JP4412376B2 - Salt-water resistant magnet alloy powder, and resin composition for bond magnet, bond magnet or compacted magnet obtained by using the same - Google Patents
Salt-water resistant magnet alloy powder, and resin composition for bond magnet, bond magnet or compacted magnet obtained by using the same Download PDFInfo
- Publication number
- JP4412376B2 JP4412376B2 JP2007254363A JP2007254363A JP4412376B2 JP 4412376 B2 JP4412376 B2 JP 4412376B2 JP 2007254363 A JP2007254363 A JP 2007254363A JP 2007254363 A JP2007254363 A JP 2007254363A JP 4412376 B2 JP4412376 B2 JP 4412376B2
- Authority
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- Japan
- Prior art keywords
- alloy powder
- magnet
- salt
- metal
- phosphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 229910045601 alloy Inorganic materials 0.000 title claims description 98
- 239000000956 alloy Substances 0.000 title claims description 98
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- 239000011342 resin composition Substances 0.000 title claims description 10
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 48
- 229910001463 metal phosphate Inorganic materials 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 43
- 150000003839 salts Chemical class 0.000 claims description 42
- 239000011248 coating agent Substances 0.000 claims description 36
- 238000000576 coating method Methods 0.000 claims description 36
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- 229910052761 rare earth metal Inorganic materials 0.000 claims description 28
- 239000002131 composite material Substances 0.000 claims description 26
- 229910052751 metal Inorganic materials 0.000 claims description 26
- 239000002184 metal Substances 0.000 claims description 26
- 229910052742 iron Inorganic materials 0.000 claims description 25
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- 239000003960 organic solvent Substances 0.000 claims description 21
- 229910019142 PO4 Inorganic materials 0.000 claims description 19
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- 239000002245 particle Substances 0.000 claims description 16
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- 239000002904 solvent Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
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- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
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- 239000011737 fluorine Substances 0.000 description 3
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- 238000004519 manufacturing process Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
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- SPDJAIKMJHJYAV-UHFFFAOYSA-H trizinc;diphosphate;tetrahydrate Chemical compound O.O.O.O.[Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SPDJAIKMJHJYAV-UHFFFAOYSA-H 0.000 description 3
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- 229910021380 Manganese Chloride Inorganic materials 0.000 description 2
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- Powder Metallurgy (AREA)
- Chemical Treatment Of Metals (AREA)
- Hard Magnetic Materials (AREA)
Description
本発明は、耐塩水性磁石合金粉、及びそれを用いて得られるボンド磁石用樹脂組成物、ボンド磁石又は圧密磁石に関し、さらに詳しくは、塩水に触れる環境下でも錆が発生しない耐塩水性磁石合金粉、及びそれを用いて得られるボンド磁石用樹脂組成物、ボンド磁石又は圧密磁石に関するものである。 TECHNICAL FIELD The present invention relates to a salt water resistant magnet alloy powder, and a resin composition for a bond magnet, a bond magnet or a compacted magnet obtained by using the same, and more specifically, a salt water resistant magnet alloy powder that does not generate rust even in an environment where it is exposed to salt water. , And a bonded magnet resin composition, a bonded magnet, or a compacted magnet obtained using the same.
近年、フェライト磁石、アルニコ磁石、希土類磁石などが、一般家電製品、通信・音響機器、医療機器、一般産業機器をはじめとする種々の製品にモーターやセンサーなどとして組込まれ、使用されている。これら磁石は、主に焼結法で製造されるが、脆く、薄肉化しにくいため複雑形状への成形は困難であり、また焼結時に15〜20%も収縮するため寸法精度を高められず、研磨等の後加工が必要で、用途面で大きな制約を受けている。 In recent years, ferrite magnets, alnico magnets, rare earth magnets, and the like have been incorporated and used as motors and sensors in various products including general household electrical appliances, communication / acoustic equipment, medical equipment, and general industrial equipment. Although these magnets are mainly manufactured by a sintering method, they are fragile and difficult to be thinned, so it is difficult to mold them into complex shapes. Also, since they shrink by 15 to 20% during sintering, the dimensional accuracy cannot be increased. Post-processing such as polishing is necessary, and there are significant restrictions in terms of application.
これに対し、ボンド磁石(樹脂結合型磁石)は、ポリアミド樹脂、ポリフェニレンサルファイド樹脂などの熱可塑性樹脂、あるいは、エポキシ樹脂、ビス・マレイミドトリアジン樹脂、不飽和ポリエステル樹脂、ビニルエステル樹脂などの熱硬化性樹脂をバインダーとし、これに磁石合金粉を充填して容易に製造できるため、新しい用途開拓が繰り広げられている。 In contrast, bonded magnets (resin-bonded magnets) are thermosetting such as polyamide resins, thermoplastic resins such as polyphenylene sulfide resins, or epoxy resins, bis-maleimide triazine resins, unsaturated polyester resins, and vinyl ester resins. New applications are being developed because it can be easily manufactured by using resin as a binder and filling it with magnet alloy powder.
希土類元素を含む鉄系の磁石合金粉を、樹脂バインダーと混練してボンド磁石を製造する場合、磁石合金粉を数μm程度に粉砕する必要がある。粉砕は不活性ガスまたは有機溶媒中で行うが、粉砕後の磁石合金粉は極めて活性であり、大気に触れると急激に酸化が進み磁気特性を劣化させるので、微粉砕後に、僅かな酸素を不活性雰囲気に導入して徐酸化する方法が採られている。 When a bonded magnet is manufactured by kneading iron-based magnet alloy powder containing a rare earth element with a resin binder, the magnet alloy powder needs to be pulverized to about several μm. Grinding is carried out in an inert gas or an organic solvent, but the magnet alloy powder after grinding is extremely active, and when exposed to the atmosphere, oxidation rapidly proceeds and deteriorates the magnetic properties. A method of introducing into an active atmosphere and gradual oxidation is employed.
こうしたボンド磁石の中でも、特に、希土類元素を含む鉄系磁石合金粉を用いたボンド磁石は、塩水中で錆が発生しやすいため、例えば、成形体表面に熱硬化性樹脂等のコーティング膜を形成することで発錆を抑制したり、また、特開2000−208321号公報に開示されているように、成形体表面にリン酸塩含有塗料による被覆処理を施すことで発錆を抑制している。しかし、上記方法で作製された磁石合金粉でも塩水中のような腐食性の厳しい環境下では、錆の抑制に対して十分に満足できるものではなかった。 Among these bonded magnets, in particular, bonded magnets using iron-based magnet alloy powders containing rare earth elements are prone to rust in salt water. For example, a coating film such as a thermosetting resin is formed on the surface of the molded body. In order to suppress rusting, and as disclosed in JP-A-2000-208321, rusting is suppressed by applying a coating treatment with a phosphate-containing coating to the surface of the molded body. . However, even the magnetic alloy powder produced by the above method is not sufficiently satisfactory for the suppression of rust in a corrosive environment such as salt water.
従来、磁石合金粉を被膜処理する場合、粉砕溶媒中にリン酸を添加し、希土類や鉄のリン酸塩を合金粉表面に生成させる方法が検討されている。しかし、この方法で作製した磁石合金粉は、高温高湿度の環境下では磁気特性の低下が非常に少ないものの、これを用いて作製したボンド磁石を塩水中に24時間浸漬すると、赤錆の発生を多少は低減できるが完全になくすことはできなかった。 Conventionally, in the case of coating a magnetic alloy powder, a method has been studied in which phosphoric acid is added to a grinding solvent to generate a rare earth or iron phosphate on the surface of the alloy powder. However, although the magnetic alloy powder produced by this method has very little deterioration in magnetic properties in a high temperature and high humidity environment, when a bonded magnet produced using this is immersed in salt water for 24 hours, red rust is generated. Although it could be reduced somewhat, it could not be completely eliminated.
近年、家電機器用モーター、自動車用センサーやモーターにおいて、海外で部品を組み立てるため船などによる輸送が必要となり、その使用環境、輸送環境がさらに厳しくなり、また機器を小型化するため、上記課題とともに磁気特性にも優れたものが要求されている。 In recent years, motors for home appliances, sensors and motors for automobiles have to be transported by ship in order to assemble parts overseas, and their use environment and transport environment have become more severe, and the size of the equipment has been reduced. What has excellent magnetic properties is also required.
前記のような希土類元素を含む鉄系磁石合金粉から得られるボンド磁石の磁気特性は、これら用途に使用するには不十分であり、希土類元素を含む鉄系磁石合金粉の耐塩水性を早期に改善し、ボンド磁石の磁気特性を向上させることが強く望まれていた。 The magnetic properties of the bond magnet obtained from the iron-based magnet alloy powder containing the rare earth element as described above are insufficient for use in these applications, and the salt water resistance of the iron-based magnet alloy powder containing the rare earth element is accelerated. There has been a strong desire to improve and improve the magnetic properties of bonded magnets.
また、ボンド磁石よりもエネルギー積を高めるためには、磁石体の見かけ密度を、その磁石合金粉の真密度に近づけることが必要である。先に述べた焼結法がその解決方法として一般的な製造方法となるが、その他にも熱間圧縮成形法で圧密化する方法もある。たとえば、液体急冷法で製造されたネオジム−鉄−ほう素系磁石合金粉をホットプレスすることによって、最大エネルギー積が112kJ/m3程度の等方性圧密磁石が製造されている。 Further, in order to increase the energy product as compared with the bonded magnet, it is necessary to bring the apparent density of the magnet body closer to the true density of the magnet alloy powder. The sintering method described above is a general manufacturing method as a solution to this problem, but there is also a method of compacting by a hot compression molding method. For example, an isotropic compacted magnet having a maximum energy product of about 112 kJ / m 3 is manufactured by hot pressing neodymium-iron-boron magnet alloy powder manufactured by a liquid quenching method.
また、サマリウム−鉄−窒素系磁石合金粉では、およそ600℃以上に加熱するとサマリウム−鉄−窒素系化合物が分解するため、「粉体および粉末冶金」47号(2000)第801頁に示された等方性熱間圧縮成形法(HIP)、特開平6−077027号公報に開示された衝撃圧縮法、特開2000−294415号公報に開示された通電粉末圧延法が検討されている。 In addition, samarium-iron-nitrogen-based magnet alloy powder decomposes the samarium-iron-nitrogen-based compound when heated to about 600 ° C. or higher, and therefore is shown in “Powder and Powder Metallurgy” 47 (2000), page 801. The isotropic hot compression molding method (HIP), the impact compression method disclosed in Japanese Patent Application Laid-Open No. 6-077027, and the electric powder rolling method disclosed in Japanese Patent Application Laid-Open No. 2000-294415 have been studied.
これらの圧密磁石においても、磁気特性に優れた磁石は得られるものの、その使用環境、輸送環境などの過酷化は、ボンド磁石の場合と同様であり、耐塩水性を改善する必要があった。また、従来の磁石合金粉を用いて圧密磁石を製造する場合には、サマリウム−鉄−窒素系化合物の分解、脱窒素あるいは磁石合金粉粒子同士の金属結合による粒子間磁気的相互作用が強まるためか、圧密磁石の保磁力が低く実用材としてはまだ不十分である。
本発明の目的は、前述した従来技術の問題点に鑑み、塩水に触れる環境下で錆が発生しない耐塩水性磁石合金粉、及びそれを用いて得られるボンド磁石用樹脂組成物、ボンド磁石又は圧密磁石を提供することにある。 The object of the present invention is to solve the above-mentioned problems of the prior art, and is a salt-water resistant magnetic alloy powder that does not generate rust in an environment where it is exposed to salt water, and a resin composition for a bonded magnet, a bonded magnet, or a consolidated compact obtained using the same. It is to provide a magnet.
本発明者らは、上記課題を解決するために鋭意研究を重ねた結果、希土類元素を含む鉄系の磁石合金粉に、鉄と希土類元素の金属リン酸塩、及びアルミニウム、亜鉛、マンガン、銅又はカルシウムから選ばれた1種以上の金属リン酸塩の2種類が複合化した金属リン酸塩被膜を形成すると、該被膜が塩水を遮断し、磁石合金粉の発錆を抑制する耐塩水性に優れた磁石合金粉が得られることを見出し、本発明を完成するに至った。 As a result of intensive studies to solve the above-mentioned problems, the present inventors have found that iron-based magnet alloy powders containing rare earth elements, metal phosphates of iron and rare earth elements, and aluminum, zinc, manganese, copper Alternatively, when forming a metal phosphate coating in which two or more of one or more metal phosphates selected from calcium are combined, the coating blocks salt water and is resistant to salt water to suppress rusting of magnet alloy powder. The inventors have found that an excellent magnet alloy powder can be obtained, and have completed the present invention.
即ち、本発明の第1の発明によれば、希土類元素を含む鉄系磁石合金粉からなる磁石粉末(A)が、少なくともアルミニウム、亜鉛、マンガン、銅又はカルシウムから選ばれた1種以上の金属の酸化物、複合酸化物、リン酸塩又はリン酸水素化合物とリン酸が添加された有機溶媒中で、平均粒径8μm以下に粉砕されることで、磁石合金粉の表面上に、鉄と希土類元素の金属リン酸塩(b−1)、及びアルミニウム、亜鉛、マンガン、銅又はカルシウムから選ばれた1種以上の金属リン酸塩(b−2)からなる複合金属リン酸塩被膜(B)が均一に形成されており、かつ、金属リン酸塩(b−2)の金属成分が、複合金属リン酸塩被膜(B)の金属成分に対して50重量%以上であることを特徴とする耐塩水性磁石合金粉が提供される。 That is, according to the first invention of the present invention, the magnet powder (A) made of an iron-based magnet alloy powder containing a rare earth element is at least one metal selected from aluminum, zinc, manganese, copper or calcium. In an organic solvent to which an oxide, a composite oxide, a phosphate or a hydrogen phosphate compound and phosphoric acid are added , the average particle size is pulverized to 8 μm or less. Composite metal phosphate coating (B) comprising a rare earth element metal phosphate (b-1) and one or more metal phosphates (b-2) selected from aluminum, zinc, manganese, copper or calcium ) Is uniformly formed, and the metal component of the metal phosphate (b-2) is 50% by weight or more based on the metal component of the composite metal phosphate coating (B). A salt-resistant magnetic alloy powder is provided.
また、本発明の第2の発明によれば、第1の発明において、複合金属リン酸塩被膜(B)の厚さが、5〜100nmであることを特徴とする耐塩水性磁石合金粉が提供される。 According to the second invention of the present invention, there is provided a salt-water resistant magnetic alloy powder characterized in that, in the first invention, the composite metal phosphate coating (B) has a thickness of 5 to 100 nm. Is done.
また、本発明の第3の発明によれば、第1の発明において、有機溶媒が、N,N−ジメチルホルムアミド、ホルムアミド、2−メトキシエタノール、エタノール、メタノール又はイソプロピルアルコールから選ばれた1種以上であることを特徴とする耐塩水性磁石合金粉が提供される。 According to the third invention of the present invention, in the first invention, the organic solvent is one or more selected from N, N-dimethylformamide, formamide, 2-methoxyethanol, ethanol, methanol or isopropyl alcohol. A salt-water resistant magnetic alloy powder is provided.
また、本発明の第4の発明によれば、第1の発明において、リン酸塩溶液を形成する金属成分は、希土類元素を含む鉄系磁石合金粉に対して、0.01〜1mol/kg(粉末重量当たり)の割合で添加されることを特徴とする耐塩水性磁石合金粉が提供される。 According to the fourth invention of the present invention, in the first invention, the metal component forming the phosphate solution is 0.01 to 1 mol / kg with respect to the iron-based magnet alloy powder containing the rare earth element. A salt-water resistant magnetic alloy powder characterized in that it is added at a ratio of (per powder weight) is provided.
さらに、本発明の第5の発明によれば、第1の発明において、リン酸は、希土類元素を含む鉄系磁石合金粉に対して、0.1〜2mol/kg(粉末重量当たり)の割合で添加されることを特徴とする耐熱性磁石合金粉が提供される。 Furthermore, according to the fifth invention of the present invention, in the first invention, phosphoric acid is a ratio of 0.1 to 2 mol / kg (per powder weight) with respect to the iron-based magnet alloy powder containing rare earth elements. A heat-resistant magnet alloy powder is provided, which is characterized in that it is added in the following manner.
一方、本発明の第6の発明によれば、第1〜5のいずれかの耐塩水性磁石合金粉に、少なくとも熱可塑性樹脂を含有してなるボンド磁石用樹脂組成物が提供される。 On the other hand, according to the sixth aspect of the present invention, there is provided a bonded magnet resin composition comprising at least a thermoplastic resin in any of the salt-resistant water-resistant magnet alloy powders of the first to fifth aspects.
また、本発明の第7の発明によれば、第6の発明のボンド磁石用樹脂組成物を、射出成形法、射出圧縮成形法、押出成形法又は射出プレス成形法から選ばれるいずれかの成形法により成形したボンド磁石が提供される。 According to the seventh invention of the present invention, the bonded magnet resin composition of the sixth invention is molded by any one selected from an injection molding method, an injection compression molding method, an extrusion molding method or an injection press molding method. A bonded magnet molded by the method is provided.
さらに、本発明の第8の発明によれば、第1〜5のいずれかの耐塩水性磁石合金粉を圧密化して、見かけ密度を真密度の85%以上にしたことを特徴とする圧密磁石が提供される。 Furthermore, according to the eighth invention of the present invention, there is provided a compacted magnet characterized in that the salt-water resistant magnet alloy powder according to any one of the first to fifth items is consolidated to make the apparent density 85% or more of the true density. Provided.
以上説明したように、本発明の磁石合金粉は、その表面を特定の金属リン酸塩が複合化した被膜によって均一に保護されているため、従来法により得られる磁石合金粉とは異なり、塩水に触れる環境下で錆が発生しない。この磁石合金粉を用いれば、耐塩水性ボンド磁石および圧密磁石の製造が可能となり、その工業的価値は極めて大きい。 As described above, the magnetic alloy powder of the present invention is uniformly protected on its surface by a film in which a specific metal phosphate is complexed. Therefore, unlike the magnetic alloy powder obtained by the conventional method, Rust does not occur in an environment where it touches. If this magnet alloy powder is used, it becomes possible to produce salt-resistant bond magnets and compacted magnets, and their industrial value is extremely high.
以下、本発明の耐塩水性磁石合金粉、及びそれを用いたボンド磁石用樹脂組成物、ボンド磁石又は圧密磁石について詳細に説明する。 Hereinafter, the salt-water resistant magnetic alloy powder of the present invention, and the resin composition for bonded magnets, bonded magnets or compacted magnets using the same will be described in detail.
1.耐塩水性磁石合金粉
本発明の耐塩水性磁石合金粉は、希土類元素を含む鉄系磁石合金粉からなる磁石合金粉(A)の表面に、特定な金属リン酸塩が複合化した被膜(B)を形成してなる耐塩水性磁石合金粉である。
1. Salt-resistant magnetic alloy powder The salt-resistant magnetic alloy powder of the present invention is a film (B) in which a specific metal phosphate is combined on the surface of a magnetic alloy powder (A) made of an iron-based magnet alloy powder containing a rare earth element. Is a salt water-resistant magnetic alloy powder.
A 磁石合金粉
磁石合金粉は、希土類元素を含む鉄系磁石合金の粉末であれば、特に制限されない。希土類−鉄系磁石合金粉としては、例えば、希土類−鉄−ほう素系、希土類−鉄−窒素系などの各種磁石合金粉を使用でき、中でも希土類−鉄−窒素系の磁石合金粉が好適である。希土類元素としては、Sm、Nd、Pr、Y、La、Ce、またはGd等が挙げられ、単独若しくは混合物として使用できる。これらの中では、特にSm又はNdを5〜40at.%、Feを50〜90at.%含有するものが好ましい。
A Magnet alloy powder The magnet alloy powder is not particularly limited as long as it is a powder of an iron-based magnet alloy containing a rare earth element. As the rare earth-iron-based magnet alloy powder, for example, various magnetic alloy powders such as rare-earth-iron-boron-based and rare-earth-iron-nitrogen-based can be used. is there. Examples of the rare earth element include Sm, Nd, Pr, Y, La, Ce, and Gd, which can be used alone or as a mixture. Among these, in particular, Sm or Nd is 5 to 40 at. %, Fe 50-90 at. % Content is preferred.
希土類−鉄系磁石合金粉には、フェライト、アルニコなど、ボンド磁石や圧密磁石の原料となる各種磁石合金粉を混合してもよく、異方性磁石合金粉だけでなく、等方性磁石合金粉も対象となるが、異方性磁場(HA)が、4.0MA/m以上の磁石合金粉が好ましい。 The rare earth-iron-based magnet alloy powder may be mixed with various magnetic alloy powders, such as ferrite and alnico, which are raw materials for bonded magnets and compacted magnets. Although powder is also an object, magnet alloy powder having an anisotropic magnetic field (HA) of 4.0 MA / m or more is preferable.
また、ボンド磁石や圧密磁石の原料となるため、磁石合金粉の平均粒径は、8μm以下、特に5μm以下であることが望ましい。平均粒径が8μmを超えると、成形性が悪化するので好ましくない。 Moreover, since it becomes a raw material of a bond magnet or a compacted magnet, the average particle diameter of the magnet alloy powder is desirably 8 μm or less, particularly 5 μm or less. If the average particle size exceeds 8 μm, the moldability deteriorates, which is not preferable.
B 複合金属リン酸塩被膜
本発明の磁石合金粉は、その表面が鉄と希土類元素の金属リン酸塩(b−1)、及びアルミニウム、亜鉛、マンガン、銅又はカルシウムのいずれか1種以上を含む金属のリン酸塩(b−2)が複合化した被膜で均一に被覆されている。ここで、均一に被覆されるとは、磁石合金粉表面の80%以上、好ましくは85%以上、さらに好ましくは90%以上が複合金属リン酸塩被膜で覆われていることをいう。
B. Composite metal phosphate coating The magnet alloy powder of the present invention has at least one of iron and rare earth metal phosphate (b-1) and aluminum, zinc, manganese, copper or calcium. The metal phosphate (b-2) contained is uniformly coated with a composite film. Here, being uniformly coated means that 80% or more, preferably 85% or more, more preferably 90% or more of the surface of the magnet alloy powder is covered with the composite metal phosphate coating.
金属リン酸塩(b−1)は、リン酸サマリウム、リン酸鉄などで、これは磁石合金粉を構成する希土類や鉄にリン酸が反応して形成されたものである。一方、金属リン酸塩(b−2)は、例えば、リン酸アルミニウム、リン酸亜鉛、リン酸マンガン、リン酸銅、リン酸カルシウム又はこれらが2種以上複合した金属塩などである。これらアルミニウム、亜鉛、マンガン、銅およびカルシウム以外に、クロム、ニッケル、マグネシウムなどの金属リン酸塩が含まれていてもかまわない。 The metal phosphate (b-1) is samarium phosphate, iron phosphate or the like, which is formed by reacting phosphoric acid with the rare earth or iron constituting the magnet alloy powder. On the other hand, the metal phosphate (b-2) is, for example, aluminum phosphate, zinc phosphate, manganese phosphate, copper phosphate, calcium phosphate, or a metal salt in which two or more of these are combined. In addition to these aluminum, zinc, manganese, copper and calcium, metal phosphates such as chromium, nickel and magnesium may be contained.
金属リン酸塩(b−1)と、金属リン酸塩(b−2)とが複合化した金属リン酸塩は、樹脂バインダーとの結合力を高め、磁石合金粉の耐塩水性を高める成分である。但し、充分な耐塩水性を得るためには、金属リン酸塩(b−2)の金属成分、すなわちアルミニウム、亜鉛、マンガン、銅又はカルシウムから選択された1種以上が、複合金属リン酸塩被膜(B)の金属成分に対して、50重量%以上、好ましくは80重量%以上含まれた複合金属リン酸塩とする。 The metal phosphate in which the metal phosphate (b-1) and the metal phosphate (b-2) are combined is a component that increases the binding strength with the resin binder and increases the salt water resistance of the magnet alloy powder. is there. However, in order to obtain sufficient salt water resistance, the metal component of the metal phosphate (b-2), that is, one or more selected from aluminum, zinc, manganese, copper or calcium is a composite metal phosphate coating. A composite metal phosphate containing 50% by weight or more, preferably 80% by weight or more based on the metal component (B).
複合金属リン酸塩被膜は、平均で5〜100nmの厚さが必要である。平均厚さが5nm未満であると十分な耐塩水性が得られず、一方、100nmを越えると磁気特性が低下し、またボンド磁石を作製する際には混練性や成形性が低下する。 The composite metal phosphate coating must have an average thickness of 5 to 100 nm. When the average thickness is less than 5 nm, sufficient salt water resistance cannot be obtained. On the other hand, when the average thickness exceeds 100 nm, the magnetic properties are deteriorated, and when a bonded magnet is produced, kneadability and formability are deteriorated.
この磁石合金粉を樹脂バインダーと混合してボンド磁石を作製した場合、海水の塩分濃度付近である5%塩水中に24時間浸漬しても、ボンド磁石に赤錆は全く生じない。また磁石合金粉を圧密化した磁石についても、同様に高い耐塩水性を示す。 When this magnet alloy powder is mixed with a resin binder to produce a bonded magnet, no red rust is generated in the bonded magnet even if it is immersed in 5% salt water near the salt concentration of seawater for 24 hours. Similarly, magnets made by compacting magnet alloy powder also exhibit high salt water resistance.
2.耐塩水性磁石合金粉の製造方法
本発明の耐塩水性磁石合金粉を製造するには、希土類元素を含む鉄系磁石合金粉を、一段階で複合リン酸塩化するか、二段階で複合リン酸塩化するかで区別される二通りの方法がある。
2. Method for Producing Salt-Resistant Magnetic Alloy Powder In order to produce the salt-resistant magnetic alloy powder of the present invention, iron-based magnet alloy powder containing rare earth elements is complexed in one stage or complexed in two stages. There are two ways to distinguish between.
希土類元素を含む鉄系磁石合金粉を、一段階で複合リン酸塩化する方法とは、平均粒径20μmを超える希土類元素を含む鉄系磁石合金粉を、有機溶媒中で、平均粒径8μm以下に粉砕する際、少なくともアルミニウム、亜鉛、マンガン、銅又はカルシウムから選ばれた1種以上の金属の酸化物、複合酸化物、リン酸塩又はリン酸水素化合物と、リン酸を添加した後、該溶液を攪拌する方法である。 The method of complex phosphating iron-based magnet alloy powder containing rare earth elements in one step is that iron-based magnet alloy powder containing rare earth elements having an average particle size exceeding 20 μm is averaged in an organic solvent with an average particle size of 8 μm or less. When pulverizing to at least one oxide of at least one metal selected from aluminum, zinc, manganese, copper or calcium, a composite oxide, a phosphate or a hydrogen phosphate compound, and after adding phosphoric acid, This is a method of stirring the solution.
先ず、平均粒径20μmを超える希土類元素を含む鉄系磁石合金の粉末に、有機溶媒を加え、磁石合金粉の粉砕前、あるいは粉砕中に、アルミニウム、亜鉛、マンガン、銅又はカルシウムから選ばれた1種以上の酸化物、リン酸塩又はリン酸水素化合物の1種以上からなる金属成分を添加する。該金属成分がリン酸塩又はリン酸水素化合物以外の場合、及びリン酸塩又はリン酸水素化合物が有機溶媒に溶解し難い場合には、リン酸を添加して、攪拌を続ける。攪拌は、通常1〜180分間続行する。 First, an organic solvent was added to a powder of an iron-based magnet alloy containing a rare earth element having an average particle size exceeding 20 μm, and the powder was selected from aluminum, zinc, manganese, copper, or calcium before or during pulverization of the magnet alloy powder. A metal component composed of one or more oxides, phosphates or hydrogen phosphate compounds is added. When the metal component is other than a phosphate or a hydrogen phosphate compound, and when the phosphate or hydrogen phosphate compound is difficult to dissolve in an organic solvent, phosphoric acid is added and stirring is continued. Stirring is usually continued for 1 to 180 minutes.
金属成分は、アルミニウム、亜鉛、マンガン、銅又はカルシウムなどのイオンの供給源であり、有機溶媒に溶け金属イオンを生成する酸化物、複合酸化物、リン酸塩又はリン酸水素化合物などの金属化合物である。 The metal component is a source of ions such as aluminum, zinc, manganese, copper or calcium, and a metal compound such as an oxide, composite oxide, phosphate or hydrogen phosphate compound that dissolves in an organic solvent and generates metal ions It is.
有機溶媒としては、特に制限はなく、2−メトキシエタノール、イソプロピルアルコール、エタノール、トルエン、メタノール、ヘキサン等のいずれか1種または2種以上の混合物を用いると良い。但し、メタノールは、リン酸と速やかに反応してエステル化し、良好な被覆が形成されるのを妨げる恐れがあるので取り扱いには注意を要する。 There is no restriction | limiting in particular as an organic solvent, It is good to use any 1 type, or 2 or more types of mixtures, such as 2-methoxyethanol, isopropyl alcohol, ethanol, toluene, methanol, hexane. However, since methanol reacts quickly with phosphoric acid to esterify and prevent the formation of a good coating, it must be handled with care.
前記の金属成分が容易に金属イオンを生成し、磁石合金粉の溶解を適度に調整するためには、N,N−ジメチルホルムアミド、ホルムアミド等の極性溶媒を混合することが望ましい。また、磁石合金粉の溶解を促進するために、有機溶媒に水や酸を混合しても良い。 In order for the metal component to easily generate metal ions and appropriately adjust the dissolution of the magnet alloy powder, it is desirable to mix a polar solvent such as N, N-dimethylformamide or formamide. Moreover, in order to accelerate | stimulate melt | dissolution of magnet alloy powder, you may mix water and an acid with an organic solvent.
アルミニウム化合物としては、アルミニウムイオンの供給源となり、有機溶媒に溶ける化合物であれば、特に制限されず、例えば、酢酸アルミニウム、硫酸アルミニウム、塩化アルミニウム、塩化アルミニウムアンモニウム、安息香酸アルミニウム、炭酸アルミニウム、エチルアセト酢酸アルミニウム、ぎ酸アルミニウム、水酸化アルミニウム、硝酸アルミニウム、ナフテン酸アルミニウム、オレイン酸アルミニウム、しゅう酸アルミニウム、酸化アルミニウム、リン酸アルミニウム、リン酸水素アルミニウム、塩化カリウムアルミニウム、ステアリン酸アルミニウム、硫化アルミニウム、フタロシアニンアルミニウム、又は酒石酸アルミニウムが例示される。特に好ましいのは、リン酸アルミニウム、あるいはリン酸水素アルミニウムである。 The aluminum compound is not particularly limited as long as it is a source of aluminum ions and is soluble in an organic solvent. For example, aluminum acetate, aluminum sulfate, aluminum chloride, aluminum chloride ammonium, aluminum benzoate, aluminum carbonate, ethyl acetoacetate Aluminum, aluminum formate, aluminum hydroxide, aluminum nitrate, aluminum naphthenate, aluminum oleate, aluminum oxalate, aluminum oxide, aluminum phosphate, aluminum hydrogen phosphate, potassium chloride aluminum, aluminum stearate, aluminum sulfide, phthalocyanine aluminum Or aluminum tartrate. Particularly preferred is aluminum phosphate or aluminum hydrogen phosphate.
亜鉛化合物としては、亜鉛イオンの供給源となり、有機溶媒に溶ける化合物であれば、特に制限されず、例えば、酢酸亜鉛、硫酸亜鉛、塩化亜鉛、塩化亜鉛アンモニウム、安息香酸亜鉛、炭酸亜鉛、エチルアセト酢酸亜鉛、ぎ酸亜鉛、水酸化亜鉛、硝酸亜鉛、ナフテン酸亜鉛、オレイン酸亜鉛、しゅう酸亜鉛、酸化亜鉛、リン酸亜鉛、リン酸亜鉛四水和物、リン酸水素亜鉛、リン酸亜鉛カルシウム、塩化カリウム亜鉛、ステアリン酸亜鉛、硫化亜鉛、フタロシアニン亜鉛、又は酒石酸亜鉛が例示される。特に好ましいのは、酸化亜鉛、リン酸亜鉛四水和物、或いはリン酸水素亜鉛である。 The zinc compound is not particularly limited as long as it is a source of zinc ions and is soluble in an organic solvent. For example, zinc acetate, zinc sulfate, zinc chloride, zinc ammonium chloride, zinc benzoate, zinc carbonate, ethyl acetoacetate Zinc, zinc formate, zinc hydroxide, zinc nitrate, zinc naphthenate, zinc oleate, zinc oxalate, zinc oxide, zinc phosphate, zinc phosphate tetrahydrate, zinc hydrogen phosphate, zinc calcium phosphate, Examples include potassium zinc chloride, zinc stearate, zinc sulfide, zinc phthalocyanine, or zinc tartrate. Particularly preferred is zinc oxide, zinc phosphate tetrahydrate, or zinc hydrogen phosphate.
マンガン化合物としては、マンガンイオンの供給源となり、有機溶媒に溶ける化合物であれば、特に制限されず、例えば、酢酸マンガン、硫酸マンガン、塩化マンガン、塩化マンガンアンモニウム、安息香酸マンガン、炭酸マンガン、エチルアセト酢酸マンガン、ぎ酸マンガン、水酸化マンガン、硝酸マンガン、ナフテン酸マンガン、オレイン酸マンガン、しゅう酸マンガン、酸化マンガン、リン酸マンガン、リン酸水素マンガン、塩化カリウムマンガン、ステアリン酸マンガン、硫化マンガン、フタロシアニンマンガン、又は酒石酸マンガンが例示される。特に好ましいのは、酸化マンガン、或いはリン酸水素マンガンである。 The manganese compound is not particularly limited as long as it is a source of manganese ions and is soluble in an organic solvent. For example, manganese acetate, manganese sulfate, manganese chloride, manganese chloride, manganese benzoate, manganese carbonate, ethyl acetoacetate Manganese, manganese formate, manganese hydroxide, manganese nitrate, manganese naphthenate, manganese oleate, manganese oxalate, manganese oxide, manganese phosphate, manganese hydrogen phosphate, potassium chloride, manganese stearate, manganese sulfide, manganese phthalocyanine Or manganese tartrate. Particularly preferred is manganese oxide or manganese hydrogen phosphate.
また、銅化合物としては、銅イオンの供給源となり、有機溶媒に溶ける化合物であれば、特に制限されず、例えば、酢酸銅、硫酸銅、塩化銅、塩化銅アンモニウム、安息香酸銅、炭酸銅、エチルアセト酢酸銅、ぎ酸銅、水酸化銅、硝酸銅、ナフテン酸銅、オレイン酸銅、しゅう酸銅、酸化銅、リン酸銅、リン酸水素銅、塩化カリウム銅、ステアリン酸銅、硫化銅、フタロシアニン銅、または酒石酸銅などが用いられる。特に好ましいのは、酸化銅(I)、或いはリン酸水素銅である。 The copper compound is not particularly limited as long as it is a compound that is a source of copper ions and is soluble in an organic solvent. For example, copper acetate, copper sulfate, copper chloride, ammonium copper chloride, copper benzoate, copper carbonate, Copper ethyl acetoacetate, copper formate, copper hydroxide, copper nitrate, copper naphthenate, copper oleate, copper oxalate, copper oxide, copper phosphate, copper hydrogen phosphate, potassium copper chloride, copper stearate, copper sulfide, For example, copper phthalocyanine or copper tartrate is used. Particularly preferred is copper (I) oxide or copper hydrogen phosphate.
さらに、カルシウム化合物としては、カルシウムイオンの供給源となり、有機溶媒に溶ける化合物であれば、特に制限されず、例えば、酢酸カルシウム、硫酸カルシウム、塩化カルシウム、塩化カルシウムアンモニウム、安息香酸カルシウム、炭酸カルシウム、エチルアセト酢酸カルシウム、ぎ酸カルシウム、水酸化カルシウム、硝酸カルシウム、ナフテン酸カルシウム、オレイン酸カルシウム、しゅう酸カルシウム、酸化カルシウム、リン酸カルシウム、リン酸水素カルシウム、塩化カリウムカルシウム、ステアリン酸カルシウム、硫化カルシウム、フタロシアニンカルシウム、又は酒石酸カルシウムが例示される。特に好ましいのは、酸化カルシウム、或いはリン酸水素カルシウムである。 Furthermore, the calcium compound is not particularly limited as long as it is a source of calcium ions and is soluble in an organic solvent. For example, calcium acetate, calcium sulfate, calcium chloride, calcium chloride ammonium, calcium benzoate, calcium carbonate, Calcium ethyl acetoacetate, calcium formate, calcium hydroxide, calcium nitrate, calcium naphthenate, calcium oleate, calcium oxalate, calcium oxide, calcium phosphate, calcium hydrogen phosphate, potassium chloride, calcium stearate, calcium sulfide, calcium phthalocyanine, Or calcium tartrate is illustrated. Particularly preferred is calcium oxide or calcium hydrogen phosphate.
金属成分であるアルミニウム、亜鉛、マンガン、銅又はカルシウムから選ばれた1種以上の金属の酸化物、複合酸化物、リン酸塩又はリン酸水素化合物は、粉砕する磁石合金粉の粒径、表面積等に合わせて最適量を添加するが、該磁石合金粉に対して、0.01〜1mol/kg(粉末重量当たり)とする。すなわち、0.01mol/kg未満であると磁石合金粉の表面が十分に被覆されないために耐塩水性が改善されず、1mol/kgを超えると磁化の低下が著しくなり、磁石としての性能が低下する。 One or more metal oxides, composite oxides, phosphates or hydrogen phosphates selected from aluminum, zinc, manganese, copper or calcium, which are metal components, are the particle size and surface area of the magnet alloy powder to be crushed. The optimum amount is added in accordance with the above, but is 0.01 to 1 mol / kg (per powder weight) with respect to the magnet alloy powder. That is, when the amount is less than 0.01 mol / kg, the surface of the magnet alloy powder is not sufficiently covered, so that the salt water resistance is not improved. When the amount exceeds 1 mol / kg, the magnetization is remarkably lowered, and the performance as a magnet is lowered. .
上記の金属化合物は、溶媒中でイオン化し、磁石合金粉の成分である希土類金属や鉄が溶媒へ溶け出すにともない、磁石合金粉の表面で反応して金属リン酸塩が複合した被膜を形成する。 The above metal compounds are ionized in a solvent and react with the surface of the magnet alloy powder to form a composite film of metal phosphates as the rare earth metal and iron, which are components of the magnet alloy powder, dissolve into the solvent. To do.
リン酸としては、金属化合物と反応して金属リン酸塩を生成するオルトリン酸をはじめ、亜リン酸、次亜リン酸、ピロリン酸、直鎖状のポリリン酸、環状のメタリン酸が使用できる。また、リン酸アンモニウム、リン酸アンモニウムマグネシウムなども使用できる。これら化合物は、単独でも複数種を組み合わせてもよく、通常、キレート剤、中和剤などと混合して処理剤とされる。 Examples of phosphoric acid include orthophosphoric acid that reacts with a metal compound to form a metal phosphate, phosphorous acid, hypophosphorous acid, pyrophosphoric acid, linear polyphosphoric acid, and cyclic metaphosphoric acid. Moreover, ammonium phosphate, ammonium magnesium phosphate, etc. can also be used. These compounds may be used alone or in combination of a plurality of types, and are usually mixed with a chelating agent, a neutralizing agent or the like to form a treating agent.
これらのうち、オルトリン酸が好ましい性能を発揮するが、その理由は、これが上記の金属化合物と反応しやすく、希土類系金属を成分とする磁石合金粉の表面に保護膜を形成しやすいためと考えられる。 Among these, orthophosphoric acid exhibits desirable performance because it is easy to react with the above metal compound and to form a protective film on the surface of the magnet alloy powder containing rare earth metal as a component. It is done.
リン酸は、磁石合金粉の粒径、表面積等に合わせて最適量を添加するが、通常は、粉砕する磁石合金粉に対して0.1〜2mol/kg(粉末重量当たり)であり、好ましくは0.15〜1.5mol/kg、さらに好ましくは0.2〜0.4mol/kgである。 Phosphoric acid is added in an optimum amount according to the particle diameter, surface area, etc. of the magnet alloy powder, but is usually 0.1 to 2 mol / kg (per powder weight) with respect to the magnet alloy powder to be pulverized, preferably Is 0.15 to 1.5 mol / kg, more preferably 0.2 to 0.4 mol / kg.
すなわち、0.1mol/kg未満であると、磁石合金粉の表面が十分に被覆されないために耐塩水性が改善されず、また大気中で乾燥させると酸化・発熱して磁気特性が極端に低下する。2mol/kgを超えると、磁石合金粉との反応が激しく起こって磁石合金粉が溶解する。 That is, when the amount is less than 0.1 mol / kg, the surface of the magnet alloy powder is not sufficiently covered, so that the salt water resistance is not improved, and when dried in the air, the magnetic properties are extremely lowered due to oxidation and heat generation. . When it exceeds 2 mol / kg, the reaction with the magnet alloy powder occurs vigorously and the magnet alloy powder is dissolved.
リン酸の濃度は、特に制限されず、無水リン酸、50〜99%リン酸水溶液(例えば、85%リン酸水溶液、75%リン酸水溶液)などが用いられる。なお、有機溶剤も、特に制限はなく、通常はエタノールまたはイソプロピルアルコール等のアルコール類、ケトン類、低級炭化水素類、芳香族類、またはこれらの混合物が用いられる。但し、メタノールは、リン酸と速やかに反応してエステル化し、良好な被覆が形成されるのを妨げる恐れがあるので取り扱いには注意を要する。 The concentration of phosphoric acid is not particularly limited, and phosphoric anhydride, 50-99% phosphoric acid aqueous solution (for example, 85% phosphoric acid aqueous solution, 75% phosphoric acid aqueous solution) and the like are used. The organic solvent is not particularly limited, and usually alcohols such as ethanol or isopropyl alcohol, ketones, lower hydrocarbons, aromatics, or a mixture thereof is used. However, since methanol reacts quickly with phosphoric acid to esterify and prevent the formation of a good coating, it must be handled with care.
金属成分を添加する時期は、磁石粉末を粉砕する際で有れば、いつでも良く、粉砕前に溶媒に溶かしておき、粉砕途中に一度に添加する方法、粉砕中、徐々に添加する方法などが用いられる。 The metal component may be added at any time as long as the magnetic powder is pulverized, and may be dissolved in a solvent before pulverization and added at one time during pulverization, or gradually added during pulverization. Used.
これによって、粉砕中に溶けだした希土類元素、鉄など磁石を構成する元素がリン酸塩を形成し、これに添加した金属化合物も反応しあって、複合金属リン酸塩が磁石合金粉を被覆する。この反応が完結し、充分な膜厚の被膜を形成するには、金属化合物の種類などにもよるが、1〜180分間、好ましくは3〜150分、さらに好ましくは5〜60分の攪拌(粉砕)、保持時間が必要である。 As a result, rare earth elements dissolved during grinding, elements constituting the magnet such as iron form phosphates, and metal compounds added thereto react with each other, and the composite metal phosphate covers the magnet alloy powder. . In order to complete this reaction and form a film having a sufficient film thickness, depending on the type of metal compound, etc., it is stirred for 1 to 180 minutes, preferably 3 to 150 minutes, more preferably 5 to 60 minutes. Pulverization), holding time is required.
平均粒径20μmを超える鉄系磁石合金粗粉は、平均粒径8μm以下、好ましくは1〜5μmまで粉砕される。 The iron-based magnet alloy coarse powder having an average particle size exceeding 20 μm is pulverized to an average particle size of 8 μm or less, preferably 1 to 5 μm.
複合リン酸塩被膜を形成させる第二の方法は、先ず、リン酸を含む有機溶媒に磁石合金粉を配合して該合金粉を粉砕し、次に、このリン酸塩溶液に金属化合物を添加して攪拌する方法である。 The second method for forming the composite phosphate coating is to first mix the magnet alloy powder in an organic solvent containing phosphoric acid, pulverize the alloy powder, and then add the metal compound to the phosphate solution. And stirring.
有機溶媒の種類、リン酸や金属成分の添加量などは、前記第一の方法と同じ条件が採用される。第二の方法であれば、耐塩水性に優れる金属リン酸塩(b−2)が、金属リン酸塩(b−1)よりも後に形成されるので、さらに良好な複合金属リン酸塩被膜が得られるので一層有利である。 The same conditions as in the first method are employed for the type of organic solvent, the addition amount of phosphoric acid and metal components, and the like. In the second method, since the metal phosphate (b-2) having excellent salt water resistance is formed after the metal phosphate (b-1), an even better composite metal phosphate coating is formed. Since it is obtained, it is more advantageous.
上記のうち、いずれかの湿式処理法で被覆処理された磁石合金粉は、その後に加熱し乾燥することで、表面の被膜が磁石合金粉に定着する。すなわち、処理溶液と磁石合金粉は、被膜形成後に、100〜500℃の真空オーブン中で1〜30時間乾燥させる。不活性ガス中または真空中で加熱処理を施すことが好ましい。100℃未満で加熱処理を施すと、磁石合金粉の乾燥が十分進まずに、安定な表面被膜の形成が阻害され、また、500℃を超える温度で加熱処理を施すと、磁石合金粉が熱的なダメージを受け、保磁力がかなり低くなるという問題がある。 Among the above, the magnet alloy powder coated by any of the wet processing methods is heated and dried thereafter, so that the coating on the surface is fixed to the magnet alloy powder. That is, the treatment solution and the magnet alloy powder are dried in a vacuum oven at 100 to 500 ° C. for 1 to 30 hours after the coating is formed. Heat treatment is preferably performed in an inert gas or in a vacuum. When heat treatment is performed at a temperature lower than 100 ° C., the drying of the magnet alloy powder does not proceed sufficiently and the formation of a stable surface film is hindered. When the heat treatment is performed at a temperature exceeding 500 ° C., the magnet alloy powder is heated. There is a problem that the coercive force is considerably lowered due to damage.
金属リン酸塩被膜を形成した耐塩水性磁石合金粉には、必要に応じて、さらにシラン系、アルミネート系、チタネート系など各種のカップリング剤やアビエチン酸系化合物などから選択された1種以上を用いて被覆してもよい。 The salt-resistant water-resistant magnet alloy powder on which the metal phosphate coating is formed may be one or more selected from various coupling agents such as silane-based, aluminate-based, titanate-based, and abietic acid-based compounds as necessary. You may coat using.
3.ボンド磁石用樹脂組成物及びボンド磁石
本発明のボンド磁石は、金属リン酸塩を被覆した耐塩水性磁石合金粉に、熱可塑性樹脂や熱硬化性樹脂を樹脂バインダーとして配合することで容易に製造できる。
3. Bonded Magnet Resin Composition and Bonded Magnet The bonded magnet of the present invention can be easily produced by blending a salt-resistant water-resistant magnet alloy powder coated with a metal phosphate with a thermoplastic resin or a thermosetting resin as a resin binder. .
樹脂バインダーは、磁石粉末の結合材として働く成分であり、ポリアミド樹脂、ポリフェニレンサルファイド樹脂などの熱可塑性樹脂、あるいは、エポキシ樹脂、ビス・マレイミドトリアジン樹脂、不飽和ポリエステル樹脂、ビニルエステル樹脂、硬化反応型シリコーンゴムなどの熱硬化性樹脂が使用できるが、特に熱可塑性樹脂が好ましい。 Resin binder is a component that acts as a binder for magnet powder, and is a thermoplastic resin such as polyamide resin, polyphenylene sulfide resin, or epoxy resin, bis-maleimide triazine resin, unsaturated polyester resin, vinyl ester resin, curing reaction type Although thermosetting resins such as silicone rubber can be used, thermoplastic resins are particularly preferable.
熱可塑性樹脂は、特に制限されず、従来樹脂バインダーとして公知のものを使用できる。熱可塑性樹脂の具体例としては、6ナイロン、6、6ナイロン、11ナイロン、12ナイロン、6、12ナイロン、芳香族系ナイロン、これらの分子を一部変性した変性ナイロン等のポリアミド樹脂;直鎖型ポリフェニレンサルファイド樹脂、架橋型ポリフェニレンサルファイド樹脂、セミ架橋型ポリフェニレンサルファイド樹脂;低密度ポリエチレン、線状低密度ポリエチレン樹脂、高密度ポリエチレン樹脂、超高分子量ポリエチレン樹脂、ポリプロピレン樹脂、エチレン−酢酸ビニル共重合樹脂、エチレン−エチルアクリレート共重合樹脂、アイオノマー樹脂、ポリメチルペンテン樹脂;ポリスチレン樹脂、アクリロニトリル−ブタジエン−スチレン共重合樹脂、アクリロニトリル−スチレン共重合樹脂;ポリ塩化ビニル樹脂、ポリ塩化ビニリデン樹脂、ポリ酢酸ビニル樹脂、ポリビニルアルコール樹脂、ポリビニルブチラール樹脂、ポリビニルホルマール樹脂;メタクリル樹脂;ポリフッ化ビニリデン樹脂、ポリ三フッ化塩化エチレン樹脂、四フッ化エチレン−六フッ化プロピレン共重合樹脂、エチレン−四フッ化エチレン共重合樹脂、四フッ化エチレン−パーフルオロアルキルビニルエーテル共重合樹脂、ポリテトラフルオロエチレン樹脂;ポリカーボネート樹脂、ポリアセタール樹脂、ポリエチレンテレフタレート樹脂、ポリブチレンテレフタレート樹脂、ポリフェニレンオキサイド樹脂、ポリアリルエーテルアリルスルホン樹脂、ポリエーテルスルホン樹脂、ポリエーテルエーテルケトン樹脂、ポリアリレート樹脂、芳香族ポリエステル樹脂、酢酸セルロース樹脂、前出の各樹脂系エラストマー等が挙げられ、これらの単重合体や他種モノマーとのランダム共重合体、ブロック共重合体、グラフト共重合体、他の物質による末端基変性品等が挙げられる。 The thermoplastic resin is not particularly limited, and a conventionally known resin binder can be used. Specific examples of the thermoplastic resin include 6 nylon, 6, 6 nylon, 11 nylon, 12 nylon, 6, 12 nylon, aromatic nylon, polyamide resin such as modified nylon partially modified from these molecules; Type polyphenylene sulfide resin, crosslinked polyphenylene sulfide resin, semi-crosslinked polyphenylene sulfide resin; low density polyethylene, linear low density polyethylene resin, high density polyethylene resin, ultrahigh molecular weight polyethylene resin, polypropylene resin, ethylene-vinyl acetate copolymer resin , Ethylene-ethyl acrylate copolymer resin, ionomer resin, polymethylpentene resin; polystyrene resin, acrylonitrile-butadiene-styrene copolymer resin, acrylonitrile-styrene copolymer resin; polyvinyl chloride resin, polychlorinated resin Nylidene resin, polyvinyl acetate resin, polyvinyl alcohol resin, polyvinyl butyral resin, polyvinyl formal resin; methacrylic resin; polyvinylidene fluoride resin, polytrifluoroethylene chloride resin, tetrafluoroethylene-hexafluoropropylene copolymer resin, ethylene -Tetrafluoroethylene copolymer resin, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer resin, polytetrafluoroethylene resin; polycarbonate resin, polyacetal resin, polyethylene terephthalate resin, polybutylene terephthalate resin, polyphenylene oxide resin, polyallyl ether Allyl sulfone resin, polyether sulfone resin, polyether ether ketone resin, polyarylate resin, aromatic polyester resin, cellulose acetate resin, front Mentioned respective resin elastomers, etc. are random copolymers of these homopolymers and other species monomer, block copolymers, graft copolymers, and end-group modified products by other materials.
これら熱可塑性樹脂は、得られるボンド磁石に所望の機械的強度が得られる範囲で、溶融粘度や分子量が低いものが望ましい。また、熱可塑性樹脂の形状は、パウダー状、ビーズ状、ペレット状等、特に限定されないが、磁石合金粉と均一に混合される点で、パウダー状が望ましい。 These thermoplastic resins are desirably those having a low melt viscosity and molecular weight within a range where desired mechanical strength can be obtained in the obtained bonded magnet. Further, the shape of the thermoplastic resin is not particularly limited, such as powder, bead, pellet, etc., but powder is preferable in that it is uniformly mixed with the magnet alloy powder.
熱可塑性樹脂の配合量は、磁石合金粉100重量部に対して、通常5〜100重量部、好ましくは5〜50重量部である。熱可塑性樹脂の配合量が5重量部未満であると、組成物の混練抵抗(トルク)が大きくなったり、流動性が低下して磁石の成形が困難となり、一方、100重量部を超えると、所望の磁気特性が得られない。 The compounding quantity of a thermoplastic resin is 5-100 weight part normally with respect to 100 weight part of magnet alloy powder, Preferably it is 5-50 weight part. When the blending amount of the thermoplastic resin is less than 5 parts by weight, the kneading resistance (torque) of the composition is increased, or the fluidity is lowered, making it difficult to mold the magnet. Desired magnetic properties cannot be obtained.
熱硬化性樹脂であれば、その取扱い性、ポットライフの面から2液型が有利であり、2液を混合後は、常温から200℃までの温度で硬化しうるものが好ましい。その反応機構は、一般的な付加重合型でも縮重合型であってもよい。また、必要に応じて過酸化物等の架橋反応型モノマーやオリゴマーを添加しても差し支えない。 If it is a thermosetting resin, a two-pack type is advantageous from the viewpoint of its handleability and pot life, and after mixing the two liquids, a resin that can be cured at a temperature from room temperature to 200 ° C. is preferable. The reaction mechanism may be a general addition polymerization type or a condensation polymerization type. Further, a crosslinking reaction type monomer or oligomer such as peroxide may be added as necessary.
これらは、反応可能な状態にあれば、重合度や分子量に制約されないが、硬化剤や他の添加剤等との最終混合状態で、ASTM100型レオメーターで測定した150℃における動的粘度が500Pa・s以下、好ましくは400Pa・s以下、特に好ましくは、100〜300Pa・sである。動的粘度が500Pa・sを超えると、成形時に著しい混練トルクの上昇、流動性の低下を招き、成形困難になるので好ましくない。一方、動的粘度が小さくなりすぎると、磁石粉末と樹脂バインダーが成形時に分離しやすくなるため、0.5Pa・s以上であることが望ましい。 These are not limited by the degree of polymerization or molecular weight as long as they are in a reactable state, but in a final mixed state with a curing agent or other additives, the dynamic viscosity at 150 ° C. measured by an ASTM 100 rheometer is 500 Pa. · S or less, preferably 400 Pa · s or less, particularly preferably 100 to 300 Pa · s. If the dynamic viscosity exceeds 500 Pa · s, the kneading torque is significantly increased during molding and the fluidity is lowered, which is not preferable because molding becomes difficult. On the other hand, if the dynamic viscosity becomes too small, the magnet powder and the resin binder are easily separated at the time of molding, and thus it is preferably 0.5 Pa · s or more.
樹脂バインダーは、磁石合金粉100重量部に対して、3〜50重量部の割合で添加される。添加量は7〜30重量部、さらには、10〜20重量部がより好ましい。3重量部未満では、著しい混練トルクの上昇、流動性の低下を招いて、成形困難になり、一方、50重量部を超えると、所望の磁気特性が得られないので好ましくない。 The resin binder is added at a ratio of 3 to 50 parts by weight with respect to 100 parts by weight of the magnet alloy powder. The addition amount is preferably 7 to 30 parts by weight, and more preferably 10 to 20 parts by weight. If it is less than 3 parts by weight, the kneading torque will be significantly increased and the fluidity will be lowered, making it difficult to mold. On the other hand, if it exceeds 50 parts by weight, the desired magnetic properties cannot be obtained, which is not preferable.
本発明における樹脂バインダーには、滑剤、紫外線吸収剤、難燃剤や種々の安定剤等を添加できる。 A lubricant, an ultraviolet absorber, a flame retardant, various stabilizers, and the like can be added to the resin binder in the present invention.
滑剤としては、例えば、パラフィンワックス、流動パラフィン、ポリエチレンワックス、ポリプロピレンワックス、エステルワックス、カルナウバ、マイクロワックス等のワックス類;ステアリン酸、1,2−オキシステアリン酸、ラウリン酸、パルミチン酸、オレイン酸等の脂肪酸類;ステアリン酸カルシウム、ステアリン酸バリウム、ステアリン酸マグネシウム、ステアリン酸リチウム、ステアリン酸亜鉛、ステアリン酸アルミニウム、ラウリン酸カルシウム、リノール酸亜鉛、リシノール酸カルシウム、2−エチルヘキソイン酸亜鉛等の脂肪酸塩(金属石鹸類);ステアリン酸アミド、オレイン酸アミド、エルカ酸アミド、ベヘン酸アミド、パルミチン酸アミド、ラウリン酸アミド、ヒドロキシステアリン酸アミド、メチレンビスステアリン酸アミド、エチレンビスステアリン酸アミド、エチレンビスラウリン酸アミド、ジステアリルアジピン酸アミド、エチレンビスオレイン酸アミド、ジオレイルアジピン酸アミド、N−ステアリルステアリン酸アミド等の脂肪酸アミド類;ステアリン酸ブチル等の脂肪酸エステル;エチレングリコール、ステアリルアルコール等のアルコール類;ポリエチレングリコール、ポリプロピレングリコール、ポリテトラメチレングリコール、及びこれら変性物からなるポリエーテル類;ジメチルポリシロキサン、シリコングリース等のポリシロキサン類;弗素系オイル、弗素系グリース、含弗素樹脂粉末といった弗素化合物;窒化珪素、炭化珪素、酸化マグネシウム、アルミナ、二酸化珪素、二硫化モリブデン等の無機化合物粉体が挙げられる。これらの滑剤は、一種単独でも二種以上組み合わせても良い。該滑剤の配合量は、磁石合金粉100重量部に対して、通常0.01〜20重量部、好ましくは0.1〜10重量部である。 Examples of the lubricant include waxes such as paraffin wax, liquid paraffin, polyethylene wax, polypropylene wax, ester wax, carnauba, and microwax; stearic acid, 1,2-oxystearic acid, lauric acid, palmitic acid, oleic acid, and the like Fatty acid salts such as calcium stearate, barium stearate, magnesium stearate, lithium stearate, zinc stearate, aluminum stearate, calcium laurate, zinc linoleate, calcium ricinoleate, zinc 2-ethylhexoate (metal soap) ); Stearic acid amide, oleic acid amide, erucic acid amide, behenic acid amide, palmitic acid amide, lauric acid amide, hydroxystearic acid amide, methylene bisste Fatty acid amides such as phosphoric acid amide, ethylene bis stearic acid amide, ethylene bis lauric acid amide, distearyl adipic acid amide, ethylene bis oleic acid amide, dioleyl adipic acid amide, N-stearyl stearic acid amide; butyl stearate, etc. Fatty acid esters; alcohols such as ethylene glycol and stearyl alcohol; polyethers composed of polyethylene glycol, polypropylene glycol, polytetramethylene glycol, and modified products thereof; polysiloxanes such as dimethylpolysiloxane and silicon grease; fluorine-based oils Fluorine compounds such as fluorine-based grease and fluorine-containing resin powders; inorganic compound powders such as silicon nitride, silicon carbide, magnesium oxide, alumina, silicon dioxide, molybdenum disulfideThese lubricants may be used alone or in combination of two or more. The blending amount of the lubricant is usually 0.01 to 20 parts by weight, preferably 0.1 to 10 parts by weight with respect to 100 parts by weight of the magnet alloy powder.
紫外線吸収剤としては、フェニルサリシレート等のベンゾフェノン系;2−(2’−ヒドロキシ−5’−メチルフェニル)ベンゾトリアゾール等のベンゾトリアゾール系;蓚酸アニリド誘導体などが挙げられる。 Examples of the ultraviolet absorber include benzophenone series such as phenyl salicylate; benzotriazole series such as 2- (2'-hydroxy-5'-methylphenyl) benzotriazole; oxalic acid anilide derivatives and the like.
また、安定剤としては、ビス(2、2、6、6−テトラメチル−4−ピペリジル)セバケート、ビス(1、2、2、6、6−ペンタメチル−4−ピペリジル)セバケート、1−[2−{3−(3,5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオニルオキシ}エチル]−4−{3−(3、5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオニルオキシ}−2、2、6、6−テトラメチルピペリジン、8−ベンジル−7、7、9、9−テトラメチル−3−オクチル−1、2、3−トリアザスピロ[4、5]ウンデカン−2、4−ジオン、4−ベンゾイルオキシ−2、2、6、6−テトラメチルピペリジン、こはく酸ジメチル−1−(2−ヒドロキシエチル)−4−ヒドロキシ−2、2、6、6−テトラメチルピペリジン重縮合物、ポリ[[6−(1、1、3、3−テトラメチルブチル)イミノ−1、3、5−トリアジン−2、4−ジイル][(2、2、6、6−テトラメチル−4−ピペリジル)イミノ]ヘキサメチレン[[2、2、6、6−テトラメチル−4−ピペリジル]イミノ]]、2−(3、5−ジ−第三ブチル−4−ヒドロキシベンジル)−2−n−ブチルマロン酸ビス(1、2、2、6、6−ペンタメチル−4−ピペリジル)等のヒンダード・アミン系安定剤のほか、フェノール系、ホスファイト系、チオエーテル系などの抗酸化剤等が挙げられる。これらの安定剤も、一種単独でも二種以上組み合わせても良い。該安定剤の配合量は、磁石合金粉100重量部に対して、通常0.01〜5重量部、好ましくは0.05〜3重量部である。 As stabilizers, bis (2,2,6,6-tetramethyl-4-piperidyl) sebacate, bis (1,2,2,6,6-pentamethyl-4-piperidyl) sebacate, 1- [2 -{3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionyloxy} ethyl] -4- {3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionyloxy} -2,2,6,6-tetramethylpiperidine, 8-benzyl-7,7,9,9-tetramethyl-3-octyl-1,2,3-triazaspiro [4,5] undecane-2, 4- Dione, 4-benzoyloxy-2,2,6,6-tetramethylpiperidine, succinic acid dimethyl-1- (2-hydroxyethyl) -4-hydroxy-2,2,6,6-tetramethylpiperidine polycondensate Poly [[6- (1,1,3,3-tetramethylbutyl) imino-1,3,5-triazine-2,4-diyl] [(2,2,6,6-tetramethyl-4-piperidyl ) Imino] hexamethylene [[2,2,6,6-tetramethyl-4-piperidyl] imino]], 2- (3,5-di-tert-butyl-4-hydroxybenzyl) -2-n-butyl In addition to hindered amine stabilizers such as bis (1,2,2,6,6-pentamethyl-4-piperidyl) malonate, antioxidants such as phenols, phosphites, and thioethers can be used. These stabilizers may be used alone or in combination of two or more. The amount of the stabilizer is usually 0.01 to 5 parts by weight, preferably 0.05 to 3 parts by weight with respect to 100 parts by weight of the magnet alloy powder.
混合方法は、特に限定されず、例えば、リボンブレンダー、タンブラー、ナウターミキサー、ヘンシェルミキサー、スーパーミキサー、プラネタリーミキサー等の混合機、或いはバンバリーミキサー、ニーダー、ロール、ニーダールーダー、単軸押出機、二軸押出機等の混練機が使用できる。 The mixing method is not particularly limited, for example, a blender such as a ribbon blender, tumbler, nauter mixer, Henschel mixer, super mixer, planetary mixer or the like, or a Banbury mixer, a kneader, a roll, a kneader ruder, a single screw extruder A kneader such as a twin screw extruder can be used.
次いで、上記のボンド磁石用組成物は、熱可塑性樹脂の場合、その溶融温度で加熱溶融された後、所望の形状を有する磁石に成形される。その際、成形法としては、従来からプラスチック成形加工等に利用されている射出成形法、押出成形法、射出圧縮成形法、射出プレス成形法、トランスファー成形法等の各種成形法が挙げられるが、これらの中では、特に射出成形法、押出成形法、射出圧縮成形法、及び射出プレス成形法が好ましい。 Next, in the case of a thermoplastic resin, the above-mentioned composition for bonded magnet is heated and melted at the melting temperature, and then formed into a magnet having a desired shape. At that time, examples of the molding method include various molding methods such as an injection molding method, an extrusion molding method, an injection compression molding method, an injection press molding method, and a transfer molding method that have been conventionally used for plastic molding and the like. Among these, an injection molding method, an extrusion molding method, an injection compression molding method, and an injection press molding method are particularly preferable.
熱硬化性樹脂は、混合時の剪断発熱等によって硬化が進まないよう、剪断力が弱く、かつ冷却機能を有する混合機を使用することが好ましい。混合により組成物が塊状化するので、これを射出成形法、圧縮成形法、押出成形法、圧延成形法、或いはトランスファー成形法等により成形する。 For the thermosetting resin, it is preferable to use a mixer having a low shearing force and a cooling function so that curing does not proceed due to shearing heat generated during mixing. Since the composition is agglomerated by mixing, it is molded by an injection molding method, compression molding method, extrusion molding method, rolling molding method, transfer molding method, or the like.
こうして得られたボンド磁石は、実用上重要な高温環境下で複合金属リン酸塩被膜に欠陥部が生じにくく、塩水の影響を受けることがない。従来は、サマリウム−鉄−窒素系合金磁石のような核発生型の保磁力発現機構を示す磁石合金粉末で、一部にでもこのような欠陥領域が生じると著しく保磁力が低下する問題があったが、本発明によれば、このような問題点が完全に克服される。 The bonded magnet thus obtained is less likely to cause a defect in the composite metal phosphate coating under a high temperature environment that is practically important, and is not affected by salt water. Conventionally, it is a magnet alloy powder showing a nucleation type coercive force generation mechanism such as a samarium-iron-nitrogen alloy magnet, and there is a problem that the coercive force is remarkably lowered when such a defective region occurs even in a part. However, according to the present invention, such a problem is completely overcome.
4.圧密磁石
本発明の耐塩水性磁石合金粉を用いて、圧密磁石を製造する方法は、特に限定されず、高い圧縮力がかけられ、見かけ密度を真密度の85%以上としうる方法であればよい。見かけ密度が85%未満では磁気特性が低く、また、磁石合金粉の劣化要因である酸素や水分の経路となるオープンポアによって耐塩水性が低下する。本発明の磁石合金粉は、そのままで高い耐塩水性を示すが、圧密磁石のオープンポアを無くすことによって、さらに高い耐塩水性を実現できる。
4). Consolidation Magnet The method for producing a consolidation magnet using the salt-resistant water-resistant magnet alloy powder of the present invention is not particularly limited as long as a high compressive force can be applied and the apparent density can be 85% or more of the true density. . When the apparent density is less than 85%, the magnetic properties are low, and the salt water resistance is lowered by open pores that are paths of oxygen and moisture, which are causes of deterioration of the magnet alloy powder. The magnet alloy powder of the present invention exhibits high salt water resistance as it is, but higher salt water resistance can be realized by eliminating the open pores of the compacted magnet.
なお、本発明のサマリウム−鉄−窒素系磁石合金粉から圧密磁石を製造する場合には、上記の耐塩水性以外に磁気特性、特に磁石の保磁力が改善される。圧密化するとき、サマリウム−鉄−窒素系化合物の分解や脱窒素を防止するとともに、粒子間に非磁性体のリン酸塩被膜が均一に存在するため保磁力の低下を防ぐことができる。 When a compacted magnet is produced from the samarium-iron-nitrogen based magnet alloy powder of the present invention, magnetic properties, particularly the coercive force of the magnet, are improved in addition to the salt water resistance. When consolidation is performed, decomposition and denitrification of the samarium-iron-nitrogen compound are prevented, and a decrease in coercive force can be prevented because a non-magnetic phosphate coating is uniformly present between the particles.
以下、実施例及び比較例を挙げて本発明を具体的に説明するが、本発明は、これら実施例によって何ら限定されるものではない。 EXAMPLES Hereinafter, although an Example and a comparative example are given and this invention is demonstrated concretely, this invention is not limited at all by these Examples.
(1)成分
磁石合金粉
・Sm−Fe−N系磁石合金粉[住友金属鉱山(株)製、平均粒径:30μm]
有機溶媒
・イソプロピルアルコール(IPA)[関東化学(株)製]
・N,N−ジメチルホルムアミド(DMF)[関東化学(株)製]
添加剤(被膜成分)
・酸化亜鉛[関東化学(株)製]
・リン酸亜鉛四水和物[関東化学(株)製]
・リン酸アルミニウム[関東化学(株)製]
・酸化マンガン[関東化学(株)製]
・酸化銅(I)[関東化学(株)製]
・酸化カルシウム[関東化学(株)製]
リン酸
・85%オルトリン酸水溶液[商品名:りん酸、関東化学(株)製]
(1) Ingredient
Magnet alloy powder / Sm—Fe—N magnet alloy powder [Sumitomo Metal Mining Co., Ltd., average particle size: 30 μm]
Organic solvent , isopropyl alcohol (IPA) [manufactured by Kanto Chemical Co., Inc.]
・ N, N-dimethylformamide (DMF) [manufactured by Kanto Chemical Co., Inc.]
Additive (coating component)
・ Zinc oxide [manufactured by Kanto Chemical Co., Ltd.]
・ Zinc phosphate tetrahydrate [Kanto Chemical Co., Ltd.]
・ Aluminum phosphate [Kanto Chemical Co., Ltd.]
・ Manganese oxide [Kanto Chemical Co., Ltd.]
・ Copper (I) [Kanto Chemical Co., Ltd.]
・ Calcium oxide [Kanto Chemical Co., Ltd.]
Phosphoric acid / 85% orthophosphoric acid aqueous solution [trade name: phosphoric acid, manufactured by Kanto Chemical Co., Inc.]
(2)被覆された磁石合金粉の特性、性能の測定、評価。
・被膜厚さ及び金属リン酸塩(b−2)被膜の複合リン酸塩被膜(B)に対する金属成分の比率
得られた磁石合金粉試料の断面をFE−TEM(電界放出型透過電子顕微鏡)で観察し、被膜厚さを測定した。また、被膜組成分析を、TEM−EDX(エネルギー分散型蛍光X線分析装置)で行い、金属リン酸塩(b−2)被膜の複合リン酸塩被膜(B)に対する金属成分の比率を求めた。
(2) Measurement and evaluation of characteristics and performance of the coated magnetic alloy powder.
-Ratio of metal component to composite phosphate coating (B) of film thickness and metal phosphate (b-2) coating FE-TEM (field emission transmission electron microscope) The film thickness was measured. Moreover, the coating composition analysis was performed with TEM-EDX (energy dispersive X-ray fluorescence analyzer), and the ratio of the metal component to the composite phosphate coating (B) of the metal phosphate (b-2) coating was determined. .
・耐塩水性
得られた磁石合金粉試料とナイロン12を、200℃のラボプラストミル中で30分混練し、空冷後、各組成物をプラスチック粉砕機により粉砕してそれぞれ成形用ペレットとした。得られたペレットを射出成形機にて7mm方向に560kA/mの配向磁界をかけながら、φ10mm×7mmの円柱状希土類系磁石を製造した。これを5%NaCl水溶液中に成形体の半分までつかるようにして浸漬後、室温にて24時間放置し、錆の発生の有無を目視観察した。
-Salt water resistance The obtained magnetic alloy powder sample and nylon 12 were kneaded in a lab plast mill at 200 ° C for 30 minutes, and after air cooling, each composition was pulverized with a plastic pulverizer to form pellets for molding. A cylindrical rare earth magnet having a diameter of 10 mm × 7 mm was manufactured while applying an orientation magnetic field of 560 kA / m in the 7 mm direction to the obtained pellets with an injection molding machine. This was immersed in a 5% NaCl aqueous solution so as to be half of the molded body, then left at room temperature for 24 hours, and the presence or absence of rust was visually observed.
・磁気特性評価
上記の円柱状希土類系磁石試料の磁気特性を、チオフィー型自記磁束計にて常温で測定した。磁気特性のうち残留磁化(Br)の結果を表1、表2に示す。
-Magnetic property evaluation The magnetic property of said cylindrical rare earth-type magnet sample was measured at normal temperature with the thiophye self-recording magnetometer. Tables 1 and 2 show the results of residual magnetization (Br) among the magnetic characteristics.
[実施例1〜7]
容器内部を窒素で置換したアトライタを用い、回転数200rpmで、還元磁石合金粉(Sm−Fe−N系)1kgを1.5kgの有機溶媒中で2時間粉砕し、平均粒径3μmの磁石合金粉を作製した。表1の記載に従って所定量の85%オルトリン酸水溶液、酸化物、リン酸塩などを合金粉に添加、攪拌した。その後、磁石合金粉を真空中150℃で4時間乾燥させた。得られた磁石合金粉の被膜厚さを測定し、金属リン酸塩(b−2)被膜の複合リン酸塩被膜(B)に対する金属成分の比率を求め、表1の結果を得た。次に、得られた磁石合金粉を用いて、磁粉体積率が60%となるように、12ナイロンを添加し、ラボプラストミルで混練後に、200℃にて射出成形してボンド磁石を作製した。得られた磁石試料の磁化を上記方法で測定し、表1の結果を得た。
[Examples 1-7]
Using an attritor substituted with nitrogen inside the container, 1 kg of reduced magnet alloy powder (Sm-Fe-N system) was pulverized in 1.5 kg of organic solvent for 2 hours at a rotation speed of 200 rpm, and a magnet alloy having an average particle diameter of 3 μm Powder was prepared. A predetermined amount of 85% orthophosphoric acid aqueous solution, oxide, phosphate and the like were added to the alloy powder and stirred according to the description in Table 1. Thereafter, the magnet alloy powder was dried in vacuum at 150 ° C. for 4 hours. The film thickness of the obtained magnet alloy powder was measured, the ratio of the metal component to the composite phosphate coating (B) of the metal phosphate (b-2) coating was determined, and the results in Table 1 were obtained. Next, using the obtained magnet alloy powder, 12 nylon was added so that the magnetic powder volume ratio was 60%, kneaded with a lab plast mill, and then injection molded at 200 ° C. to produce a bonded magnet. . The magnetization of the obtained magnet sample was measured by the above method, and the results shown in Table 1 were obtained.
[比較例1〜4]
添加剤を用いないか、添加剤やリン酸の量を変えて、上記の実施例と同様にして、磁石合金粉を処理した。結果を表1に示した。
[Comparative Examples 1-4]
The magnet alloy powder was treated in the same manner as in the above example, without using the additive or changing the amount of additive or phosphoric acid. The results are shown in Table 1.
[実施例8〜14]
実施例1〜7で用いた磁石合金粉10gを、窒素雰囲気下でアルミニウムカプセルに充填し、1600kA/mの配向磁界をかけながら50MPaで一軸加圧した。次に、この圧粉体をカプセルごと450℃、30min.、200MPaで等方性熱間圧縮法(HIP)で成形した。圧力媒体として窒素ガスを用いた。得られた磁石試料の磁化を測定し、表2の結果を得た。ここで見かけ密度は、真密度を7.67g/ccとした相対密度で表している。
[Examples 8 to 14]
10 g of the magnet alloy powder used in Examples 1 to 7 was filled in an aluminum capsule under a nitrogen atmosphere, and uniaxially pressed at 50 MPa while applying an orientation magnetic field of 1600 kA / m. Next, the green compact was encapsulated at 450 ° C. for 30 min. It was molded by an isotropic hot compression method (HIP) at 200 MPa. Nitrogen gas was used as the pressure medium. The magnetization of the obtained magnet sample was measured, and the results shown in Table 2 were obtained. Here, the apparent density is expressed as a relative density with a true density of 7.67 g / cc.
[比較例5〜8]
比較例1〜4で用いた磁石合金粉から、実施例8〜14に示した方法により等方性熱間圧縮法(HIP)で成形して圧密磁石を作製した。結果を表2に示した。
[Comparative Examples 5 to 8]
A compacted magnet was produced from the magnet alloy powder used in Comparative Examples 1 to 4 by an isotropic hot compression method (HIP) by the method shown in Examples 8 to 14. The results are shown in Table 2.
表1から、本発明の磁石合金粉を成形して得られたボンド磁石は、磁石合金粉の表面が適切な厚さの複合金属リン酸塩被膜によって均一に保護されているため、磁化が0.7T以上であり、かつ5%塩水中でも錆の発生がないことが分かる。また、表2から、本発明の磁石合金粉を見かけ密度85%以上に圧密化して得られた圧密磁石は、磁石合金粉の表面が適切な厚さの複合金属リン酸塩被膜によって均一に保護されているため、磁化が1.2T以上と十分高く、5%塩水中でも錆が見られないことが分かる。これに対して、比較例のボンド磁石、圧密磁石は、金属リン酸塩被膜が複合化されていないか、被膜の厚さが適切ではないので、磁化、保磁力が小さいか、錆が発生することが分かる。 From Table 1, since the bonded magnet obtained by molding the magnet alloy powder of the present invention is uniformly protected by the composite metal phosphate coating of the appropriate thickness on the surface of the magnet alloy powder, the magnetization is 0. It can be seen that rust is not generated even in 5% salt water. Also, from Table 2, the compacted magnet obtained by compacting the magnet alloy powder of the present invention to an apparent density of 85% or more is uniformly protected by a composite metal phosphate coating with an appropriate thickness on the surface of the magnet alloy powder. Therefore, it can be seen that the magnetization is sufficiently high as 1.2 T or more, and no rust is seen even in 5% salt water. On the other hand, the bonded magnet and the compacted magnet of the comparative example are not combined with the metal phosphate coating, or the thickness of the coating is not appropriate, so the magnetization and coercive force are small or rust is generated. I understand that.
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