久磁石用合金粉末の製造方法。   The method for producing a permanent magnet alloy powder according to claim 8, wherein the temperature of the alloy powder is maintained at 200 ° C. to 800 ° C. in the heat treatment section. 前記熱処理部に揺動、振動から選択される少なくとも1種を与えることを特徴とする請求項8記載の永久磁石用合金粉末の製造方法。   9. The method for producing a permanent magnet alloy powder according to claim 8, wherein at least one selected from oscillation and vibration is applied to the heat treatment section.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2955732A4 (en) * 2013-02-05 2016-01-13 Intermetallics Co Ltd Sintered magnet production method
CN108971499A (en) * 2018-09-19 2018-12-11 包头永真静平磁性材料科技有限公司 Hydrogen crushing furnace and its cooling means
WO2024150609A1 (en) * 2023-01-12 2024-07-18 Tdk株式会社 Kiln exhaust gas regeneration device and system, and kiln system

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2955732A4 (en) * 2013-02-05 2016-01-13 Intermetallics Co Ltd Sintered magnet production method
CN108971499A (en) * 2018-09-19 2018-12-11 包头永真静平磁性材料科技有限公司 Hydrogen crushing furnace and its cooling means
CN108971499B (en) * 2018-09-19 2021-10-22 包头永真静平磁性材料科技有限公司 Hydrogen crushing furnace and cooling method thereof
WO2024150609A1 (en) * 2023-01-12 2024-07-18 Tdk株式会社 Kiln exhaust gas regeneration device and system, and kiln system

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