JP4678003B2 - Magnet manufacturing method and molding apparatus for molding magnetic particles - Google Patents

Magnet manufacturing method and molding apparatus for molding magnetic particles Download PDF

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JP4678003B2
JP4678003B2 JP2007082722A JP2007082722A JP4678003B2 JP 4678003 B2 JP4678003 B2 JP 4678003B2 JP 2007082722 A JP2007082722 A JP 2007082722A JP 2007082722 A JP2007082722 A JP 2007082722A JP 4678003 B2 JP4678003 B2 JP 4678003B2
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陽一 國吉
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Description

本発明は、磁石の製造方法及び磁性粒子を成型するための成型装置に関する。   The present invention relates to a magnet manufacturing method and a molding apparatus for molding magnetic particles.

従来、磁性粉末を焼結して得られる焼結磁石の製造方法としては、磁石の原料となる磁性粉末を油等の溶媒と混合して得られたスラリーを金型内で圧縮成型した後、焼結するという湿式成型のプロセスを経る方法が知られている（特許文献１）。
特開平９−２８９１２７号公報 Conventionally, as a method for producing a sintered magnet obtained by sintering magnetic powder, a slurry obtained by mixing magnetic powder as a raw material of a magnet with a solvent such as oil is compression-molded in a mold, A method that undergoes a wet molding process of sintering is known (Patent Document 1).
JP-A-9-289127

しかし、上記特許文献１のように、スラリーを金型内で圧縮成型すると、脱気しながら溶媒の濾過を行うので、得られた成型体が金型の内壁に密着する。このため、成型体を金型、特に下パンチの成型面（パンチ面）から離型させ難いという問題があった。この問題のために、成型体を金型から離型させた際の成型体が破損する頻度が高く、歩留まり低下や生産効率低下の一因となっていた。   However, as in Patent Document 1, when the slurry is compression-molded in the mold, the solvent is filtered while degassing, so that the obtained molded body is in close contact with the inner wall of the mold. For this reason, there is a problem that it is difficult to release the molded body from the mold, particularly the molding surface (punch surface) of the lower punch. Because of this problem, the molded body is frequently broken when the molded body is released from the mold, which is a cause of a decrease in yield and production efficiency.

そこで、本発明は、湿式成型による磁石の製造において、圧縮成型後の成型体の離型性を向上させることを目的とする。   Then, this invention aims at improving the mold release property of the molded object after compression molding in manufacture of the magnet by wet molding.

一つの側面において、本発明は磁石の製造方法に関する。本発明に係る磁石の製造方法は、磁性粒子と溶媒とを含むスラリーを型に充填する工程と、粗面化領域を含む面を有するパンチにより該粗面化領域を含む面でスラリーを型の内部で加圧しながら溶媒を排出することによってスラリーを圧縮成型して、磁性粒子の成型体を形成する工程と、前記成型体を焼成して磁石を形成する工程と、を備える。   In one aspect, the present invention relates to a method for manufacturing a magnet. The magnet manufacturing method according to the present invention comprises a step of filling a mold with a slurry containing magnetic particles and a solvent, and a mold having a slurry on the surface including the roughened region by a punch having a surface including the roughened region. The method includes compression forming the slurry by discharging the solvent while pressurizing inside to form a molded body of magnetic particles, and firing the molded body to form a magnet.

なお、上記本発明において、「粗面化」とは、ブラスト処理などを行うことによって中心線平均粗さＲａが０．０２μｍ以上となるように表面が加工されていることを意味する。   In the present invention, “roughening” means that the surface is processed so that the centerline average roughness Ra is 0.02 μm or more by performing blasting or the like.

上記本発明においては、パンチの粗面化領域がスラリーに接触するようにパンチを型に押し込んでスラリーを圧縮する。よって、成型体は、パンチの粗面化領域を含む面と密着した状態で形成される。粗面化領域を含む面と成型体との密着性は、従来のような平坦面と成型体との密着性よりも低くなり、そのために圧縮成型後の成型体の離型性が従来に比べて向上する。   In the present invention, the slurry is compressed by pushing the punch into the mold so that the roughened region of the punch is in contact with the slurry. Thus, the molded body is formed in close contact with the surface including the roughened region of the punch. The adhesiveness between the surface including the roughened area and the molded body is lower than the adhesiveness between the flat surface and the molded body as in the past, so that the mold releasability after compression molding is lower than the conventional one. Improve.

上記粗面化領域の中心線平均粗さＲａは０．１１〜２．３２μｍである。 The center line average roughness Ra of the roughened region is 0.11 to 2.32 μm.

粗面化領域のＲａを上記範囲内とすることによって、成型体の離型性を更に向上させることができる。粗面化領域のＲａが小さいと、成型体の離型性向上の効果が小さくなる傾向がある。一方、粗面化領域のＲａが大きいと、粗面化領域の窪みに成型体の一部が入り込み、成型体の離型性向上効果が小さくなる傾向がある。   By making Ra of the roughened region within the above range, the mold release property of the molded body can be further improved. When Ra of the roughened region is small, the effect of improving the mold release property of the molded body tends to be small. On the other hand, when the Ra of the roughened region is large, a part of the molded body enters the depression of the roughened region, and the effect of improving the releasability of the molded body tends to be reduced.

上記記粗面化領域の十点平均粗さＲｚは２．４２〜２２．３μｍである。 The ten-point average roughness Rz of the roughened region is 2.42 to 22.3 μm.

粗面化領域のＲｚを上記範囲内とすることによって、成型体の離型性を更に向上させることができる。粗面化領域のＲｚが小さいと、成型体の離型性向上の効果が小さくなる傾向がある。一方、粗面化領域のＲｚが大きいと、粗面化領域の窪みに成型体の一部が入り込み、成型体の離型性向上の効果が小さくなる傾向がある。また、粗面化領域のＲｚが大き過ぎると、粗面化領域の突出部が成型体に食い込み、成型時に成型体にクラックが発生したり、粗面化領域の突出部が成型体に食い込んでアンカーとして作用し、成型体の離型性向上効果が小さくなったりする傾向がある。さらに、粗面化領域のＲｚが大きくなると、粗面化領域と接する成型体表面の表面粗さが大きくなり、これから得られる磁石の表面粗さも大きくなる。磁石の表面粗さが大きいと、磁石表面を研削、研磨等により整形加工して平坦化するために除去される部分の磁石の量が大きくなる。すなわち、用いた原料に対する製品の材料歩留が低下する。特に希土類磁石のような比較的高価な材料を用いる場合、製品の材料歩留を少しでも高めることが強く求められる。   By making Rz of the roughened region within the above range, it is possible to further improve the releasability of the molded body. When Rz in the roughened region is small, the effect of improving the mold release property of the molded body tends to be small. On the other hand, if the Rz of the roughened region is large, a part of the molded body enters the recess of the roughened region, and the effect of improving the mold release property of the molded body tends to be small. Also, if the Rz of the roughened region is too large, the protruding portion of the roughened region bites into the molded body, cracks occur in the molded body during molding, or the protruding portion of the roughened region bites into the molded body. It acts as an anchor, and there is a tendency that the effect of improving the releasability of the molded body is reduced. Furthermore, when Rz of the roughened region increases, the surface roughness of the molded body surface in contact with the roughened region increases, and the surface roughness of the magnet obtained therefrom also increases. If the surface roughness of the magnet is large, the amount of the magnet removed in order to flatten the surface of the magnet by shaping, polishing, etc., becomes large. That is, the material yield of the product with respect to the used raw material falls. In particular, when a relatively expensive material such as a rare earth magnet is used, it is strongly required to increase the material yield of the product as much as possible.

圧縮成型の際、溶媒の含有量が成型体全体に対して４．２〜１４．９質量％となるまでスラリーから溶媒を除去する。 During compression molding, you remove the solvent from the slurry to the content of the solvent is 4.2 to 14.9% by weight, based on the total molded body.

成型体全体に対する溶媒の含有量を上記範囲内とすることによって、成型体の強度が向上するとともに、成型体の密度バラツキが生じにくくなり焼結時の変形を防止できる。更に、磁性特性が特に優れた磁石を形成することができる。   By setting the content of the solvent with respect to the entire molded body within the above range, the strength of the molded body is improved and the density variation of the molded body is less likely to occur and deformation during sintering can be prevented. Furthermore, a magnet having particularly excellent magnetic properties can be formed.

上記磁性粒子の平均粒径は２〜７μｍである。 The average particle size of the magnetic particles Ru 2~7μm der.

磁性粒子の平均粒径が上記範囲内であるとき、成型体の離型性向上の効果がより一層顕著に奏される。   When the average particle diameter of the magnetic particles is within the above range, the effect of improving the releasability of the molded body is more remarkably exhibited.

別の側面において、本発明は磁性粒子を成型するための成型装置に関する。本発明に係る成型装置は、パンチと型とを有し当該パンチを当該型に押し込むことにより圧縮成型する圧縮成型部と、当該圧縮成型部に磁場を印加する磁場発生部とを備え、パンチが、粗面化領域を含む面を有し、当該粗面化領域を含む面が圧縮成型の際に当該型の内部側に向けられる面であり、型において当該型の内部から外部へ導通する排液路が形成されており、粗面化領域の中心線平均粗さＲａが０．１１〜２．３２μｍであり、粗面化領域の十点平均粗さＲｚが２．４２〜２２．３μｍである。 In another aspect, the present invention relates to a molding apparatus for molding magnetic particles. A molding apparatus according to the present invention includes a compression molding unit that includes a punch and a mold and compresses and molds the punch into the mold, and a magnetic field generation unit that applies a magnetic field to the compression molding unit. The surface including the roughened region, and the surface including the roughened region is a surface directed to the inside of the mold during compression molding, and is a drain that conducts from the inside of the mold to the outside in the mold. A liquid channel is formed, the center line average roughness Ra of the roughened region is 0.11 to 2.32 μm, and the ten-point average roughness Rz of the roughened region is 2.42 to 22.3. μm.

上記本発明に係る成型装置は、上述の本発明に係る製造方法において成型体を得るために好適に用いることができる。本発明に係る成型装置を用いることにより、湿式成型による磁石の製造において、圧縮成型後の成型体の離型性を向上させることが可能である。   The molding apparatus according to the present invention can be suitably used for obtaining a molded body in the manufacturing method according to the present invention described above. By using the molding apparatus according to the present invention, it is possible to improve the releasability of the molded body after compression molding in the production of a magnet by wet molding.

本発明に係る磁石の製造方法および成型装置によれば、湿式成型による磁石の製造において、圧縮成型後の成型体の離型性を向上させることが可能である。その結果、圧縮成型後に成型体を型及びパンチから離型させる際の成型体の破損の頻度が低下する。これにより歩留まりが向上すると共に、破損した成型体を型から除去するために製造ラインを停止させる頻度が低下して生産効率の向上が図られる。   According to the magnet manufacturing method and the molding apparatus according to the present invention, it is possible to improve the releasability of a molded body after compression molding in manufacturing a magnet by wet molding. As a result, the frequency of breakage of the molded body when the molded body is released from the mold and punch after compression molding is reduced. This improves the yield and reduces the frequency of stopping the production line in order to remove the damaged molded body from the mold, thereby improving the production efficiency.

以下、図面を適宜参照しながら、本発明の好適な一実施形態である、湿式成型による希土類磁石の製造方法ついて詳細に説明する。ただし、本発明は以下の実施形態に限定されるものではない。   Hereinafter, a method for producing a rare earth magnet by wet molding, which is a preferred embodiment of the present invention, will be described in detail with reference to the drawings as appropriate. However, the present invention is not limited to the following embodiments.

本実施形態に係る製造方法は、磁性粒子と溶媒とを含むスラリーを準備する工程と、型の内部に充填されたスラリーを、パンチを型に押し込むことにより溶媒を除去しながら圧縮成型して、磁性粒子の成型体を形成する工程と、成型体に残存した溶媒を除去する工程と、成型体を焼成して磁石を形成する工程とを備える。   In the manufacturing method according to the present embodiment, a step of preparing a slurry containing magnetic particles and a solvent, and a slurry filled in the mold are compression-molded while removing the solvent by pushing the punch into the mold, The method includes a step of forming a molded body of magnetic particles, a step of removing a solvent remaining in the molded body, and a step of firing the molded body to form a magnet.

スラリーに用いる磁性粒子は、例えば、所望の組成を有する希土類磁石が得られるような合金を粉砕する方法により得られる。合金は、例えば、希土類磁石の組成に対応する元素を含む金属や化合物等を、真空又はアルゴン等の不活性ガス雰囲気下で溶解した後、これを用いて鋳造法やストリップキャスト法等の合金製造プロセスを行うことによって作製する。   The magnetic particles used in the slurry can be obtained, for example, by a method of pulverizing an alloy that can obtain a rare earth magnet having a desired composition. For example, an alloy is produced by melting a metal or a compound containing an element corresponding to the composition of the rare earth magnet in an inert gas atmosphere such as vacuum or argon, and then using this to produce an alloy such as a casting method or a strip casting method. Produced by performing the process.

希土類磁石の種類は特に限定されないが、例えば、希土類元素として主にＮｄやＳｍを含むものが挙げられる。希土類元素と、希土類元素以外の遷移元素とを組み合わせた組成を有するものが好適である。具体的には、希土類元素（「Ｒ」で表す）として、Ｎｄ、Ｐｒ及びＤｙのうちの少なくとも１種を含み、Ｂを必須元素として１〜１２原子％含み、且つ残部がＦｅであるＲ−Ｆｅ−Ｂ系磁石が例示される。このような希土類磁石は、必要に応じて、Ｃｏ、Ｎｉ、Ｍｎ、Ａｌ、Ｎｂ、Ｚｒ、Ｔｉ、Ｗ、Ｍｏ、Ｖ、Ｇａ、Ｚｎ及びＳｉ等の元素を更に含有してもよい。Ｒ−Ｆｅ−Ｂ系磁石以外の希土類磁石としては、Ｒ−Ｃｏ系磁石（ＲはＳｍ等）が例示される。   The type of rare earth magnet is not particularly limited, and examples thereof include those containing mainly Nd and Sm as rare earth elements. Those having a composition in which a rare earth element and a transition element other than the rare earth element are combined are suitable. Specifically, as a rare earth element (represented by “R”), R—containing at least one of Nd, Pr, and Dy, 1 to 12 atomic% of B as an essential element, and the balance being Fe An Fe-B magnet is exemplified. Such a rare earth magnet may further contain elements such as Co, Ni, Mn, Al, Nb, Zr, Ti, W, Mo, V, Ga, Zn, and Si, if necessary. Examples of rare earth magnets other than R-Fe-B magnets include R-Co magnets (R is Sm or the like).

合金を粗粉砕して、数百μｍ程度の粒径を有する磁性粗粉を形成し、更に磁性粗粉を微粉砕して、磁性粒子を形成する。   The alloy is coarsely pulverized to form a magnetic coarse powder having a particle size of about several hundred μm, and the magnetic coarse powder is further finely pulverized to form magnetic particles.

希土類磁石を用いる場合、微粉砕後に得られる磁性粒子の平均粒径は２〜７μｍである。磁性粒子の平均粒径を上記範囲内とすることによって、成型体の離型性向上効果が特に顕著に得られる傾向がある。 When using a rare earth magnet, an average particle diameter of the magnetic particles obtained after milling is Ru 2~7μm der. By making the average particle diameter of the magnetic particles within the above range, the effect of improving the releasability of the molded body tends to be obtained particularly remarkably.

合金を粗粉砕する方法としては、例えば、ジョークラッシャー、ブラウンミル、スタンプミル等の粗粉砕機を用いる方法、または、合金に水素を吸蔵させた後、異なる相間の水素吸蔵量の相違に基づく自己崩壊的な粉砕を生じさせる方法（水素吸蔵粉砕法）が挙げられる。磁性粗粉を微粉砕する方法としては、例えば、磁性粗粉を、粉砕時間等の条件を適宜調整しながら、ジェットミル、ボールミル、振動ミル、湿式アトライター等の微粉砕機を用いて粉砕する方法が挙げられる。   As a method of coarsely pulverizing an alloy, for example, a method using a coarse pulverizer such as a jaw crusher, a brown mill, a stamp mill, or the like, or self-based on the difference in hydrogen storage amount between different phases after hydrogen is occluded in the alloy. Examples thereof include a method (hydrogen storage pulverization method) that causes disintegrative pulverization. As a method for finely pulverizing the magnetic coarse powder, for example, the magnetic coarse powder is pulverized using a fine pulverizer such as a jet mill, a ball mill, a vibration mill, or a wet attritor while appropriately adjusting the conditions such as the pulverization time. A method is mentioned.

スラリーは、磁性粒子と溶媒とを混合した混合物を混練し、必要により更に分散処理を施して調製される。混錬は、例えば、加圧ニーダ、オープンニーダ、２軸押出機、プラネタリーミキサー等の方法によって行うことができる。溶媒としては、磁石の湿式成型に常用される溶媒であれば特に限定されず、例えば、鉱物油、合成油、植物油等の油や、アセトン、アルコールといった有機溶媒が挙げられる。スラリー中での磁性粒子の分散性を良好に保つ観点からは、溶媒としては油を用いることが好ましく、鉱物油を用いることがより好ましい。また、実質的に有機溶媒を含まない油を用いることが更に好ましい。   The slurry is prepared by kneading a mixture in which magnetic particles and a solvent are mixed, and further performing a dispersion treatment if necessary. The kneading can be performed by a method such as a pressure kneader, an open kneader, a twin screw extruder, or a planetary mixer. The solvent is not particularly limited as long as it is a solvent commonly used in magnet wet molding, and examples thereof include oils such as mineral oil, synthetic oil and vegetable oil, and organic solvents such as acetone and alcohol. From the viewpoint of maintaining good dispersibility of the magnetic particles in the slurry, oil is preferably used as the solvent, and mineral oil is more preferably used. Further, it is more preferable to use an oil substantially free of an organic solvent.

磁性粒子と溶媒との混合においては、溶媒以外に、所望の特性が得られる他の添加剤を更に加えることもできる。添加剤としては、例えば、磁性粒子の分散を促進することができる分散剤が挙げられる。   In the mixing of the magnetic particles and the solvent, in addition to the solvent, other additives capable of obtaining desired characteristics can be further added. Examples of the additive include a dispersant that can promote dispersion of magnetic particles.

スラリーの分散処理は、ボールミル、超音波拡散、ホモジナイザー、アルティマイザー等を用いることによって行うことができる。   The slurry can be dispersed by using a ball mill, ultrasonic diffusion, homogenizer, optimizer, or the like.

図１〜６は、スラリーを圧縮成型する工程の一実施形態を示す模式図である。本実施形態では、図１に示す成型装置を用いて、上述のようにして得られたスラリーを圧縮成型し、磁性粒子の成型体を形成する。   FIGS. 1-6 is a schematic diagram which shows one Embodiment of the process of compressing and molding a slurry. In this embodiment, using the molding apparatus shown in FIG. 1, the slurry obtained as described above is compression molded to form a molded body of magnetic particles.

図１に示す成型装置２は、主として、圧縮成型部４と、磁場発生部６とから構成される。圧縮成型部４は、主として、下パンチ８と、筒状の臼１４及びこれの一端面に対して固定可能な上型１２を有する型１０とから構成される。型１０の内部には、臼１４と上型１２に囲まれた室１６が形成されている。室１６は成型体の形状に対応した形状を有する。上型１２においては、型１０の内部（室１６）から外部へ導通する排液路１８が形成されている。下パンチ８は臼１４に嵌まる形状を有しており、臼１４内を上下自在に摺動させることができる。また、上型１２も臼１４に対して離接自在に上下移動させることができる。   A molding apparatus 2 shown in FIG. 1 mainly includes a compression molding unit 4 and a magnetic field generation unit 6. The compression molding part 4 is mainly composed of a lower punch 8, a mold 10 having a cylindrical mortar 14 and an upper mold 12 that can be fixed to one end face of the cylindrical mortar 14. A chamber 16 surrounded by a mortar 14 and an upper mold 12 is formed inside the mold 10. The chamber 16 has a shape corresponding to the shape of the molded body. In the upper mold 12, a drainage path 18 is formed which conducts from the inside (chamber 16) of the mold 10 to the outside. The lower punch 8 has a shape that fits into the mortar 14 and can be slid freely in the mortar 14. Further, the upper die 12 can also be moved up and down so as to be detachable from the die 14.

磁場発生部６は臼１４の周囲に配置され、圧縮成型部４に磁場を印加することができる。磁場発生部６としては、磁性粒子の成型において、必要とされる磁場の強度等に応じて適宜磁界を発生するものである。   The magnetic field generation unit 6 is disposed around the mortar 14 and can apply a magnetic field to the compression molding unit 4. The magnetic field generator 6 generates a magnetic field as appropriate according to the strength of the required magnetic field in the formation of magnetic particles.

下パンチ８は、粗面化領域を含む面（以下「パンチ面」という）８ａを有する。圧縮成型の際、下パンチ８は、パンチ面８ａを型１０の内部側に向けた向きで型１０の内部（室１６）に押し込まれる。粗面化領域は、パンチ面８ａの全体に形成されていてもよく、パンチ面８ａの一部に形成されていてもよい。成型体の離型性向上の観点から、パンチ面８ａ全体の面積のうち、５０％以上が粗面化領域であることが好ましい。   The lower punch 8 has a surface (hereinafter referred to as “punch surface”) 8 a including a roughened region. During compression molding, the lower punch 8 is pushed into the interior of the mold 10 (chamber 16) with the punch surface 8a facing toward the interior of the mold 10. The roughened region may be formed on the entire punch surface 8a or may be formed on a part of the punch surface 8a. From the viewpoint of improving the releasability of the molded body, it is preferable that 50% or more of the entire area of the punch surface 8a is a roughened region.

粗面化領域は、非周期的な凹凸形状を有していることが好ましい。これにより、成型体をパンチ面８ａから引き剥がす際の離型性が、引き剥がす力を加える方向に依存することなく高められるため、引き剥がしに伴う成型体破損の頻度が特に小さくなる。パンチ面８ａにおける粗面化領域は、中心線平均粗さＲａが、０．１１〜２．３２μｍ、より好ましくは０．１１〜１．３μｍとなるように粗面化されている。 The roughened region preferably has an aperiodic uneven shape. Thereby, the releasability when the molded body is peeled off from the punch surface 8a is enhanced without depending on the direction in which the peeling force is applied, and therefore the frequency of the molded body breakage accompanying the peeling is particularly reduced. Roughened region in the punch surface 8a has a center line average roughness Ra, from 0.11 to 2.32 [mu] m, and more preferably is roughened to a 0.11 ~1.3μm.

また、パンチ面８ａにおける粗面化領域は、十点平均粗さＲｚが、２．４２〜２２．３μｍとなるように粗面化されている。 Further, the roughened region on the punch surface 8a is roughened so that the ten-point average roughness Rz is 2.42 to 22.3 μm.

粗面化領域を粗面化する方法としては、特に限定されないが、好適な方法として研磨材（メディア）を圧縮ガスにより吹き付けるブラスト処理、または、ダイヤモンドやセラミックなどの研磨材を固着した電着砥石、レジンボンド砥石等を用いた研磨処理によれば、非周期的な凹凸形状が均一に分布した粗面化領域が形成される。   A method for roughening the roughened region is not particularly limited, but a suitable method is a blasting process in which an abrasive (media) is sprayed with a compressed gas, or an electrodeposition grindstone to which an abrasive such as diamond or ceramic is fixed. According to the polishing process using a resin bond grindstone or the like, a roughened region in which non-periodic uneven shapes are uniformly distributed is formed.

図２、３はスラリーを型の内部に充填する工程を示す。まず、図２に示すように、上型１２を、臼１４の上方に移動させると共に、搬送装置２２によって、スラリー充填装置２４を臼１４の上方へ移動、配置させる。次いで、図３に示すように、スラリー充填装置２４から上述のスラリー２６を下パンチ８と臼１４とで囲まれた空間（室１６）へ所定量供給し、室１６にスラリー２６を充填する。   2 and 3 show the process of filling the slurry into the mold. First, as shown in FIG. 2, the upper mold 12 is moved above the die 14, and the slurry filling device 24 is moved and arranged above the die 14 by the conveying device 22. Next, as shown in FIG. 3, a predetermined amount of the slurry 26 is supplied from the slurry filling device 24 to a space (chamber 16) surrounded by the lower punch 8 and the die 14, and the chamber 26 is filled with the slurry 26.

スラリー充填装置２４を臼１４の上方から移動させた後、図４に示すように、上型１２を下降させて臼１４の上部に固定する。これにより型１０の内部にスラリー２６が充填された状態となる。続いて磁場発生部６によって、圧縮成型部４の内部に位置するスラリー２６に磁場Ｍを印加する。その結果、スラリー２６に含まれる磁性粒子が磁場配向する。磁場Ｍの方向は、後述する圧縮成型時の加圧方向に対して垂直であり、これにより優れた磁気特性を有する磁石が得られる。また、磁場Ｍの強度は、特に限定されないが、通常１０〜２０ｋＯｅ（約７９０〜約１５８０ｋＡ／ｍ）程度である。   After the slurry filling device 24 is moved from above the die 14, the upper mold 12 is lowered and fixed to the upper portion of the die 14 as shown in FIG. 4. As a result, the slurry 26 is filled in the mold 10. Subsequently, the magnetic field generator 6 applies a magnetic field M to the slurry 26 located inside the compression molding unit 4. As a result, the magnetic particles contained in the slurry 26 are magnetically oriented. The direction of the magnetic field M is perpendicular to the pressurizing direction at the time of compression molding, which will be described later, whereby a magnet having excellent magnetic properties can be obtained. The strength of the magnetic field M is not particularly limited, but is usually about 10 to 20 kOe (about 790 to about 1580 kA / m).

スラリー２６に磁場Ｍを印加した状態で、図５に示すように、粗面化領域を含むパンチ面８ａをスラリー２６に接触させながら下パンチ８を上型１２に向かって移動させる。このように、臼１４の内部に押し込まれた下パンチ８によって、スラリー２６を圧縮成型する。圧縮成型の結果、スラリー２６から排液路１８を通して溶媒が除去されると共に、スラリー２６の全体が圧縮され、所定の配向度を有する磁性粒子の成型体が形成される。   With the magnetic field M applied to the slurry 26, the lower punch 8 is moved toward the upper mold 12 while the punch surface 8 a including the roughened region is in contact with the slurry 26 as shown in FIG. 5. Thus, the slurry 26 is compression-molded by the lower punch 8 pushed into the die 14. As a result of the compression molding, the solvent is removed from the slurry 26 through the drainage channel 18 and the entire slurry 26 is compressed to form a molded body of magnetic particles having a predetermined degree of orientation.

圧縮成型後、図６に示すように、上型１２を臼１４から上方へ向かって移動させ、下パンチ８を臼１４の上部に更に移動させることによって、得られた成型体２８は下パンチ８のパンチ面８ａに密着した状態で臼１４の外部へ取り出される。成型体２８は図示しない成型体移送装置によってパンチ面８ａから引き剥がされて次の工程に供される。パンチ面８ａが粗面化領域を有していることにより、成型体２８のパンチ面８ａからの離型性が良好であり、剥離の際に破損した成型体２８の一部がパンチ面８ａ側に密着したまま残ってしまうといったトラブルが発生する頻度は十分に低い。   After compression molding, as shown in FIG. 6, the upper die 12 is moved upward from the die 14, and the lower punch 8 is further moved to the upper portion of the die 14. The die 14 is taken out of the die 14 in close contact with the punch surface 8a. The molded body 28 is peeled off from the punch surface 8a by a molded body transfer device (not shown) and used for the next step. Since the punch surface 8a has a roughened region, the mold 28 has good releasability from the punch surface 8a, and a part of the molded body 28 that is damaged at the time of peeling is part of the punch surface 8a. The frequency of occurrence of troubles such as remaining in close contact with is sufficiently low.

成型体２８の形状は、特に限定されず、柱状、平板状、瓦状、リング状等、所望とする希土類磁石の形状に応じて変更することができる。   The shape of the molded body 28 is not particularly limited, and can be changed according to the desired shape of the rare earth magnet, such as a columnar shape, a flat plate shape, a tile shape, or a ring shape.

圧縮成型においてスラリー２６（成型体２８）に加わる圧力は、特に限定されないが、通常、約２９．４〜約２９４ＭＰａ程度である。また、圧縮成型の所要時間は、数秒〜数十秒とすることが好ましい。このような条件下で圧縮成型を行うことにより、良好な磁気特性を有する希土類磁石が得られる。   The pressure applied to the slurry 26 (molded body 28) in compression molding is not particularly limited, but is usually about 29.4 to about 294 MPa. The time required for compression molding is preferably several seconds to several tens of seconds. By performing compression molding under such conditions, a rare earth magnet having good magnetic properties can be obtained.

圧縮成型では、溶媒の含有量が、得られる成型体２８全体に対して４．２〜１４．９質量％となるまで、スラリー２６から溶媒を除去する。成型体２８全体に対する溶媒の含有量を上記範囲内とすることによって、成型体２８の強度が向上し、また、成型体の密度バラツキが生じにくくなり焼結時の変形を防止できる。更に、成型体２８に含まれる磁性粒子の磁場配向性も向上する。その結果、良好な機械強度を有するとともに、高い残留磁束密度Ｂｒを有する磁石を形成することができる。 In compression molding, the content of the solvent is, until 4.2 to 14.9% by weight, based on the total molded body 28 obtained, remove the solvent from the slurry 26. By setting the content of the solvent with respect to the entire molded body 28 within the above range, the strength of the molded body 28 is improved, and the density variation of the molded body is less likely to occur and deformation during sintering can be prevented. Furthermore, the magnetic field orientation of the magnetic particles contained in the molded body 28 is also improved. As a result, a magnet having a good mechanical strength and a high residual magnetic flux density Br can be formed.

圧縮成型時にスラリー２６から除去された溶媒は、排液路１８を通って、型１０の内部から外部へ排出される。また、型１０の内部（室１６）から外部へ磁性粒子が流出することを防止するために、上型の内面１２ａに布製、紙製等のフィルターを配置するか、或いは、上型の一部（内面１２ａ）の材質を多孔質とすることが好ましい。   The solvent removed from the slurry 26 at the time of compression molding is discharged from the inside of the mold 10 to the outside through the drainage path 18. Further, in order to prevent the magnetic particles from flowing out from the inside (chamber 16) of the mold 10 to the outside, a filter made of cloth, paper or the like is disposed on the inner surface 12a of the upper mold, or a part of the upper mold The material of the (inner surface 12a) is preferably porous.

得られた成型体２８に対し、例えば真空加熱を行うことにより、成型体２８に残存した溶媒や添加剤が除去される（脱バインダー処理）。なお、脱バインダー処理では、通常は成型体２８の焼結は進行しないが、焼結が部分的に進行してもよい。   The obtained molded body 28 is subjected to, for example, vacuum heating to remove the solvent and additives remaining in the molded body 28 (debinding process). In the debinding process, usually, the sintering of the molded body 28 does not proceed, but the sintering may partially proceed.

脱バインダー処理後の成型体２８を焼成して、焼結体である希土類磁石を得る。焼成は、例えば、真空中又は不活性ガスの雰囲気下、成型体２８を、１０００〜１２００℃で、１〜１０時間加熱した後、急冷することによって行うことができる。   The molded body 28 after the binder removal treatment is fired to obtain a rare earth magnet that is a sintered body. Firing can be performed, for example, by heating the molded body 28 at 1000 to 1200 ° C. for 1 to 10 hours in a vacuum or in an inert gas atmosphere and then rapidly cooling it.

得られた焼結体は、好ましくは、その磁気特性を向上させるために焼成時よりも低い温度で加熱する時効処理が施される。時効処理は、例えば、７００〜９００℃で１〜３時間、更に５００〜７００℃で１〜３時間加熱する２段階加熱や、６００℃付近で１〜３時間加熱する１段階加熱によって行う。   The obtained sintered body is preferably subjected to an aging treatment in which it is heated at a temperature lower than that at the time of firing in order to improve its magnetic properties. The aging treatment is performed, for example, by two-step heating at 700 to 900 ° C. for 1 to 3 hours, further heating at 500 to 700 ° C. for 1 to 3 hours, or one-step heating at about 600 ° C. for 1 to 3 hours.

時効処理後の焼結体（希土類磁石）は、通常、表面（下パンチ８との接触面等）を平滑化する処理が施される。また、焼結体を所望のサイズに切断してもよい、得られた希土類磁石の表面に防錆するための保護層を更に形成させてもよい。   The sintered body (rare earth magnet) after the aging treatment is usually subjected to a treatment for smoothing the surface (the contact surface with the lower punch 8, etc.). In addition, the sintered body may be cut into a desired size, and a protective layer for rust prevention may be further formed on the surface of the obtained rare earth magnet.

以上、本発明に係る磁石の製造方法の好適な実施形態として、希土類磁石の製造方法について説明したが、本発明は必ずしも上述した実施形態に限定されるものではない。   As mentioned above, although the manufacturing method of the rare earth magnet was demonstrated as suitable embodiment of the manufacturing method of the magnet which concerns on this invention, this invention is not necessarily limited to embodiment mentioned above.

例えば、磁性粒子としてフェライト磁石等を用いてもよい。この場合も上述の実施形態と同様に、成型体２８の離型性が向上する。具体的なフェライト磁石としては、特に限定されないが、ＳｒＯ・６Ｆｅ2Ｏ3（Ｍ型フェライト）、ＳｒＯ・２（ＦｅＯ）・ｎ（Ｆｅ2Ｏ3）（Ｗ型フェライト）等が例示される。なお、磁性粒子がフェライト磁石である場合、得られる磁性粒子の平均粒径が０．６〜２μｍとなるように、微粉砕処理を行うことが好ましい。磁性粒子の平均粒径を上記範囲内とすることによって、成型体の離型性が、更に向上する。 For example, a ferrite magnet or the like may be used as the magnetic particles. In this case as well, the releasability of the molded body 28 is improved as in the above embodiment. Specific ferrite magnets, but are not limited to, SrO · 6Fe 2 O 3 ( M -type ferrite), SrO · 2 (FeO) · n (Fe 2 O 3) (W -type ferrite), and the like. In addition, when a magnetic particle is a ferrite magnet, it is preferable to pulverize so that the average particle diameter of the magnetic particle obtained may be 0.6-2 micrometers. By setting the average particle size of the magnetic particles within the above range, the releasability of the molded body is further improved.

以下、本発明を実施例により更に詳細に説明する。ただし、本発明はこれらの実施例に限定されるものではない。   Hereinafter, the present invention will be described in more detail with reference to examples. However, the present invention is not limited to these examples.

希土類磁石の作製
（試料１）
Ｎｄ：３０質量％，Ｄｙ：１．８質量％，Ａｌ：０．２質量％，Ｃｏ：０．５質量％，Ｆｅ：６７．５質量％からなるインゴットを粗粉砕した後、ジェットミルを用いて窒素雰囲気下で微粉砕し、平均粒径Ｄが４μｍである磁性粒子を得た。得られた磁性粒子を、分散剤、及び、溶媒として分留点が２００〜２５０℃である合成油と混合し、得られた混合物を、磁性粒子濃度９１％でプラネタリーディスパー（浅田鐵工製）を用いて混練し、スラリーを作製した。この際、混練時間は６０分とした。混練後、合成油を加えて更に希釈し、スラリーの最終的な磁性粒子濃度を７０質量％に調整した。 Production of rare earth magnet (sample 1)
An ingot composed of Nd: 30% by mass, Dy: 1.8% by mass, Al: 0.2% by mass, Co: 0.5% by mass, Fe: 67.5% by mass was roughly pulverized, and then a jet mill was used. And finely pulverized in a nitrogen atmosphere to obtain magnetic particles having an average particle diameter D of 4 μm. The obtained magnetic particles were mixed with a dispersant and a synthetic oil having a fractional distillation point of 200 to 250 ° C. as a solvent, and the resulting mixture was mixed with planetary disperse (manufactured by Asada Seiko Co., Ltd.) with a magnetic particle concentration of 91% ) To prepare a slurry. At this time, the kneading time was 60 minutes. After kneading, synthetic oil was added to further dilute, and the final magnetic particle concentration of the slurry was adjusted to 70% by mass.

得られたスラリーを、図１〜６に示す成型装置２を用いて圧縮成型し、成型体を形成した。下パンチ８として、中心線平均粗さＲａが０．５８μｍ、十点平均粗さＲｚが７．０５μｍとなるようにサンドブラストによってパンチ面８ａ全体が粗面化されたものを用いた。また、圧縮成型直後（脱バインダー前）の成型体に含まれる溶媒の含有量ａが、成型体全体に対して７質量％となるまで、スラリーから溶媒を除去した。圧縮成型の際、スラリー（成型体）に１５ｋＯｅ（約１１８５ｋＡ／ｍ）の配向磁場を印加した。圧縮成型中に型１０の内部から流出した溶媒が排液路１８を通じて型１０の外部に良好に排出されるように、上型１２の内面１２ａに予め濾紙を設置した。   The obtained slurry was compression molded using a molding apparatus 2 shown in FIGS. 1 to 6 to form a molded body. As the lower punch 8, the entire punch surface 8 a was roughened by sandblasting so that the center line average roughness Ra was 0.58 μm and the ten-point average roughness Rz was 7.05 μm. Moreover, the solvent was removed from the slurry until the content a of the solvent contained in the molded body immediately after compression molding (before debinding) was 7% by mass with respect to the entire molded body. During compression molding, an orientation magnetic field of 15 kOe (about 1185 kA / m) was applied to the slurry (molded body). A filter paper was previously installed on the inner surface 12a of the upper mold 12 so that the solvent that flowed out from the inside of the mold 10 during the compression molding was well discharged to the outside of the mold 10 through the drainage path 18.

得られた成型体を真空中で１５０℃に加熱して、成型体に含まれる溶媒を除去した。次に、成型体を、真空中で１１００℃、５時間で焼成した。得られた焼結体に対して、５００℃、１時間で時効処理を施した。このようにして、試料１の希土類磁石を得た。上述の方法で試料１の希土類磁石を１００個作製した。   The obtained molded body was heated to 150 ° C. in a vacuum to remove the solvent contained in the molded body. Next, the molded body was fired in vacuum at 1100 ° C. for 5 hours. The obtained sintered body was subjected to an aging treatment at 500 ° C. for 1 hour. Thus, a rare earth magnet of Sample 1 was obtained. 100 rare earth magnets of Sample 1 were produced by the method described above.

（試料２〜３９）
粗面化領域の中心線平均粗さＲａおよび十点平均粗さＲｚ、成型体に含まれる溶媒の含有量ａ、成型体の形成に用いた磁性粒子の粒径Ｄを、それぞれ表１に示す値としたこと以外は、試料１と同様の方法で試料２〜３９の希土類磁石をそれぞれ１００個作製した。なお、試料２、８、１５、２２、２９では、下パンチ８としてパンチ面８ａが粗面化されていないものを用いた。粗面化されていないパンチ面の中心線平均粗さＲａは０．０１μｍであり、十点平均粗さＲｚは０．５４μｍであった。 (Samples 2 to 39)
Table 1 shows the centerline average roughness Ra and ten-point average roughness Rz of the roughened region, the content a of the solvent contained in the molded body, and the particle diameter D of the magnetic particles used for forming the molded body. Except for the values, 100 rare earth magnets of Samples 2 to 39 were produced in the same manner as Sample 1, respectively. In Samples 2, 8, 15, 22, and 29, the lower punch 8 having a roughened punch surface 8a was used. The center line average roughness Ra of the punch surface not roughened was 0.01 μm, and the ten-point average roughness Rz was 0.54 μm.

Figure 0004678003
Figure 0004678003

離型不良率の測定
試料１〜３９それぞれの作製過程において、成型体を成型装置２の下パンチ８（パンチ面８ａ）から剥離する際に、成型体の一部が剥がれてパンチ面８ａに付着したもの、成型体が割れたもの、成型体の一部が欠けたもの、および、焼成後に焼結体で割れ、欠けが検出されたものの数（以下、離型不良品数）を計量した。試料１〜３９それぞれについて、全試料数１００個に対する離型不良品数の割合（離型不良率、単位％）を求めた。結果を表１に示す。なお、表１において、離型不良率が１００％の試料は、×と判定した。また、離型不良率が１００％未満の試料は、△と判定した。また、離型不良率が１％以下の試料は、○と判定した。離型不良率が０％の試料は、◎と判定した。離型不良率は小さいほど好ましい。 In the production process of each of the measurement samples 1 to 39 of the mold release failure rate, when the molded body is peeled from the lower punch 8 (punch surface 8a) of the molding apparatus 2, a part of the molded body is peeled off and adheres to the punch surface 8a. The number of the molded body, the molded body cracked, the part of the molded body chipped, and the one that was cracked and chipped in the sintered body after firing (hereinafter referred to as the number of defective mold release) were measured. For each of Samples 1 to 39, the ratio of the number of defective mold releases to the total number of samples 100 (release defective ratio, unit%) was determined. The results are shown in Table 1. In Table 1, a sample having a mold release failure rate of 100% was determined as x. A sample having a defective mold release rate of less than 100% was determined to be Δ. A sample having a release defect rate of 1% or less was judged as ◯. Samples with a mold release failure rate of 0% were judged as ◎. The smaller the release defect rate, the better.

表１に示されるように、試料１〜７を比較すると、パンチ面８ａが粗面化されている成型装置２を用いてプレス成型した試料１，３〜７は、パンチ面８ａが粗面化されていない成型装置を用いて圧縮成型した試料２に比べて、離型不良率が小さいことが確認された。   As shown in Table 1, when samples 1 to 7 are compared, samples 1 and 3 to 7 which are press-molded using the molding apparatus 2 having a roughened punch surface 8a have a roughened punch surface 8a. It was confirmed that the mold release failure rate was smaller than that of Sample 2 that was compression molded using a molding apparatus that was not used.

パンチ面８ａのＲａが０．１１〜２．３２μｍである試料１、４〜６は、試料３、７に比べて、離型不良率が更に小さいことが確認された。Ｒａが０．１１〜１．２１μｍである試料１、４、５は、試料６に比べて、離型不良率が更に小さいことが確認された。   It was confirmed that Samples 1 and 4 to 6 in which Ra of the punch surface 8a was 0.11 to 2.32 μm had a smaller release defect rate than Samples 3 and 7. It was confirmed that Samples 1, 4, and 5 having Ra of 0.11 to 1.21 μm had a smaller release defect rate than Sample 6.

また、Ｒｚが２．４２〜２２．３μｍである試料１、４〜６は、試料３、７に比べて、離型不良率が更に小さいことが確認された。また、Ｒｚが２．４２〜７．０５μｍである試料１、４、５は、試料６に比べて、離型不良率が更に小さいことが確認された。   In addition, it was confirmed that Samples 1 and 4 to 6 having Rz of 2.42 to 22.3 μm had a smaller release defect rate than Samples 3 and 7. In addition, it was confirmed that Samples 1, 4, and 5 having Rz of 2.42 to 7.05 μm had a smaller release defect rate than Sample 6.

試料８〜１４の比較、試料１５〜２１の比較、試料２２〜２８の比較、試料２９〜３５の比較においても、試料１〜７を比較した場合と同様の結果が確認された。   In the comparison of samples 8 to 14, the comparison of samples 15 to 21, the comparison of samples 22 to 28, and the comparison of samples 29 to 35, the same results as in the case of comparing samples 1 to 7 were confirmed.

図１は、成型装置の一実施形態を示す概略図である。FIG. 1 is a schematic view showing an embodiment of a molding apparatus. 図２は、磁性粒子の成型体を形成する工程の一部を示す概略図である。FIG. 2 is a schematic view showing a part of a process of forming a molded body of magnetic particles. 図３は、磁性粒子の成型体を形成する工程の一部を示す概略図である。FIG. 3 is a schematic view showing a part of a process of forming a molded body of magnetic particles. 図４は、磁性粒子の成型体を形成する工程の一部を示す概略図である。FIG. 4 is a schematic view showing a part of a process of forming a molded body of magnetic particles. 図５は、磁性粒子の成型体を形成する工程の一部を示す概略図である。FIG. 5 is a schematic view showing a part of a process of forming a molded body of magnetic particles. 図６は、磁性粒子の成型体を形成する工程の一部を示す概略図である。FIG. 6 is a schematic view showing a part of a process of forming a molded body of magnetic particles.

符号の説明Explanation of symbols

２…磁性粒子の成型装置、４…圧縮成型部、６…磁場発生部、８…下パンチ、８ａ…パンチ面、１０…型、１２…上型、１４…臼、１８…排液路、２６…スラリー、２８…成型体。   DESCRIPTION OF SYMBOLS 2 ... Magnetic particle shaping | molding apparatus, 4 ... Compression molding part, 6 ... Magnetic field generation | occurrence | production part, 8 ... Lower punch, 8a ... Punch surface, 10 ... Type | mold, 12 ... Upper type | mold, 14 ... Dice, 18 ... Drainage path, 26 ... Slurry, 28 ... Molded product.

Claims (2)

磁性粒子と溶媒とを含むスラリーを型に充填する工程と、
粗面化領域を含む面を有するパンチにより該粗面化領域を含む面で前記スラリーを前記型の内部で加圧しながら前記溶媒を排出することによって前記スラリーを圧縮成型して、前記磁性粒子の成型体を形成する工程と、
前記成型体を焼成して磁石を形成する工程と、を備え、
前記粗面化領域の中心線平均粗さＲａが０．１１〜２．３２μｍであり、
前記粗面化領域の十点平均粗さＲｚが２．４２〜２２．３μｍであり、
前記磁性粒子の平均粒径が２〜７μｍであり、
前記溶媒の含有量が前記成型体全体に対して４．２〜１４．９質量％となるまで前記スラリーから前記溶媒を除去する、
磁石の製造方法。 Filling a mold with a slurry containing magnetic particles and a solvent;
The slurry is compression-molded by discharging the solvent while pressurizing the slurry inside the mold on the surface including the roughened region by a punch having a surface including the roughened region, and Forming a molded body; and
And firing the molded body to form a magnet.
The center line average roughness Ra of the roughened region is 0.11 to 2.32 μm,
Wherein Ri ten-point average roughness Rz of the roughened area is from 2.42 to 22.3 [mu] m der,
The magnetic particles have an average particle size of 2 to 7 μm,
Removing the solvent from the slurry until the content of the solvent is 4.2 to 14.9% by mass relative to the entire molded body;
Magnet manufacturing method. パンチと型とを有し当該パンチを当該型に押し込むことにより圧縮成型する圧縮成型部と、
前記圧縮成型部に磁場を印加する磁場発生部と、を備え、
前記パンチが、粗面化領域を含む面を有し、当該粗面化領域を含む面が圧縮成型の際に当該型の内部側に向けられる面であり、
前記型において当該型の内部から外部へ導通する排液路が形成されており、
前記粗面化領域の中心線平均粗さＲａが０．１１〜２．３２μｍであり、
前記粗面化領域の十点平均粗さＲｚが２．４２〜２２．３μｍである、
磁性粒子を成型するための成型装置。 A compression molding part that has a punch and a mold and compresses and molds the punch into the mold;
A magnetic field generation unit that applies a magnetic field to the compression molding unit,
The punch has a surface including a roughened region, and the surface including the roughened region is a surface directed toward the inner side of the mold during compression molding,
In the mold, a drainage path is formed that conducts from the inside of the mold to the outside,
The center line average roughness Ra of the roughened region is 0.11 to 2.32 μm,
Ten-point average roughness Rz of the roughened region is 2.42 to 22.3 μm.
Molding device for molding magnetic particles.
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