JP2003234228A - Rare-earth bonded magnet and its manufacturing method - Google Patents
Rare-earth bonded magnet and its manufacturing methodInfo
- Publication number
- JP2003234228A JP2003234228A JP2002030640A JP2002030640A JP2003234228A JP 2003234228 A JP2003234228 A JP 2003234228A JP 2002030640 A JP2002030640 A JP 2002030640A JP 2002030640 A JP2002030640 A JP 2002030640A JP 2003234228 A JP2003234228 A JP 2003234228A
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- magnet
- bonded magnet
- rare earth
- earth bonded
- rare
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、耐酸化性を改善し
た希土類ボンド磁石およびその製造方法に関するもので
ある。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a rare earth bonded magnet having improved oxidation resistance and a method for manufacturing the same.
【０００２】[0002]
【従来の技術】近年の電化製品の発展に伴い、軽量、小
型化が可能な高性能磁石として希土類ボンド磁石の需要
は増大し、更なる性能の向上が求められている。高特性
を有する希土類磁石の代表としては、Ｎｄ−Ｆｅ−Ｂ系
磁石がある。しかし、この磁石合金は組織中に極めて酸
化しやすいＮｄ−Ｆｅ合金相を含み、さらにＮｄ２Ｆｅ
１４Ｂ相も酸化しやすいため、Ｓｍ−Ｃｏ系磁石に比較
して磁石の酸化による磁気特性の劣化やばらつきが大き
い。さらに、磁気回路等の装置に組み込んだ場合、磁石
から発生した酸化物の飛散による周辺部品への汚染を引
き起こすおそれがある。2. Description of the Related Art With the recent development of electric appliances, light weight and small size
Demand for rare earth bonded magnets as high-performance magnets that can be modeled
Is increasing, and further improvement in performance is required. High characteristic
A typical rare earth magnet having Nd is a Nd-Fe-B system.
There is a magnet. However, this magnet alloy is extremely acidic in the tissue.
Contains an Nd-Fe alloy phase that easily forms, and further NdTwoFe
14Compared to Sm-Co magnets, B phase is also easily oxidized.
As a result, there is a great deal of deterioration and variation in magnetic characteristics due to oxidation of the magnet.
Yes. Furthermore, when incorporated in a device such as a magnetic circuit, a magnet
The pollution of surrounding parts due to the scattering of oxides generated from
There is a risk of causing it.
【０００３】[0003]
【発明が解決しようとする課題】この問題を解決する方
法として、特開昭６０−５４４０６号公報や特開昭６０
−６３９０３号公報が提案されている。しかしながら、
これらの公報に提案されている耐酸化性被膜は、被膜形
成工程中で多量の水を使用するため、処理工程中で磁石
材料が酸化したり、処理後であっても微量の水分の残留
が原因となって酸化する場合が多く、耐酸化性が十分と
は言い難い。As a method for solving this problem, JP-A-60-54406 and JP-A-60-54406 are available.
No. 63903 has been proposed. However,
The oxidation-resistant coatings proposed in these publications use a large amount of water in the coating forming step, so that the magnet material is oxidized in the treatment step and a trace amount of water remains even after the treatment. In many cases, it is oxidized as a cause, and it cannot be said that the oxidation resistance is sufficient.
【０００４】また、金属の防錆表面処理の一般的方法で
ある塗装法では、塗料の基材が有機高分子であるため金
属との親和性が不十分で、磁石の部品化工程や使用時に
おいて亀裂や剥離を生じやすいこと、また特に反応硬化
型の塗料の場合は痕跡程度の未反応の官能基の経時変化
が発錆の原因となることもあり、特に、このような合金
系では、信頼性が不十分で、用途が限定されているのが
現状である。In addition, in the coating method which is a general method of rust preventive surface treatment of metal, since the base material of the coating material is an organic polymer, the affinity with the metal is insufficient, and the magnet is used in the process of forming parts or during use. In the case of easily cracking and peeling in, and in the case of a reaction-curing type coating, aging may cause aging due to changes in unreacted functional groups of traces, in particular, in such an alloy system, At present, the reliability is insufficient and the applications are limited.
【０００５】さらに、スパッター、イオン蒸着法を用い
た金属被膜形成による酸化防止法は、磁石全体への均一
コーティングが困難であること、また被覆層組織が下地
面に垂直方向に方向性を持つため、被覆層に微細な間隙
を生じ、十分な耐食性が期待できない等の問題がある。Further, in the oxidation prevention method by forming a metal coating film using sputtering or ion vapor deposition, it is difficult to uniformly coat the entire magnet, and the coating layer structure has a directionality in the direction perpendicular to the base surface. However, there is a problem that a fine gap is generated in the coating layer and sufficient corrosion resistance cannot be expected.
【０００６】そこで、本発明の技術的課題は、上記欠点
に鑑み、より耐食性に優れた希土類ボンド磁石およびそ
の製造方法を提供することにある。Therefore, in view of the above-mentioned drawbacks, a technical object of the present invention is to provide a rare earth bonded magnet having more excellent corrosion resistance and a method for producing the same.
【０００７】[0007]
【課題を解決するための手段】本発明は、希土類合金の
粉末を樹脂と混練成形してなる希土類ボンド磁石表面
に、化２で表される少なくとも１種のメルカプト基を含
むトリアジン系化合物（但し、Ｍ１およびＭ２はＨ、ア
ルカリ金属またはアルカリ土類金属／２、ＲはＮＨ
Ｒ１、ＮＲ１Ｒ２またはＳＨ、Ｒ１およびＲ２はＨ、ア
ルキル基またはフェニル基）からなる被膜と、該被膜の
上に耐酸化めっき層を有することを特徴とする希土類ボ
ンド磁石である。According to the present invention, a triazine-based compound containing at least one mercapto group represented by Chemical formula 2 is provided on the surface of a rare earth bonded magnet obtained by kneading and molding a powder of a rare earth alloy with a resin. , M 1 and M 2 are H, alkali metal or alkaline earth metal / 2, R is NH
R 1 , NR 1 R 2 or SH, R 1 and R 2 are H, an alkyl group or a phenyl group), and a rare earth bonded magnet characterized by having an oxidation resistant plating layer on the coating. .
【０００８】[0008]
【化２】 [Chemical 2]
【０００９】また、本発明は、前記トリアジン系化合物
の溶液中で電解処理することにより前記磁石表面に被膜
を形成することを特徴とする上記の希土類ボンド磁石の
製造方法である。The present invention is also the above-mentioned method for producing a rare earth bonded magnet, characterized in that a coating film is formed on the surface of the magnet by electrolytically treating it in a solution of the triazine compound.
【００１０】[0010]
【発明の実施の形態】本発明は、希土類ボンド磁石表面
に生成する酸化物を抑制するため、この表面にメルカプ
ト基を含むトリアジン系化合物（以下、トリアジン系化
合物と称する）からなる強固かつ安定な耐酸化性被膜を
設けた後、耐酸化めっき層を積層形成するものである。BEST MODE FOR CARRYING OUT THE INVENTION The present invention suppresses oxides formed on the surface of a rare earth bonded magnet, so that a strong and stable triazine compound containing a mercapto group on the surface (hereinafter referred to as a triazine compound) is used. After providing the oxidation resistant coating, the oxidation resistant plating layer is laminated.
【００１１】この耐酸化性被膜の被覆方法としては、ト
リアジン系化合物の有機溶媒液を電解液として用い、磁
石を陽極にして、液温０〜８０℃、電圧２０Ｖ以下、電
流密度１０ｍＡ／ｄｍ２〜１０Ａ／ｄｍ２で０.１秒〜
１０分間、電解する。As a method for coating the oxidation resistant coating, an organic solvent solution of a triazine compound is used as an electrolytic solution, a magnet is used as an anode, a liquid temperature is 0 to 80 ° C., a voltage is 20 V or less, and a current density is 10 mA / dm 2. 10 seconds at 0.1 A / dm 2
Electrolyze for 10 minutes.
【００１２】上記電解液中では、トリアジン環がマイナ
スイオンに解離するので、メルカプト基を２個含むトリ
アジン系化合物を電解した場合、陽極の金属表面にトリ
アジンジチオール化合物が電着して被膜を形成する。In the above-mentioned electrolytic solution, the triazine ring dissociates into negative ions, so when a triazine compound containing two mercapto groups is electrolyzed, the triazinedithiol compound is electrodeposited on the metal surface of the anode to form a film. .
【００１３】トリアジン系化合物より磁石表面に生成さ
れた膜は、従来の化成被膜等と比べ、きわめて耐食性、
耐久性に優れ、金属表面との結合力が強い。さらに、撥
水性および潤滑性が付与されるので着水、着氷などを防
止できる。The film formed from the triazine-based compound on the surface of the magnet has extremely high corrosion resistance as compared with conventional chemical conversion coatings.
It has excellent durability and has a strong bond with the metal surface. Furthermore, since water repellency and lubricity are imparted, it is possible to prevent water landing, ice landing and the like.
【００１４】トリアジン系化合物としては、次の化３で
示される化合物である。The triazine-based compound is a compound represented by the following chemical formula 3.
【化３】 [Chemical 3]
【００１５】またバインダーとする樹脂としては、ポリ
エチレン、ポリプロピレンなどのオレフィン系樹脂、ナ
イロン６、ナイロン１２などのポリアミド樹脂、ポリエ
チレンテレフタレート、ポリブチレンテレフタレート、
などのポリエステル樹脂、エチレン−酢酸ビニル共重合
体、エチレン−エチルアクリレート共重合体、ポリフェ
ニレンサルファイド、及びこれらの変性タイプの樹脂が
用いられる。As the binder resin, olefin resins such as polyethylene and polypropylene, polyamide resins such as nylon 6 and nylon 12, polyethylene terephthalate, polybutylene terephthalate,
For example, polyester resins such as ethylene-vinyl acetate copolymer, ethylene-ethyl acrylate copolymer, polyphenylene sulfide, and modified types of these resins are used.
【００１６】電解液は、トリアジン系化合物を有機溶剤
に溶解させることにより調製できる。有機溶剤として
は、０〜８０℃の温度範囲で低粘度であれば、ほとんど
のものを使用できる。例えば、メチルアルコール、エチ
ルアルコール、イソプロピルアルコール、エチルセロソ
ルブのようなアルコール、アセトン、メチルエチルケト
ンのようなケトン、ジメチルホルムアミドのようなアミ
ド、酢酸エチルエステルのようなエーテル、テトラヒド
ロフランのようなフラン、ベンゼン、トルエンのような
芳香族炭化水素などが使用できる。濃度はトリアジンジ
チオール化合物が１×１０−１〜１×１０−６モル／
ｌ、好ましくは５×１０−２〜５×１０−４モル／ｌに
なるようにする。The electrolytic solution can be prepared by dissolving a triazine compound in an organic solvent. As the organic solvent, almost any organic solvent can be used as long as it has a low viscosity in the temperature range of 0 to 80 ° C. For example, alcohols such as methyl alcohol, ethyl alcohol, isopropyl alcohol, ethyl cellosolve, acetone, ketones such as methyl ethyl ketone, amides such as dimethylformamide, ethers such as ethyl acetate, furan such as tetrahydrofuran, benzene, toluene. Aromatic hydrocarbons such as can be used. The concentration of the triazinedithiol compound is 1 × 10 −1 to 1 × 10 −6 mol /
1, preferably 5 × 10 −2 to 5 × 10 −4 mol / l.
【００１７】陰極には、陰極からの溶出物が被膜中に混
入するのを避けるため不溶性材料を使用する。このよう
な材料としては、例えば、白金、チタン、ステンレス
鋼、カーボン、グラファイトなどがある。電解は、液温
０〜８０℃に調整して、電圧２０Ｖ以下、電流密度１０
ｍＡ／ｄｍ２〜１０Ａ／ｄｍ２で０.１秒〜１０分間行
う。液温を０℃より低くすると、被膜を形成するために
長時間を要し、８０℃より高くすると、被膜の厚さをコ
ントロールするのが困難となり、また、電圧を２０Ｖよ
り高くすると、被膜が金属表面にむらとなって形成す
る。さらに、電流密度は１０ｍＡ／ｄｍ２より小さくす
ると、被膜は形成されず、１０Ａ／ｄｍ２より大きくす
ると、被膜がむらとなって形成する。また、電解時間は
０.１秒未満であると、電流密度を１０Ａ／ｄｍ２にし
ても、金属表面全体に被膜を形成できず、１０分を越え
ると、被膜が絶縁体になり、電解が困難になる。For the cathode, an insoluble material is used in order to prevent the eluate from the cathode from being mixed in the coating film. Examples of such a material include platinum, titanium, stainless steel, carbon and graphite. The electrolysis is adjusted to a liquid temperature of 0 to 80 ° C., a voltage of 20 V or less, and a current density of 10
It is carried out for 0.1 second to 10 minutes at mA / dm 2 to 10 A / dm 2 . When the liquid temperature is lower than 0 ° C, it takes a long time to form a coating film, and when the liquid temperature is higher than 80 ° C, it becomes difficult to control the thickness of the coating film. It forms unevenly on the metal surface. Further, when the current density is less than 10 mA / dm 2 , the coating film is not formed, and when it is more than 10 A / dm 2 , the coating film becomes uneven. If the electrolysis time is less than 0.1 second, a coating cannot be formed on the entire metal surface even if the current density is 10 A / dm 2 , and if it exceeds 10 minutes, the coating becomes an insulator and electrolysis It will be difficult.
【００１８】この耐酸化性被膜の表面に積層する耐酸化
めっき層としては、Ｎｉ、Ｃｕ、Ｚｎ等の耐酸化性を有
する金属または合金のめっき、あるいはこれらの複合め
っきであればよく、めっき処理方法としては、無電解め
っきまたは電解めっき、あるいは前記めっきの併用によ
る方法でもよい。The oxidation resistant plating layer laminated on the surface of the oxidation resistant coating may be a plating of a metal or an alloy having oxidation resistance such as Ni, Cu, Zn, or a composite plating thereof, and a plating treatment As a method, electroless plating or electrolytic plating, or a method using a combination of the above platings may be used.
【００１９】また、めっき層の厚みは、２５μｍを越え
る厚みでは、めっき膜の強度が劣化するとともに、製品
の寸法精度を得ることが困難になり、かつ、めっき処理
時間に長時間を要し、コスト的にも好ましくないため、
めっき層厚みは２５μｍ以下が好ましい。When the thickness of the plating layer exceeds 25 μm, the strength of the plating film deteriorates, it becomes difficult to obtain the dimensional accuracy of the product, and it takes a long time for the plating treatment. Because it is not preferable in terms of cost,
The thickness of the plating layer is preferably 25 μm or less.
【００２０】[0020]
【実施例】以下に、本発明について実施例を挙げ、説明
する。EXAMPLES The present invention will be described below with reference to examples.
【００２１】（実施例１）希土類合金粉末として、Ｎｄ
３１ｗｔ％−Ｂ１.１ｗｔ％−残部Ｆｅの組成の粉末を
用意した。この粉末にナイロン１２を混合し、プレス機
により圧縮成形を行い、１０ｍｍ×１０ｍｍ×１０ｍｍ
の寸法のボンド磁石を作製した。Example 1 Nd was used as rare earth alloy powder.
A powder having a composition of 31 wt% -B1.1 wt% -the balance of Fe was prepared. Nylon 12 is mixed with this powder, and compression molding is performed by a press machine to obtain 10 mm x 10 mm x 10 mm.
A bonded magnet having the dimensions of was prepared.
【００２２】次に、２−ジブチルアミノ−４，６−ジチ
オール−Ｓ−トリアジンおよびＬｉＣｌＯ４（支持電解
質）の濃度が、それぞれ５×１０−２モル／ｌおよび５
×１０−４モル／ｌであるエチルアルコール電解液を調
製した。この電解液を用いて、アセトンで洗浄した上記
のＮｄ−Ｆｅ−Ｂボンド磁石試料片を陽極、ステンレス
鋼板（ＳＵＳ３０４）を陰極にして、液温２５〜３０℃
にて電流密度１.０〜２.０Ａ／ｄｍ２で１０〜２４０秒
間電解し、耐酸化性被膜を形成した。Next, the concentrations of 2-dibutylamino-4,6-dithiol-S-triazine and LiClO 4 (supporting electrolyte) were 5 × 10 −2 mol / l and 5 respectively.
An ethyl alcohol electrolyte solution having a concentration of × 10 -4 mol / l was prepared. Using this electrolytic solution, the acetone-washed Nd-Fe-B bonded magnet sample piece was used as an anode and a stainless steel plate (SUS304) was used as a cathode, and the liquid temperature was 25 to 30 ° C.
At a current density of 1.0 to 2.0 A / dm 2 for 10 to 240 seconds to form an oxidation resistant film.
【００２３】その後、この試料片に対し、めっき浴にワ
ット浴（液温度５０℃）を用い、電流密度２.０Ａ／ｄ
ｍ２で４８０秒間処理し、厚さ１０μｍのＮｉめっき層
を形成した。Thereafter, a Watt bath (liquid temperature 50 ° C.) was used as a plating bath for this sample piece, and the current density was 2.0 A / d.
It was treated with m 2 for 480 seconds to form a Ni plating layer having a thickness of 10 μm.
【００２４】また、別の試料片に対しては、めっき浴に
青化浴（液温度室温）を用い、電流密度１.０Ａ／ｄｍ
２で６００秒間処理し、厚さ６μｍのＣｕめっき層を形
成した。For another sample piece, a bluing bath (liquid temperature room temperature) was used as the plating bath, and the current density was 1.0 A / dm.
The treatment was performed at 2 for 600 seconds to form a Cu plating layer having a thickness of 6 μm.
【００２５】（実施例２）実施例１と同様に調製した試
験片を用い、電解液として２−オレイルアミノ−４，６
−ジメルカプト−Ｓ−トリアジンモノナトリウムの濃度
が５×１０−４モル／ｌ、ＬｉＣｌＯ４支持電解質の代
わりに用いたＬｉＢＦ４の濃度が５×１０ −４モル／ｌ
のものを用い、実施例１と同様の条件で電解し、耐酸化
性被膜を得た。Example 2 A test prepared in the same manner as in Example 1.
Using a test piece, 2-oleylamino-4,6 as an electrolytic solution
-Concentration of dimercapto-S-triazine monosodium
Is 5 × 10-4Mol / l, LiClOFourCost of supporting electrolyte
LiBF used insteadFourConcentration of 5 × 10 -4Mol / l
Electrolyzed under the same conditions as in Example 1, using
A protective coating was obtained.
【００２６】その後、この試料片に対し、めっき浴にワ
ット浴（液温度５０℃）を用い、電流密度２.０Ａ／ｄ
ｍ２で４８０秒間処理し、厚さ１０μｍのＮｉめっき層
を形成した。Thereafter, a Watt bath (solution temperature 50 ° C.) was used as the plating bath for this sample piece, and the current density was 2.0 A / d.
It was treated with m 2 for 480 seconds to form a Ni plating layer having a thickness of 10 μm.
【００２７】また、別の試料片に対しては、めっき浴に
青化浴（液温度３０℃）を用い、電流密度３.０Ａ／ｄ
ｍ２で４８０秒間処理し、厚さ１２μｍのＺｎめっき層
を形成した。For another sample piece, a bluing bath (solution temperature 30 ° C.) was used as the plating bath, and the current density was 3.0 A / d.
It was treated with m 2 for 480 seconds to form a Zn plating layer having a thickness of 12 μm.
【００２８】以上のようにして得られた試験片、および
比較のための無処理試験片の７２時間５％食塩水噴霧試
験結果およびゴバン目試験の結果を表１に示す。Table 1 shows the results of the 72-hour 5% saline spray test and the goose eye test of the test pieces thus obtained and untreated test pieces for comparison.
【００２９】[0029]
【表１】 [Table 1]
【００３０】表１より、実施例１、実施例２とも食塩水
噴霧試験結果およびゴバン目試験において、良好な結果
が得られていることがわかる。It can be seen from Table 1 that good results were obtained in both the salt spray test results and the goose eye test in both Example 1 and Example 2.
【００３１】[0031]
【発明の効果】以上述べたように、本発明による希土類
ボンド磁石は、表面に順次積層形成された耐酸化性被
膜、および耐酸化めっき層を有するため、耐食性、耐久
性に優れ、特性の安定化および信頼性の向上にきわめて
有効である。As described above, since the rare earth bonded magnet according to the present invention has the oxidation resistant coating and the oxidation resistant plating layer, which are sequentially laminated on the surface, it has excellent corrosion resistance, durability and stable characteristics. It is extremely effective in improving reliability and reliability.
Claims (2)
なる希土類ボンド磁石表面に、化１で表される少なくと
も１種のメルカプト基を含むトリアジン系化合物（但
し、Ｍ１およびＭ２はＨ、アルカリ金属またはアルカリ
土類金属／２、ＲはＮＨＲ１、ＮＲ１Ｒ２またはＳＨ、
Ｒ１およびＲ２はＨ、アルキル基またはフェニル基）か
らなる被膜と、該被膜の上に耐酸化めっき層を有するこ
とを特徴とする希土類ボンド磁石。 【化１】 1. A triazine-based compound containing at least one mercapto group represented by Chemical formula 1 on the surface of a rare earth bonded magnet formed by kneading and molding a rare earth alloy powder with a resin (wherein M 1 and M 2 are H , Alkali metal or alkaline earth metal / 2, R is NHR 1 , NR 1 R 2 or SH,
R 1 and R 2 are coatings made of H, an alkyl group or a phenyl group), and an oxidation resistant plating layer on the coating, a rare earth bonded magnet. [Chemical 1]
処理することにより前記磁石表面に被膜を形成すること
を特徴とする請求項１記載の希土類ボンド磁石の製造方
法。2. The method for producing a rare earth bonded magnet according to claim 1, wherein a coating film is formed on the surface of the magnet by performing an electrolytic treatment in a solution of the triazine-based compound.
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