JPH059784A - Method for baking ni-plated rare earth alloy - Google Patents
Method for baking ni-plated rare earth alloyInfo
- Publication number
- JPH059784A JPH059784A JP19342891A JP19342891A JPH059784A JP H059784 A JPH059784 A JP H059784A JP 19342891 A JP19342891 A JP 19342891A JP 19342891 A JP19342891 A JP 19342891A JP H059784 A JPH059784 A JP H059784A
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- earth alloy
- atmosphere
- heat treatment
- plating film
- 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.)
- Withdrawn
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 50
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 46
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 44
- 239000000956 alloy Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000007747 plating Methods 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 238000009713 electroplating Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 6
- 239000011261 inert gas Substances 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 28
- 239000001257 hydrogen Substances 0.000 description 21
- 229910052739 hydrogen Inorganic materials 0.000 description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 239000000203 mixture Substances 0.000 description 6
- 229910001172 neodymium magnet Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000010791 quenching Methods 0.000 description 4
- 230000000171 quenching effect Effects 0.000 description 4
- 229910052772 Samarium Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 229910052735 hafnium Inorganic materials 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- ULSLJYXHZDTLQK-UHFFFAOYSA-N Coumatetralyl Chemical compound C1=CC=CC2=C1OC(=O)C(C1C3=CC=CC=C3CCC1)=C2O ULSLJYXHZDTLQK-UHFFFAOYSA-N 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- DLDJFQGPPSQZKI-UHFFFAOYSA-N but-2-yne-1,4-diol Chemical compound OCC#CCO DLDJFQGPPSQZKI-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、希土類合金表面にＮｉ
めっき膜を形成した後に施す熱処理方法に関する。BACKGROUND OF THE INVENTION The present invention relates to a rare earth alloy surface with Ni.
The present invention relates to a heat treatment method performed after forming a plated film.
【０００２】[0002]
【従来の技術】高性能を有する永久磁石としては、粉末
冶金法によるＳｍ−Ｃｏ系磁石が知られている。しか
し、このものは、Ｓｍ、Ｃｏの原料価格が高いという欠
点を有する。希土類の中では原子量の小さい希土類元
素、たとえばセリウムやプラセオジム、ネオジムは、サ
マリウムよりも豊富にあり価格が安い。また、Ｆｅは安
価である。そこで、近年Ｎｄ−Ｆｅ−Ｂ系磁石が開発さ
れ、特開昭５９−４６００８号公報では、焼結磁石が、
また特開昭６０−９８５２号公報では、高速急冷法によ
るものが開示されている。2. Description of the Related Art As a permanent magnet having high performance, an Sm-Co type magnet produced by powder metallurgy is known. However, this material has a drawback that the raw material prices of Sm and Co are high. Among rare earth elements, rare earth elements with a small atomic weight, such as cerium, praseodymium, and neodymium, are more abundant and cheaper than samarium. Further, Fe is inexpensive. Therefore, in recent years, Nd-Fe-B system magnets have been developed, and in JP-A-59-46008, a sintered magnet is
Further, Japanese Patent Application Laid-Open No. Sho 60-9852 discloses a method using a rapid quenching method.
【０００３】Ｎｄ−Ｆｅ−Ｂ系磁石は、酸化され易い希
土類元素と鉄とを主成分とするため、耐食性が低く、性
能の劣化、バラつき等が問題となっている。このため、
各種の防食膜が提案ないし実用化されているが、これら
のうち、電気めっき法によるＮｉめっき膜、特に半光沢
Ｎｉめっき膜は、耐食性が良好で量産性にも優れ、しか
も機械的強度の点においても補強効果を発揮するため有
用である。Since the Nd-Fe-B system magnets contain a rare earth element which is easily oxidized and iron as the main components, they have low corrosion resistance and have problems such as deterioration of performance and variation. For this reason,
Various anticorrosion films have been proposed or put into practical use. Among them, the Ni plating film by electroplating method, especially the semi-bright Ni plating film, has good corrosion resistance and excellent mass productivity, and has a mechanical strength. Also, it is useful because it exerts a reinforcing effect.
【０００４】しかし、Ｎｉが水素より卑であるために、
電気めっき法によりＮｉめっき膜を形成する際や、めっ
きの前処理である酸洗工程などにおいて微量の水素が発
生する。Ｎｄ−Ｆｅ−Ｂ系磁石は、水素吸蔵による粉砕
が行なわれているように水素を極めて吸蔵しやすいた
め、発生した水素が磁石に吸蔵されて水素脆化を生じ
る。そして、脆化により磁石表面付近に剥離が発生する
ため、Ｎｉめっき膜にフクレが発生して不良品が生じや
すい。However, since Ni is baser than hydrogen,
A small amount of hydrogen is generated when the Ni plating film is formed by the electroplating method or in the pickling step which is a pretreatment of plating. Since Nd-Fe-B magnets are extremely apt to absorb hydrogen as pulverized by hydrogen absorption, the generated hydrogen is occluded by the magnet and hydrogen embrittlement occurs. Then, the embrittlement causes peeling in the vicinity of the surface of the magnet, so that blisters are generated in the Ni plating film and defective products are likely to occur.
【０００５】なお、このような事情は、水素を吸蔵しや
すい他の希土類合金にＮｉ電気めっき膜を形成した場合
に関しても同様である。Incidentally, such a circumstance also applies to the case where a Ni electroplating film is formed on another rare earth alloy which easily absorbs hydrogen.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、表面にＮｉ
めっき膜を形成した希土類合金において、Ｎｉめっき膜
のフクレを防止することを目的とする。DISCLOSURE OF INVENTION Problems to be Solved by the Invention The present invention is based on
The purpose of the present invention is to prevent blistering of a Ni plating film in a rare earth alloy having a plating film formed thereon.
【０００７】[0007]
【課題を解決するため 手段】このような目的は、下記
（１）〜（５）の本発明により達成される。
（１）電気めっき法により形成されたＮｉめっき膜を表
面に有する希土類合金を、水蒸気含有量が１体積％以下
である雰囲気中において、１００〜２００℃にて熱処理
することを特徴とするＮｉめっき希土類合金のベーキン
グ方法。Such objects are achieved by the present invention described in (1) to (5) below. (1) Ni plating characterized in that a rare earth alloy having a Ni plating film formed by an electroplating method on its surface is heat-treated at 100 to 200 ° C. in an atmosphere having a water vapor content of 1% by volume or less. Baking method for rare earth alloys.
【０００８】（２）前記熱処理を前記雰囲気の気流中に
おいて行なう上記（１）に記載のＮｉめっき希土類合金
のベーキング方法。(2) The method for baking a Ni-plated rare earth alloy as described in (1) above, wherein the heat treatment is carried out in an air stream of the atmosphere.
【０００９】（３）前記熱処理を０．１〜２４時間行な
う上記（１）または（２）に記載のＮｉめっき希土類合
金のベーキング方法。(3) The method for baking a Ni-plated rare earth alloy as described in (1) or (2) above, wherein the heat treatment is performed for 0.1 to 24 hours.
【００１０】（４）前記雰囲気が、Ｎ2 ガスまたはＡｒ
ガスである上記（１）ないし（３）のいずれかに記載の
Ｎｉめっき希土類合金のベーキング方法。(4) The atmosphere is N 2 gas or Ar
The method for baking a Ni-plated rare earth alloy as described in any of (1) to (3) above, which is a gas.
【００１１】（５）前記希土類合金が、Ｎｄ、Ｆｅおよ
びＢを含有する永久磁石である上記（１）ないし（４）
のいずれかに記載のＮｉめっき希土類合金のベーキング
方法。(5) The rare earth alloy is a permanent magnet containing Nd, Fe and B. (1) to (4)
The method for baking a Ni-plated rare earth alloy according to any one of 1.
【００１２】[0012]
【作用】本発明では、Ｎｉめっき膜を形成した希土類合
金を、水蒸気含有量が所定値以下である雰囲気中で熱処
理する。Ｎｉめっき膜形成時に希土類合金に吸蔵された
水素は、前記熱処理により合金から放出され、Ｎｉめっ
き膜を通過して雰囲気中に放出される。また、熱処理雰
囲気中に水蒸気が存在すると、この水蒸気がＮｉめっき
膜を通して希土類合金表面に達し、ここで還元されて水
素が発生してしまうが、本発明では熱処理雰囲気中の水
蒸気含有量を上記のように極めて少なく抑えるため、希
土類合金表面での水蒸気還元が防止され、熱処理により
再び水素を吸蔵することが避けられる。このため、本発
明によれば希土類合金の水素脆化が効果的に防止され、
Ｎｉめっき膜のフクレ発生が防止される。In the present invention, the rare earth alloy having the Ni plating film formed thereon is heat-treated in an atmosphere having a water vapor content of not more than a predetermined value. The hydrogen stored in the rare earth alloy at the time of forming the Ni plating film is released from the alloy by the heat treatment, passes through the Ni plating film, and is released into the atmosphere. Further, when water vapor is present in the heat treatment atmosphere, this water vapor reaches the surface of the rare earth alloy through the Ni plating film and is reduced there to generate hydrogen, but in the present invention, the water vapor content in the heat treatment atmosphere is Since it is suppressed to such an extremely low level, steam reduction on the surface of the rare earth alloy is prevented, and it is possible to avoid occluding hydrogen again by heat treatment. Therefore, according to the present invention, hydrogen embrittlement of the rare earth alloy is effectively prevented,
Generation of blisters on the Ni plating film is prevented.
【００１３】なお、従来、鉄鋼材料等においては、めっ
き膜形成後に水素除去のための熱処理を施すことは知ら
れているが、希土類合金からの水素除去に特に適した熱
処理方法は提案されていない。It has been known that a steel material or the like is subjected to a heat treatment for removing hydrogen after forming a plating film, but no heat treatment method particularly suitable for removing hydrogen from a rare earth alloy has been proposed. .
【００１４】[0014]
【具体的構成】以下、本発明の具体的構成について詳細
に説明する。本発明では、希土類合金の表面に電気めっ
き法によりＮｉめっき膜を形成した後、水蒸気含有量が
１体積％以下、好ましくは０．１体積％以下である雰囲
気中において前記希土類合金に熱処理を施す。熱処理雰
囲気中の水蒸気含有量が前記範囲を超えると、熱処理に
より希土類合金が逆に脆化してしまう。Specific Structure The specific structure of the present invention will be described in detail below. In the present invention, after the Ni plating film is formed on the surface of the rare earth alloy by the electroplating method, the rare earth alloy is heat-treated in an atmosphere having a water vapor content of 1% by volume or less, preferably 0.1% by volume or less. . When the water vapor content in the heat treatment atmosphere exceeds the above range, the heat treatment causes the rare earth alloy to become brittle.
【００１５】熱処理時の雰囲気は、水蒸気含有量以外に
特に制限はなく、雰囲気中にＯ2 ガスが含まれていても
構わないが、好ましくは不活性ガス雰囲気とする。用い
る不活性ガスに特に制限はないが、例えば、Ａｒガスや
Ｎ2 ガスを好ましく用いることができる。The atmosphere during the heat treatment is not particularly limited other than the water vapor content, and O 2 gas may be contained in the atmosphere, but an inert gas atmosphere is preferred. The inert gas used is not particularly limited, but for example, Ar gas or N 2 gas can be preferably used.
【００１６】熱処理温度は、１００〜２００℃、好まし
くは１００〜１５０℃とする。熱処理温度が前記範囲未
満であると、希土類合金に吸蔵された水素の放出が不十
分となる。また、Ｎｉめっき膜と希土類合金とは熱膨張
率が異なるため、前記範囲を超える温度で熱処理を行な
うと、Ｎｉめっき膜と希土類合金表面との密着性が低下
し、めっき膜が剥離することがある。The heat treatment temperature is 100 to 200 ° C., preferably 100 to 150 ° C. If the heat treatment temperature is lower than the above range, the hydrogen stored in the rare earth alloy will be insufficiently released. Further, since the Ni plating film and the rare earth alloy have different coefficients of thermal expansion, if heat treatment is performed at a temperature exceeding the above range, the adhesion between the Ni plating film and the surface of the rare earth alloy may decrease, and the plating film may peel off. is there.
【００１７】なお、熱処理時間に特に制限はなく、水素
が十分に除去できるように適宜選択すればよいが、通
常、０．１〜２４時間、特に０．５〜１０時間とするこ
とが好ましい。熱処理時間が前記範囲未満であると、水
素放出が不十分となりやすく、前記範囲を超えても熱処
理による効果は殆ど向上しない。The heat treatment time is not particularly limited and may be appropriately selected so that hydrogen can be sufficiently removed, but it is usually preferably 0.1 to 24 hours, particularly preferably 0.5 to 10 hours. If the heat treatment time is less than the above range, hydrogen release tends to be insufficient, and even if it exceeds the above range, the effect of the heat treatment is hardly improved.
【００１８】熱処理は、気流中において行なうことが好
ましい。すなわち、前記した雰囲気の気流中で、上記熱
処理を行なうことが好ましい。本発明では、雰囲気制御
を行なうため、通常、熱処理は電気炉などにより行なわ
れるが、熱処理空間が密閉されていると、希土類合金中
から放出された水素が滞留して熱処理空間内の水素ガス
分圧が上昇するため、水素の放出と吸蔵が平衡に達し、
水素を十分に除去することが困難となる。しかし、熱処
理を気流中で行ない、希土類合金から放出された水素を
熱処理空間内から速やかに除去することにより、このよ
うな現象が防止できる。The heat treatment is preferably performed in an air stream. That is, it is preferable to perform the heat treatment in the air flow of the atmosphere described above. In the present invention, since the atmosphere is controlled, the heat treatment is usually performed by an electric furnace or the like. However, when the heat treatment space is closed, hydrogen released from the rare earth alloy is retained and the hydrogen gas content in the heat treatment space is reduced. As the pressure rises, hydrogen release and occlusion reach equilibrium,
It becomes difficult to remove hydrogen sufficiently. However, such a phenomenon can be prevented by carrying out the heat treatment in an air stream and quickly removing the hydrogen released from the rare earth alloy from the heat treatment space.
【００１９】本発明が適用される希土類合金のＮｉめっ
き膜は、通常、下記のようにして形成される。The rare earth alloy Ni plating film to which the present invention is applied is usually formed as follows.
【００２０】Ｎｉめっき膜は、電気めっき法により形成
される。用いるめっき浴に特に制限はなく、各種半光沢
めっき浴や無光沢めっき浴等、例えば、ワット浴、スル
ファミン酸浴、ホウフッ化浴、臭化ニッケル浴等から適
宜選択すればよい。なお、Ｎｉ電気めっき浴のpHは、通
常、２．７〜４．５程度、温度は３５〜７０℃程度、電
流密度は０．２〜２０A/m2程度である。The Ni plating film is formed by the electroplating method. The plating bath used is not particularly limited and may be appropriately selected from various semi-bright plating baths and dull plating baths such as Watts bath, sulfamic acid bath, borofluoride bath, nickel bromide bath and the like. The pH of the Ni electroplating bath is usually about 2.7 to 4.5, the temperature is about 35 to 70 ° C., and the current density is about 0.2 to 20 A / m 2 .
【００２１】Ｎｉめっき膜の厚さは、用途等により最適
な範囲を選択すればよいが、通常、５〜１００μm 程度
である。The thickness of the Ni plating film may be selected in an optimum range depending on the application etc., but is usually about 5 to 100 μm.
【００２２】なお、前記の電気めっきを行なう前に、被
めっき物である希土類合金表面を、硝酸等によりエッチ
ングすることが好ましい。このようなエッチングによ
り、希土類合金とＮｉめっき膜との密着性を向上させる
ことができる。Before performing the above electroplating, it is preferable to etch the surface of the rare earth alloy, which is the object to be plated, with nitric acid or the like. By such etching, the adhesion between the rare earth alloy and the Ni plating film can be improved.
【００２３】本発明が適用される希土類合金に特に制限
はなく、本発明は、例えば、希土類磁石、磁歪材などの
各種希土類合金のＮｉめっき膜のフクレ防止に好適であ
る。The rare earth alloy to which the present invention is applied is not particularly limited, and the present invention is suitable for preventing blistering of Ni plating films of various rare earth alloys such as rare earth magnets and magnetostrictive materials.
【００２４】希土類磁石としては、Ｎｄ−Ｆｅ−Ｂ系永
久磁石や、Ｓｍ−Ｃｏ系永久磁石などが挙げられる。Ｓ
ｍ−Ｃｏ系永久磁石としては、Ｓｍ2 （Ｃｏ，Ｃｕ，Ｆ
ｅ，Ｍ）17（Ｍ＝Ｔｉ，Ｚｒ，Ｈｆ）などのＳｍ2 Ｃｏ
17系や、ＳｍＣｏ5 等が挙げられる。これらのうち、Ｎ
ｄ−Ｆｅ−Ｂ系永久磁石は水素吸蔵性が高いので、本発
明は特に有効である。Examples of rare earth magnets include Nd-Fe-B system permanent magnets and Sm-Co system permanent magnets. S
As the m-Co based permanent magnet, Sm 2 (Co, Cu, F
e, M) 17 (M = Ti, Zr, Hf) and other Sm 2 Co
Examples include 17 series and SmCo 5 . Of these, N
The present invention is particularly effective because the d-Fe-B permanent magnet has a high hydrogen storage property.
【００２５】磁歪材としては、Ｔｂ−ＦｅやＳｍ−Ｆｅ
等の希土類−遷移金属系超磁歪材料などが挙げられる。The magnetostrictive material is Tb-Fe or Sm-Fe.
Rare earth-transition metal-based giant magnetostrictive materials and the like.
【００２６】本発明が適用される希土類合金の形状およ
び製造方法にも特に制限はない。例えば、製造方法が、
焼結法、急冷法、鋳造法等のいずれであった場合でも、
本発明の効果は実現する。The shape and manufacturing method of the rare earth alloy to which the present invention is applied are not particularly limited. For example, the manufacturing method is
Whether it is a sintering method, a quenching method, or a casting method,
The effects of the present invention are realized.
【００２７】以下、本発明が特に好ましく適用されるＮ
ｄ−Ｆｅ−Ｂ系永久磁石について説明する。Hereinafter, the present invention is particularly preferably applied to N.
The d-Fe-B permanent magnet will be described.
【００２８】Ｎｄ−Ｆｅ−Ｂ系永久磁石は、Ｎｄ2 Ｆｅ
14Ｂ金属間化合物を主相とし、この主相は実質的に正方
晶系の結晶構造を有する。The Nd-Fe-B system permanent magnet is composed of Nd 2 Fe.
The 14 B intermetallic compound is the main phase, and this main phase has a substantially tetragonal crystal structure.
【００２９】本発明が適用される場合、磁石全体の組成
は特に限定されない。すなわち、焼結法や急冷法等の製
造方法に応じてあるいは要求される磁気特性等に応じて
適宜選択されたいずれの組成に対しても本発明は効果を
発揮するが、通常、Ｎｄ−Ｆｅ−Ｂ系永久磁石の組成
は、５．５原子％≦Ｎｄ≦３０原子％、４２原子％≦Ｆ
ｅ≦９０原子％および２原子％≦Ｂ≦２８原子％程度と
される。When the present invention is applied, the composition of the whole magnet is not particularly limited. That is, the present invention is effective for any composition selected appropriately according to the manufacturing method such as the sintering method or the quenching method, or according to the required magnetic properties, etc. The composition of the B type permanent magnet is 5.5 at% ≦ Nd ≦ 30 at%, 42 at% ≦ F.
e is set to about 90 atomic% and 2 atomic% ≦ B ≦ 28 atomic%.
【００３０】そして、Ｎｄの一部を、他の希土類元素、
例えば、Ｐｒ、Ｈｏ、Ｔｂ、Ｌａ、Ｓｍ、Ｃｅ、Ｇｄ、
Ｅｒ、Ｅｕ、Ｐｍ、Ｔｍ、Ｙｂ、Ｙ等の１種以上で置換
してもよい。Ｎｄに対するこれらの元素の置換率は、２
０％以下であることが好ましい。Then, a part of Nd is replaced with another rare earth element,
For example, Pr, Ho, Tb, La, Sm, Ce, Gd,
You may substitute by 1 or more types, such as Er, Eu, Pm, Tm, Yb, and Y. The substitution rate of these elements for Nd is 2
It is preferably 0% or less.
【００３１】また、温度特性の改善のために、Ｆｅの一
部をＣｏで置換してもよい。Ｆｅに対するＣｏの置換率
は、５０％以下とすることが好ましい。Further, in order to improve the temperature characteristics, a part of Fe may be replaced with Co. The substitution rate of Co for Fe is preferably 50% or less.
【００３２】また、これらの元素の他、Ｃａ、Ｃ、Ｐ、
Ｓ、Ｃｕ、Ａｌ、Ｔｉ、Ｖ、Ｃｒ、Ｍｎ、Ｂｉ、Ｎｂ、
Ｔａ、Ｍｏ、Ｗ、Ｓｂ、Ｇｅ、Ｓｎ、Ｚｒ、Ｎｉ、Ｓ
ｉ、Ｈｆ等の１種以上が含有されていてもよい。これら
の元素の含有率は、通常、総計で１０原子％以下とする
ことが好ましい。In addition to these elements, Ca, C, P,
S, Cu, Al, Ti, V, Cr, Mn, Bi, Nb,
Ta, Mo, W, Sb, Ge, Sn, Zr, Ni, S
One or more of i, Hf and the like may be contained. Generally, the total content of these elements is preferably 10 atomic% or less.
【００３３】本発明が適用される希土類磁石を製造する
方法は、前述したように特に限定されず、通常の焼結
法、急冷法、鋳造法等を用いればよい。The method for producing the rare earth magnet to which the present invention is applied is not particularly limited as described above, and a usual sintering method, quenching method, casting method or the like may be used.
【００３４】[0034]
【実施例】以下、本発明の具体的実施例を示し、本発明
をさらに詳細に説明する。EXAMPLES The present invention will be described in more detail below by showing specific examples of the present invention.
【００３５】粉末冶金法によって作製した１４Ｎｄ−１
Ｄｙ−７Ｂ−７８Ｆｅ（数字は原子比）の組成をもつ焼
結体をＡｒ雰囲気中で６００℃にて２時間時効処理を施
し、２５mm×２５mm×１．５mmの板状に加工し、さらに
バレル研磨処理により面取りを行なって、永久磁石を得
た。14Nd-1 produced by powder metallurgy
A sintered body having a composition of Dy-7B-78Fe (numbers are atomic ratios) is aged at 600 ° C for 2 hours in an Ar atmosphere, processed into a plate shape of 25 mm × 25 mm × 1.5 mm, and further barreled. Chamfering was performed by a polishing treatment to obtain a permanent magnet.
【００３６】この永久磁石を、ジャパンメタルフィニッ
シングカンパニー社製エンドックス１１４溶液（１２０
g/1 、６０℃）に１０分間浸漬した。This permanent magnet was mixed with Endox 114 solution (120 ml, manufactured by Japan Metal Finishing Company).
g / 1, 60 ° C.) for 10 minutes.
【００３７】次いで、イオン交換水（塩素含有量０．５
ppm ）を用いて１Ｎ HNO3溶液を調製した。この溶液
に、上記永久磁石を室温で５分間浸漬した後、前記イオ
ン交換水中で超音波洗浄した。Next, ion-exchanged water (with a chlorine content of 0.5
ppm) was used to prepare a 1N HNO 3 solution. The permanent magnet was immersed in this solution at room temperature for 5 minutes, and then ultrasonically washed in the ion-exchanged water.
【００３８】洗浄後、下記組成のめっき浴を用い、浴温
５５℃、電流密度３A/dm2 にてバレル法により電気めっ
きを行なった。浴pHは、４．５とした。After washing, electroplating was performed by a barrel method using a plating bath having the following composition at a bath temperature of 55 ° C. and a current density of 3 A / dm 2 . The bath pH was 4.5.
【００３９】めっき浴組成 硫酸ニッケル（Ｎｉ4 ＳＯ4 ・７Ｈ2 Ｏ） ３００g/l ホウ酸（Ｈ3 ＢＯ3 ） ４０g/l ２−ブチン−１，４−ジオール（Ｓ不含有光沢剤） ０．３g/l ラウリル硫酸ナトリウム ０．０５g/l Plating bath composition Nickel sulfate (Ni 4 SO 4 .7H 2 O) 300 g / l Boric acid (H 3 BO 3 ) 40 g / l 2-Butyne-1,4-diol (S-free brightener) 3g / l sodium lauryl sulfate 0.05g / l
【００４０】このようにして、膜厚１５μm の半光沢Ｎ
ｉめっき膜を得た。なお、膜厚はセイコー電子の蛍光Ｘ
線膜厚計により測定した。Thus, the semi-gloss N having a film thickness of 15 μm is obtained.
An i-plated film was obtained. In addition, the film thickness is Seiko electron fluorescence X.
It was measured by a linear film thickness meter.
【００４１】このようにして得られた永久磁石１００個
を、電気炉内で下記の条件にて熱処理した。100 permanent magnets thus obtained were heat-treated in an electric furnace under the following conditions.
【００４２】熱処理条件
温度：１５０℃
時間：１０時間
雰囲気ガス：Ｎ2 ガス｛日本酸素株式会社の純窒素ガス
（Ａグレード）｝
雰囲気ガス中の水蒸気含有量：０．１体積％以下
雰囲気ガス流量：１００cc／分 Heat treatment conditions Temperature: 150 ° C. Time: 10 hours Atmosphere gas: N 2 gas {Pure nitrogen gas (A grade) from Nippon Oxygen Co., Ltd.} Water vapor content in atmosphere gas: 0.1 vol% or less Atmosphere gas flow rate : 100cc / min
【００４３】熱処理後、１００個の永久磁石を高温・高
湿環境（８５℃・８０％ＲＨ）で１００時間保存した結
果、どの磁石のＮｉめっき膜にもフクレは発生しなかっ
た。After the heat treatment, 100 permanent magnets were stored in a high temperature and high humidity environment (85 ° C., 80% RH) for 100 hours. As a result, no blistering occurred on the Ni plating film of any magnet.
【００４４】また、比較のために、上記熱処理を施さな
かった磁石を上記高温・高湿環境で１００時間保存し
た。この結果、１００個の磁石中、１０個の磁石にフク
レが認められた。For comparison, the magnet not subjected to the heat treatment was stored for 100 hours in the high temperature and high humidity environment. As a result, blistering was observed in 10 of the 100 magnets.
【００４５】以上の実施例の結果から、本発明の効果が
明らかである。From the results of the above examples, the effect of the present invention is clear.
【００４６】[0046]
【発明の効果】本発明によれば、希土類合金表面に形成
されたＮｉめっき膜のフクレを効果的に防止することが
できる。According to the present invention, it is possible to effectively prevent blistering of the Ni plating film formed on the surface of the rare earth alloy.
Claims (5)
き膜を表面に有する希土類合金を、水蒸気含有量が１体
積％以下である雰囲気中において、１００〜２００℃に
て熱処理することを特徴とするＮｉめっき希土類合金の
ベーキング方法。1. A rare earth alloy having a Ni plating film formed by an electroplating method on its surface is heat-treated at 100 to 200 ° C. in an atmosphere having a water vapor content of 1% by volume or less. A method of baking a Ni-plated rare earth alloy.
て行なう請求項１に記載のＮｉめっき希土類合金のベー
キング方法。2. The method of baking a Ni-plated rare earth alloy according to claim 1, wherein the heat treatment is performed in an air stream of the atmosphere.
求項１または２に記載のＮｉめっき希土類合金のベーキ
ング方法。3. The method for baking a Ni-plated rare earth alloy according to claim 1, wherein the heat treatment is performed for 0.1 to 24 hours.
である請求項１ないし３のいずれかに記載のＮｉめっき
希土類合金のベーキング方法。4. The method for baking a Ni-plated rare earth alloy according to claim 1, wherein the atmosphere is N 2 gas or Ar gas.
を含有する永久磁石である請求項１ないし４のいずれか
に記載のＮｉめっき希土類合金のベーキング方法。5. The rare earth alloy is Nd, Fe and B.
The method for baking a Ni-plated rare earth alloy according to any one of claims 1 to 4, which is a permanent magnet containing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19342891A JPH059784A (en) | 1991-07-08 | 1991-07-08 | Method for baking ni-plated rare earth alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19342891A JPH059784A (en) | 1991-07-08 | 1991-07-08 | Method for baking ni-plated rare earth alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH059784A true JPH059784A (en) | 1993-01-19 |
Family
ID=16307813
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19342891A Withdrawn JPH059784A (en) | 1991-07-08 | 1991-07-08 | Method for baking ni-plated rare earth alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH059784A (en) |
-
1991
- 1991-07-08 JP JP19342891A patent/JPH059784A/en not_active Withdrawn
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