JPH073489A - Soft magnetic thin film - Google Patents
Soft magnetic thin filmInfo
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- JPH073489A JPH073489A JP23553793A JP23553793A JPH073489A JP H073489 A JPH073489 A JP H073489A JP 23553793 A JP23553793 A JP 23553793A JP 23553793 A JP23553793 A JP 23553793A JP H073489 A JPH073489 A JP H073489A
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- Prior art keywords
- thin film
- soft magnetic
- magnetic thin
- face
- centered cubic
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- Magnetic Heads (AREA)
- Thin Magnetic Films (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、軟磁性薄膜、特に電気
めっき法により作製した低保磁力、高飽和磁束密度の軟
磁性薄膜に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a soft magnetic thin film, and particularly to a soft magnetic thin film having a low coercive force and a high saturation magnetic flux density produced by an electroplating method.
【０００２】[0002]
【従来の技術】薄膜磁気ヘッドや薄膜トランスの磁性薄
膜には、低保磁力、高飽和磁束密度等の優れた軟磁気特
性が要求される。2. Description of the Related Art Magnetic thin films for thin film magnetic heads and thin film transformers are required to have excellent soft magnetic characteristics such as low coercive force and high saturation magnetic flux density.
【０００３】これらの磁性薄膜は、スパッタ法等の気相
成膜法やめっき法等の液相成膜法により形成されるのが
一般的であるが、めっき法、特に電気めっき法は、大面
積の成膜が容易で、しかも均一性の高い膜が得られ、ま
た、工程数が少なく設備が安価であるという利点があ
る。These magnetic thin films are generally formed by a vapor phase film forming method such as a sputtering method or a liquid phase film forming method such as a plating method. However, the plating method, especially the electroplating method is large. There are advantages that a film having a large area can be easily formed, a film with high uniformity can be obtained, and the number of steps is small and the equipment is inexpensive.
【０００４】このようなことから電着パーマロイ（Ｎｉ
−Ｆｅ合金）膜が薄膜ヘッド磁極材料として現在広く使
用されている。From these things, electrodeposited permalloy (Ni
-Fe alloy) film is currently widely used as a thin film head magnetic pole material.
【０００５】ところで、近年の記録密度の上昇は、記録
媒体の保磁力（Ｈc ）の上昇による部分が大きい。保磁
力の大きな記録媒体に十分に書き込むためには、記録ヘ
ッドからより強い磁界を発生する必要がある。また、Ｍ
Ｒ（磁気抵抗）インダクティブ複合ヘッドのシールド層
の磁性材料も、高密度記録のためには、より薄い膜で所
望のシールド効果が期待できる高飽和磁束密度材料が必
要となってきている。ところが、上記のパーマロイの飽
和磁束密度（Ｂs ）は１Ｔ以下であり、より飽和磁束密
度（Ｂs ）の高い材料が求められている。Incidentally, the recent increase in recording density is largely due to the increase in coercive force (Hc) of the recording medium. In order to sufficiently write on a recording medium having a large coercive force, it is necessary to generate a stronger magnetic field from the recording head. Also, M
For the magnetic material of the shield layer of the R (magnetoresistive) inductive composite head, a high saturation magnetic flux density material that can be expected to have a desired shield effect with a thinner film is required for high density recording. However, the saturation magnetic flux density (Bs) of permalloy is 1T or less, and a material having a higher saturation magnetic flux density (Bs) is required.
【０００６】この磁気特性的な要求を満たす磁性めっき
膜の一つとしては、Ｃｏ−Ｎｉ−Ｆｅ系合金が挙げられ
る。A Co—Ni—Fe alloy is one of the magnetic plating films satisfying the magnetic property requirements.
【０００７】このＣｏ−Ｎｉ−Ｆｅ系合金のバルク材の
磁気特性については、R.M.Bozorth,Ferromagnetism, 19
51 (D.Van Nostrand Company, Inc.)にまとめられてい
る。このなかに記載された図５−８４によれば、保磁力
（Ｈc ）が小さくなるのはＣｏが少ない組成のみであ
り、特にＨc ＜０．３Oeはわずかな組成範囲に限定され
ていることがわかる。Regarding the magnetic properties of the bulk material of this Co--Ni--Fe alloy, RMBozorth, Ferromagnetism, 19
51 (D. Van Nostrand Company, Inc.). According to FIG. 5-84 described therein, the coercive force (Hc) decreases only in the composition containing a small amount of Co, and in particular, Hc <0.3 Oe is limited to a small composition range. Recognize.
【０００８】また、特公昭６３−５３２７７号には、コ
バルト−ニッケル−鉄合金の電気めっき浴組成物が開示
されており、これを用いて電気めっきを行うことによ
り、低い保磁力、高い飽和磁化（４πＭｓ）、および０
または僅かに負の磁歪を有するコバルト−ニッケル−鉄
合金被膜が得られることが示されている。この場合保磁
力（Ｈc ）は２Oe以下となると記載されており、実施例
に示されたＣｏＮｉＦｅ被膜（約８０：１０：１０）で
は４πＭｓ＝１６ｋＧ、Ｈc ＝１．５Oeが得られてい
る。４πＭｓはパーマロイの２倍近い値となっている
が、保磁力がパーマロイに比べてかなり高く、軟磁気特
性において劣るものとなっている。Further, Japanese Patent Publication No. 63-53277 discloses a cobalt-nickel-iron alloy electroplating bath composition, which is electroplated to obtain a low coercive force and a high saturation magnetization. (4πMs), and 0
Alternatively, it has been shown that a cobalt-nickel-iron alloy coating having a slightly negative magnetostriction can be obtained. In this case, it is described that the coercive force (Hc) is not more than 2 Oe, and the CoNiFe coating (about 80:10:10) shown in the examples gives 4πMs = 16 kG and Hc = 1.5 Oe. The value of 4πMs is almost twice as large as that of permalloy, but the coercive force is considerably higher than that of permalloy, and the soft magnetic property is inferior.
【０００９】また、米国特許第５０１１５８１号（対応
特開平２−１３８７１６号）には、電着法による高飽和
磁束密度合金薄膜の製造方法が開示されている。実施例
の膜サンプルが示すとおり、Ｂs は１０５００〜１８５
００G の範囲にあり高いものとなっているが、Ｈc は最
小のものでも１Oeであり軟磁気特性が十分でない。Further, US Pat. No. 5,011,581 (corresponding to Japanese Patent Laid-Open No. 2-138716) discloses a method for producing a high saturation magnetic flux density alloy thin film by an electrodeposition method. As the membrane sample of the example shows, Bs is 10500-185.
Although it is high in the range of 00G, even the smallest Hc is 10 Oe, the soft magnetic characteristics are not sufficient.
【００１０】また、特開平２−６８９０６号には、Ｆ
ｅ、Ｃｏ、Ｎｉを主成分とし、Ｆｅが２０〜７５at% 、
Ｃｏが５〜４５at% 、Ｎｉが２０〜７０at% であり、薄
膜面として面心立方格子構造の（２２０）面または（１
１１）面を優先的に面配向させた高飽和磁束密度軟磁性
膜が開示されている。膜の製法として、蒸着法、電着法
が示されているが、実施例で電着法によって作製したサ
ンプルは（１１１）配向のＦｅ29Ｃｏ7 Ｎｉ64（数値は
at% ）膜のみであり、Ｈc は２．５Oeとなっており、軟
磁気特性が十分とはいえない。Further, in Japanese Patent Laid-Open No. 2-68906, F
e, Co, Ni as main components, Fe 20 to 75 at%,
Co is 5 to 45 at%, Ni is 20 to 70 at%, and the (220) plane of the face-centered cubic lattice structure or (1
11) A high saturation magnetic flux density soft magnetic film in which planes are preferentially oriented is disclosed. Vapor deposition method and electrodeposition method are shown as the method for forming the film, but the sample produced by the electrodeposition method in the examples is (111) oriented Fe 29 Co 7 Ni 64 (the numerical value is
At%) film only, and Hc is 2.5 Oe, so the soft magnetic characteristics cannot be said to be sufficient.
【００１１】また第１６回日本応用磁気学会学術講演概
要集の７ｐＦ−１５には、耐食性に優れ、かつ高い飽和
磁束密度を有するＣｏ−Ｆｅ−Ｎｉ膜が報告されてお
り、Ｃｏ＝５０〜６０wt% 、Ｆｅ＝２０〜３０wt% 、Ｎ
ｉ＝２０〜３０wt% の組成でのめっき軟磁性膜が示され
ている。このものは１９ｋＧ以上の高Ｂs を有するもの
であるが、透磁率（μ）は６００〜７００程度であり、
パーマロイと比べて低く、保磁力も大きいと推定され
る。Further, in 7pF-15 of the 16th Japan Society for Applied Magnetics, a summary of scientific lectures, a Co-Fe-Ni film having excellent corrosion resistance and a high saturation magnetic flux density is reported, and Co = 50-60wt. %, Fe = 20 to 30 wt%, N
A plated soft magnetic film with a composition of i = 20 to 30 wt% is shown. This has a high Bs of 19 kG or more, but the magnetic permeability (μ) is about 600 to 700,
It is presumed to have a lower coercive force and a higher coercive force than permalloy.
【００１２】以上のことから、電気めっき法により、高
Ｂs で低Ｈc のＣｏ−Ｆｅ−Ｎｉ系の軟磁性薄膜を得る
ことが望まれている。From the above, it is desired to obtain a Co--Fe--Ni type soft magnetic thin film having a high Bs and a low Hc by the electroplating method.
【００１３】[0013]
【発明が解決しようとする課題】本発明の目的は、通
常、０．５Oe以下、特に０．３Oe以下、さらには０．２
Oe以下の低保磁力を有し、かつ飽和磁束密度の高い軟磁
性薄膜を提供することにある。The object of the present invention is usually 0.5 Oe or less, particularly 0.3 Oe or less, and even 0.2 Oe or less.
It is to provide a soft magnetic thin film having a low coercive force of Oe or less and a high saturation magnetic flux density.
【００１４】[0014]
【課題を解決するための手段】このような目的は、下記
（１）〜（１３）の構成によって達成される。 （１）ＣｏとＮｉとＦｅとを含有し、面心立方晶相から
なり、Ｘ線回折における面心立方晶（２００）面のピー
ク強度および面心立方晶（１１１）面のピーク強度をそ
れぞれＩ（２００）およびＩ（１１１）としたとき、 ０．１≦Ｉ（２００）／Ｉ（１１１）≦０．２ であることを特徴とする軟磁性薄膜。 （２）ＣｏとＮｉとＦｅとを含有し、面心立方晶相を主
とし、微量の体心立方晶相を含み、Ｘ線回折における面
心立方晶（２００）面のピーク強度、面心立方晶（１１
１）面のピーク強度および体心立方晶（１１０）面のピ
ーク強度をそれぞれＩ（２００）、Ｉ（１１１）および
Ｉ（１１０）としたとき、 Ｉ（２００）／Ｉ（１１１）≧０．１かつ Ｉ（１１０）／Ｉ（１１１）≦０．１ であることを特徴とする軟磁性薄膜。 （３）Ｉ（２００）／Ｉ（１１１）≦０．２ である上記（２）の軟磁性薄膜。 （４）電気めっき法により形成され、形成直後には面心
立方晶単相であり、熱処理により体心立方晶相を共析し
たものである上記（２）または（３）の軟磁性薄膜。 （５）前記熱処理の際の温度が２４０〜３７０℃である
上記（４）の軟磁性薄膜。 （６）ａＣｏ−ｂＮｉ−ｃＦｅ［ここで、ａ、ｂおよび
ｃは、それぞれＣｏ、ＮｉおよびＦｅの比率（wt% ）を
表し、 ａ＝２８〜７５wt% 、 ｂ＝１６〜６０wt% 、 ｃ＝９〜４２wt% 、および ａ＋ｂ＋ｃ＝１００wt% の関係を満足する。］で表される組成を有する上記
（１）ないし（５）のいずれかの軟磁性薄膜。 （７）ａＣｏ−ｂＮｉ−ｃＦｅ［ここで、ａ、ｂおよび
ｃは、それぞれＣｏ、ＮｉおよびＦｅの比率（wt% ）を
表し、 ａ＝３０〜６０wt% 、 ｂ＝２０〜５０wt% 、 ｃ＝１０〜４０wt% 、および ａ＋ｂ＋ｃ＝１００wt% の関係を満足する。］で表される組成を有する上記
（６）の軟磁性薄膜。 （８）ａＣｏ−ｂＮｉ−ｃＦｅ［ここで、ａ、ｂおよび
ｃは、それぞれＣｏ、ＮｉおよびＦｅの比率（wt% ）を
表し、 ａ＝３５〜４５wt% 、 ｂ＝２５〜３５wt% 、 ｃ＝２５〜３５wt% 、および ａ＋ｂ＋ｃ＝１００wt% の関係を満足する。］で表される組成を有する上記
（７）の軟磁性薄膜。 （９）Ｃｏイオン、ＮｉイオンおよびＦｅイオンを含有
し、ｐＨ２〜１０、温度１０〜８０℃のめっき浴を用
い、電流密度０．５〜４．０A/dm2 の条件で電気めっき
法により作製した上記（１）ないし（８）のいずれかの
軟磁性薄膜。 （１０）パーマロイを下地膜として作製した上記（９）
の軟磁性薄膜。 （１１）保磁力が０．５Oe以下で、飽和磁束密度が１３
kG以上である上記（１）ないし（10）のいずれかの軟磁
性薄膜。 （１２）保磁力が０．３Oe以下である上記（11）の軟磁
性薄膜。 （１３）保磁力が０．２Oe以下である上記（12）の軟磁
性薄膜。Such an object is achieved by the following constitutions (1) to (13). (1) Containing Co, Ni, and Fe, consisting of a face-centered cubic phase, and having a peak intensity of a face-centered cubic (200) face and a face-centered cubic (111) face in X-ray diffraction, respectively. When I (200) and I (111) are satisfied, 0.1 ≦ I (200) / I (111) ≦ 0.2. (2) Containing Co, Ni, and Fe, mainly a face-centered cubic phase, and a small amount of a body-centered cubic phase, and the peak intensity and face center of the face-centered cubic (200) plane in X-ray diffraction. Cubic (11
1 (200), I (111) and I (110), the peak intensity of the (1) plane and the peak intensity of the body-centered cubic (110) plane are I (200) / I (111) ≧ 0. 1 and I (110) / I (111) ≦ 0.1, a soft magnetic thin film. (3) The soft magnetic thin film according to (2) above, wherein I (200) / I (111) ≦ 0.2. (4) The soft magnetic thin film according to the above (2) or (3), which is formed by an electroplating method, has a face-centered cubic single phase immediately after formation, and has a body-centered cubic phase co-deposited by heat treatment. (5) The soft magnetic thin film according to (4) above, wherein the temperature during the heat treatment is 240 to 370 ° C. (6) aCo-bNi-cFe [where a, b and c represent the ratio (wt%) of Co, Ni and Fe, respectively, a = 28 to 75 wt%, b = 16 to 60 wt%, c = The relations of 9 to 42 wt% and a + b + c = 100 wt% are satisfied. ] The soft magnetic thin film in any one of said (1) thru | or (5) which has a composition represented by these. (7) aCo-bNi-cFe [where a, b and c represent the ratios (wt%) of Co, Ni and Fe, respectively, a = 30 to 60 wt%, b = 20 to 50 wt%, c = The relations of 10 to 40 wt% and a + b + c = 100 wt% are satisfied. ] The soft magnetic thin film of said (6) which has a composition represented by these. (8) aCo-bNi-cFe [where a, b and c represent the ratio (wt%) of Co, Ni and Fe, respectively, a = 35 to 45 wt%, b = 25 to 35 wt%, c = The relations of 25 to 35 wt% and a + b + c = 100 wt% are satisfied. ] The soft magnetic thin film of said (7) which has a composition represented by this. (9) Produced by electroplating using a plating bath containing Co ions, Ni ions and Fe ions and having a pH of 2 to 10 and a temperature of 10 to 80 ° C. and a current density of 0.5 to 4.0 A / dm 2. The soft magnetic thin film according to any one of (1) to (8) above. (10) The above (9) in which Permalloy is prepared as a base film.
Soft magnetic thin film. (11) Coercive force of 0.5 Oe or less and saturation magnetic flux density of 13
The soft magnetic thin film according to any one of (1) to (10), which has a kG or more. (12) The soft magnetic thin film according to (11) above, which has a coercive force of 0.3 Oe or less. (13) The soft magnetic thin film according to (12), which has a coercive force of 0.2 Oe or less.
【００１５】[0015]
【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。Specific Structure The specific structure of the present invention will be described in detail below.
【００１６】本発明の軟磁性薄膜は、Ｃｏ、Ｎｉおよび
Ｆｅを含有する。この軟磁性薄膜は、面心立方晶（ｆｃ
ｃ）相の単相であるか、好ましくは面心立方晶相を主と
し微量の体心立方晶（ｂｃｃ）相を含む。The soft magnetic thin film of the present invention contains Co, Ni and Fe. This soft magnetic thin film has a face-centered cubic (fc)
c) A single phase, or preferably containing mainly a face-centered cubic phase and a small amount of a body-centered cubic (bcc) phase.
【００１７】本発明の軟磁性薄膜がｆｃｃ相の単相から
なる場合、Ｘ線回折チャートにおけるｆｃｃ（２００）
面のピーク強度およびｆｃｃ（１１１）面のピーク強度
をそれぞれＩ（２００）およびＩ（１１１）としたと
き、 ０．１≦Ｉ（２００）／Ｉ（１１１）≦０．２、好まし
くは ０．１５≦Ｉ（２００）／Ｉ（１１１）≦０．２ である。Ｉ（２００）／Ｉ（１１１）＞０．２である
と、保磁力が大きくなってしまう。When the soft magnetic thin film of the present invention is composed of a single phase of the fcc phase, fcc (200) in the X-ray diffraction chart
When the peak intensity of the plane and the peak intensity of the fcc (111) plane are I (200) and I (111), respectively, 0.1 ≦ I (200) / I (111) ≦ 0.2, preferably 0. 15 ≦ I (200) / I (111) ≦ 0.2. If I (200) / I (111)> 0.2, the coercive force increases.
【００１８】本発明の軟磁性薄膜が、ｆｃｃ相を主とし
微量のｂｃｃ相を含む場合には、Ｘ線回折におけるｂｃ
ｃ（１１０）面のピーク強度をＩ（１１０）としたと
き、 Ｉ（２００）／Ｉ（１１１）≧０．１、好ましくは Ｉ（２００）／Ｉ（１１１）≧０．１５ であって、かつ Ｉ（１１０）／Ｉ（１１１）≦０．１ である。この場合、通常、 Ｉ（２００）／Ｉ（１１１）≦１ であり、好ましくは Ｉ（２００）／Ｉ（１１１）≦０．２ である。この場合にＩ（２００）／Ｉ（１１１）＞０．
２となると、保磁力が大きくなる傾向にある。When the soft magnetic thin film of the present invention mainly contains the fcc phase and a small amount of the bcc phase, bc in X-ray diffraction is used.
When the peak intensity of the c (110) plane is I (110), I (200) / I (111) ≧ 0.1, preferably I (200) / I (111) ≧ 0.15, Further, I (110) / I (111) ≦ 0.1. In this case, usually, I (200) / I (111) ≦ 1, preferably I (200) / I (111) ≦ 0.2. In this case, I (200) / I (111)> 0.
When it becomes 2, the coercive force tends to increase.
【００１９】ｂｃｃ相の存在は、電子線回折により確認
することができるが、電子線回折によりｂｃｃ相が確認
されている場合でも、汎用のＸ線回折装置を用いた場合
にはＩ（１１０）／Ｉ（１１１）＝０となって、その存
在が確認できないこともある。これは、一般にＸ線回折
が電子線回折よりも感度が低いためである。本発明で
は、電子線回折によりｂｃｃ相が確認できればＩ（１１
０）／Ｉ（１１１）＝０であってもよい。本発明におけ
る好ましい組成範囲はｂｃｃ相が共析を開始する直前の
組成範囲なので、汎用のＸ線回折装置では検出不可能な
程度の極めて微量のｂｃｃ相が局部的に偏析することで
高特性が得られていると考えられる。具体的には、ｆｃ
ｃ相からなる結晶粒の粒界にｂｃｃ相が析出することに
より粒子分離が進むため、あるいは結晶磁気異方性の和
が小さくなる方向への変化が生じるため、低保磁力が得
られるものと考えられる。一方、Ｉ（１１０）／Ｉ（１
１１）＞０．１である場合、ｂｃｃ相自体が結晶成長し
ているため、あるいはｂｃｃ相の結晶磁気異方性の影響
が大きくなるため、保磁力が増大してしまうと考えられ
る。The presence of the bcc phase can be confirmed by electron diffraction, but even if the bcc phase is confirmed by electron diffraction, I (110) is obtained when a general-purpose X-ray diffractometer is used. In some cases, / I (111) = 0 and the existence cannot be confirmed. This is because X-ray diffraction is generally less sensitive than electron beam diffraction. In the present invention, if the bcc phase can be confirmed by electron diffraction, then I (11
It may be 0) / I (111) = 0. Since the preferred composition range in the present invention is the composition range immediately before the bcc phase starts co-deposition, a very small amount of the bcc phase, which cannot be detected by a general-purpose X-ray diffractometer, is locally segregated to obtain high characteristics. It is considered to have been obtained. Specifically, fc
A low coercive force can be obtained because the bcc phase is precipitated at the grain boundary of the crystal grain composed of the c phase to cause particle separation or change in the direction in which the sum of the crystal magnetic anisotropy decreases. Conceivable. On the other hand, I (110) / I (1
When 11)> 0.1, it is considered that the coercive force is increased because the crystal of the bcc phase itself is grown or the influence of the crystal magnetic anisotropy of the bcc phase is increased.
【００２０】本発明では、結晶相の構成および結晶面の
配向を上記のようにすることにより、低保磁力かつ高飽
和磁束密度のＣｏ−Ｎｉ−Ｆｅ軟磁性薄膜が得られる。
特に、保磁力（Ｈc ）は０．５Oe以下、好ましくは０．
３Oe以下、さらに好ましくは０．２Oe以下、特に好まし
くは０．１Oe以下が実現でき、極めて良好な軟磁気特性
を示す。また、飽和磁束密度（Ｂs ）は１３〜２０kG程
度である。In the present invention, a Co-Ni-Fe soft magnetic thin film having a low coercive force and a high saturation magnetic flux density can be obtained by setting the crystal phase constitution and the crystal plane orientation as described above.
In particular, the coercive force (Hc) is 0.5 Oe or less, preferably 0.
It is possible to achieve 3 Oe or less, more preferably 0.2 Oe or less, and particularly preferably 0.1 Oe or less, and exhibit extremely good soft magnetic properties. The saturation magnetic flux density (Bs) is about 13 to 20 kG.
【００２１】従って、本発明の軟磁性薄膜は、薄膜ヘッ
ドや薄膜トランス用の磁性薄膜として極めて有用であ
る。特に、インダクティブＭＲヘッドのオーバーライト
特性の向上効果や、シールド層間減少による記録密度の
向上効果が期待できる。Therefore, the soft magnetic thin film of the present invention is extremely useful as a magnetic thin film for thin film heads and thin film transformers. In particular, the effect of improving the overwrite characteristics of the inductive MR head and the effect of improving the recording density by reducing the shield layers can be expected.
【００２２】これに対し、主相が他の晶相である場合に
はＨc が高くなってしまう。また、Ｉ（１１０）／Ｉ
（１１１）＞０．１となる程度にｂｃｃ相が混在する場
合や、ｆｃｃ相が主相であってもＩ（２００）／Ｉ（１
１１）＜０．１である場合には、Ｈc が高くなり良好な
軟磁気特性が得られない（図１参照）。なお、図１にｆ
ｃｃ＋ｂｃｃと表示してあるものは、Ｉ（１１０）／Ｉ
（１１１）＞０．１のものである。On the other hand, when the main phase is another crystal phase, Hc becomes high. Also, I (110) / I
When bcc phases are mixed to such an extent that (111)> 0.1 or even when the fcc phase is the main phase, I (200) / I (1
11) When <0.1, Hc becomes high and good soft magnetic characteristics cannot be obtained (see FIG. 1). In addition, in FIG.
What is displayed as cc + bcc is I (110) / I
(111)> 0.1.
【００２３】本発明において、特に所望の構造とするた
めにはパーマロイを下地膜として用いることが好まし
い。例えば、銅を下地膜とすると同じ組成の膜でも所望
の結晶構造が得られないために軟磁気特性が悪くなる。
パーマロイの下地膜の厚さは、通常４００〜１０００A
程度とする。In the present invention, it is preferable to use permalloy as a base film in order to obtain a desired structure. For example, when copper is used as the base film, a desired crystal structure cannot be obtained even with a film having the same composition, so that the soft magnetic characteristics are deteriorated.
The thickness of permalloy base film is usually 400-1000A
The degree.
【００２４】本発明の軟磁性薄膜は、低Ｈc を得る上
で、下記の組成を有することが好ましい。The soft magnetic thin film of the present invention preferably has the following composition in order to obtain low Hc.
【００２５】ａＣｏ−ｂＮｉ−ｃＦｅ 上記において、ａ＋ｂ＋ｃ＝１００wt% であり、ａ＝２
８〜７５wt% 、さらには３０〜６０wt% 、特には３５〜
４５wt% が好ましく、ｂ＝１６〜５６wt% 、さらには２
０〜５０wt% 、特には２５〜３５wt% が好ましく、ｃ＝
９〜４２wt% 、さらには１０〜４０wt% 、特には２５〜
３５wt% であることが好ましい。ACo-bNi-cFe In the above, a + b + c = 100 wt% and a = 2
8 to 75 wt%, further 30 to 60 wt%, especially 35 to
45 wt% is preferable, b = 16 to 56 wt%, and further 2
0 to 50 wt%, particularly 25 to 35 wt% is preferable, and c =
9 to 42 wt%, further 10 to 40 wt%, especially 25 to
It is preferably 35 wt%.
【００２６】なお、上記のａ＝２８〜７５wt% 、ｂ＝１
６〜５６wt% 、ｃ＝９〜４２wt% で表される組成範囲
は、図２に示される点Ａ、Ｂ、Ｃ、Ｄを図示のように結
ぶ線で囲まれる領域であり、この領域内で０．５Oe以
下、特に０．４Oe以下のＨc が得られる。The above a = 28 to 75 wt% and b = 1
The composition range represented by 6 to 56 wt% and c = 9 to 42 wt% is a region surrounded by a line connecting points A, B, C and D shown in FIG. 2 within this region. Hc of 0.5 Oe or less, particularly 0.4 Oe or less, can be obtained.
【００２７】また、上記のａ＝３０〜６０wt% 、ｂ＝２
０〜５０wt% 、ｃ＝１０〜４０wt%で表される組成範囲
は図２に示される点Ｅ、Ｆ、Ｇ、Ｈ、Ｉ、Ｊを図示のよ
うに結ぶ線で囲まれる領域であり、この領域内で０．３
Oe以下のＨc が得られる。さらに、ａ＝３５〜４５wt%
、ｂ＝２５〜３５wt% 、ｃ＝２５〜３５wt% で表され
る組成範囲は図３に示される点Ｋ、Ｌ、Ｍ、Ｎ、Ｏ、Ｐ
を図示のように結ぶ線で囲まれる領域であり、これらの
領域では０．２Oe以下のＨc が得られる。従って、上記
組成式において、ａ、ｂ、ｃが大きくなりすぎても小さ
くなりすぎても低Ｈc は得られにくくなる。Further, the above a = 30 to 60 wt% and b = 2
The composition range represented by 0 to 50 wt% and c = 10 to 40 wt% is a region surrounded by a line connecting points E, F, G, H, I, and J shown in FIG. 0.3 in area
Hc below Oe is obtained. Furthermore, a = 35 to 45 wt%
, B = 25 to 35 wt%, c = 25 to 35 wt% is the composition range represented by points K, L, M, N, O and P shown in FIG.
Is a region surrounded by a line connecting them as shown in the figure, and Hc of 0.2 Oe or less is obtained in these regions. Therefore, in the above composition formula, it is difficult to obtain low Hc when a, b, and c are too large or too small.
【００２８】本発明の軟磁性薄膜は、電気めっき法によ
り作製することが好ましく、めっき浴組成やめっき条件
などを選択することによって、上記の膜特性を実現する
ことができる。また量産性に優れる。さらに、本発明に
用いるめっき浴は安定性が良好である。The soft magnetic thin film of the present invention is preferably produced by an electroplating method, and the above film characteristics can be realized by selecting the plating bath composition, plating conditions and the like. It also excels in mass productivity. Further, the plating bath used in the present invention has good stability.
【００２９】なお、特開昭６４−８６０５号公報の第３
表には、スパッタ法により形成された厚さ１．９μm の
Ｆｅ30Ｃｏ40Ｎｉ30膜が記載されている。この膜はｆｃ
ｃ単相であるが、Ｉ（２００）／Ｉ（１１１）は約０．
２２であって、本発明範囲を外れている。同公報の第１
表には、同組成の薄膜の保磁力が０．４２ Oe であるこ
とが記載されているが、この値は本発明における同様な
組成の薄膜に比べ、高い。The third method disclosed in Japanese Laid-Open Patent Publication No. 64-8605.
In the table, a 1.9 μm thick Fe 30 Co 40 Ni 30 film formed by the sputtering method is described. This film is fc
Although it is a single phase of c, I (200) / I (111) is about 0.
22 which is outside the scope of the present invention. First of the same publication
Although the table shows that the coercive force of the thin film having the same composition is 0.42 Oe, this value is higher than that of the thin film having the same composition in the present invention.
【００３０】後述するように、本発明ではｆｃｃ単相の
膜に熱処理を施して微量のｂｃｃ相を析出させることに
より、さらに低い保磁力とすることができるが、同公報
にも３５０℃で１時間のアニールを施すことが記載され
ている。しかし、同公報には、アニールによりｂｃｃ相
が析出することも保磁力が低くなることも記載されてい
ない。同公報には、アニール前後の平均結晶粒径および
保磁力の変化が第４図（Ａ）および第４図（Ｂ）に示さ
れているが、アニール前に約０．４ Oe であった保磁力
がアニール後にはかえって増加している。同公報におい
てアニールにより保磁力が低下しているのは、スパッタ
法により形成された薄膜の結晶粒径が比較的大きいため
と考えられる。As will be described later, in the present invention, an even lower coercive force can be obtained by subjecting the fcc single-phase film to a heat treatment to precipitate a trace amount of the bcc phase. It is described that a time anneal is applied. However, the publication does not disclose that the bcc phase is precipitated or the coercive force is lowered by annealing. The publication shows changes in average crystal grain size and coercive force before and after annealing in FIGS. 4 (A) and 4 (B). The magnetic force rather increases after annealing. It is considered that the coercive force is decreased by annealing in the same publication because the crystal grain size of the thin film formed by the sputtering method is relatively large.
【００３１】また、同公報第３表にはＦｅ30Ｃｏ40Ｎｉ
30膜とＦｅ86Ｓｉ14膜とを各２００層積層した多層膜が
記載されている。この多層膜では、Ｉ（２００）／Ｉ
（１１１）が約０．１５となり、アニール後には約０．
１２となることが開示されているが、製造の容易な単層
膜においてＩ（２００）／Ｉ（１１１）≦０．２が得ら
れている例はない。Further, in Table 3 of the same publication, Fe 30 Co 40 Ni is shown.
A multilayer film in which 200 films each of 30 films and Fe 86 Si 14 films are laminated is described. In this multilayer film, I (200) / I
(111) becomes about 0.15, which is about 0.1 after annealing.
However, there is no example in which I (200) / I (111) ≦ 0.2 is obtained in a single layer film that is easy to manufacture.
【００３２】また、特開平２−６８９０６号公報の実施
例にはｆｃｃ構造の（１１１）面を優先的に面配向させ
た電着膜が開示されている。しかし、本発明のものとは
面配向において異なるため、本発明のような低保磁力は
実現できない。また、同公報には（１１１）面と（２０
０）面とを優先的に配向させたスパッタ蒸着膜も開示さ
れているが、スパッタ蒸着法によるためか、あるいは面
配向比が本発明の範囲外であるためか、本発明と異な
り、良好な特性が得られないことが記載されている。Further, an example of Japanese Patent Application Laid-Open No. 2-68906 discloses an electrodeposition film in which the (111) plane of the fcc structure is preferentially plane-oriented. However, since the plane orientation is different from that of the present invention, the low coercive force as in the present invention cannot be realized. Further, in the publication, (111) plane and (20
Although a sputter-deposited film in which the (0) plane is preferentially oriented is also disclosed, it is different from the present invention, probably because of the sputter-deposition method or because the plane orientation ratio is outside the range of the present invention. It is described that the characteristics cannot be obtained.
【００３３】また、米国特許第５０１１５８１号（特開
平２−１３８７１６号）では、結晶構造や面配向につい
ては何ら示唆されておらず、本発明のような低保磁力は
実現できない。Further, US Pat. No. 5,011,581 (Japanese Unexamined Patent Publication No. Hei 2-138716) does not suggest any crystal structure or plane orientation, and the low coercive force as in the present invention cannot be realized.
【００３４】従って、本発明の効果は、上記の膜組成、
結晶構造および面配向のすべての要件を満足したとき得
られるものであり、いずれか１つの要件が欠落しても得
られるものではない。Therefore, the effect of the present invention is that the above film composition,
It is obtained when all the requirements of the crystal structure and the plane orientation are satisfied, and it is not obtained even if any one of the requirements is omitted.
【００３５】本発明の軟磁性薄膜は、前記のとおり、パ
ーマロイを下地膜とし、電気めっき法により作製するこ
とが好ましい。このとき用いるめっき浴にはＣｏイオ
ン、Ｆｅイオン、Ｎｉイオンが含有される。めっき浴中
におけるＣｏイオン、ＦｅイオンおよびＮｉイオンの濃
度は目的とする膜組成等に応じ適宜選択すればよく、通
常、Ｃｏイオン、Ｆｅイオン、Ｎｉイオンの濃度は、い
ずれも、各々０．０１モル／リットル〜溶解限度までと
することが好ましい。各金属イオンの濃度が低くなる
と、金属の析出速度が低下しやすく、実用的でない。Ｃ
ｏ、Ｆｅ、Ｎｉの各イオンの供給源は、硫酸塩、スルフ
ァミン酸塩、酢酸塩、硝酸塩等の水溶性の塩から選択す
ることが好ましく、安価であることから特に硫酸塩を用
いることが好ましい。また、ＣｏイオンおよびＦｅイオ
ンは、金属をめっき浴中に浸漬して自然溶解させたり、
電解により陽極を溶解させることにより供給することも
できる。As described above, the soft magnetic thin film of the present invention is preferably produced by an electroplating method using permalloy as a base film. The plating bath used at this time contains Co ions, Fe ions, and Ni ions. The concentrations of Co ions, Fe ions and Ni ions in the plating bath may be appropriately selected according to the intended film composition and the like. Usually, the concentrations of Co ions, Fe ions and Ni ions are each 0.01 It is preferable that the amount is from mol / liter to the solubility limit. When the concentration of each metal ion is low, the metal deposition rate tends to decrease, which is not practical. C
The supply source of each ion of o, Fe, and Ni is preferably selected from water-soluble salts such as sulfate, sulfamate, acetate, and nitrate. It is particularly preferable to use sulfate because it is inexpensive. . In addition, Co ions and Fe ions may be prepared by immersing a metal in a plating bath to spontaneously dissolve it.
It can also be supplied by dissolving the anode by electrolysis.
【００３６】めっき浴のｐＨは２〜１０、特に２．５〜
２．９とすることが好ましく、浴温度は１０〜８０℃、
特に３５〜４５℃とすることが好ましい。めっき浴のｐ
Ｈおよび温度を上記範囲とすることにより、良好なめっ
き膜を得ることができる。これに対し、ｐＨが低くなる
と金属の析出速度が低下し、ｐＨが高くなるとアンモニ
アガスの発生等により作業環境が悪くなる。また、浴温
度が低くなると金属の析出速度が低下し、浴温度が高く
なると浴の安定性が得られない。The pH of the plating bath is 2-10, especially 2.5-.
2.9 is preferable, the bath temperature is 10 to 80 ° C.,
It is particularly preferable to set the temperature to 35 to 45 ° C. Plating bath p
By setting H and temperature within the above ranges, a good plated film can be obtained. On the other hand, when the pH is low, the metal deposition rate is low, and when the pH is high, the working environment is deteriorated due to the generation of ammonia gas and the like. Further, when the bath temperature is low, the metal deposition rate is low, and when the bath temperature is high, the stability of the bath cannot be obtained.
【００３７】めっき浴中には、有機光沢剤を含有させて
もよい。有機光沢剤としてはサッカリンが好ましい。添
加量は０．５グラム／リットル以上とすれば十分である
が、使用中の消耗等を考慮して１〜６グラム／リットル
とすることが好ましい。めっき浴中には、この他、ラウ
リル硫酸ナトリウム等の界面活性剤、ホウ酸、塩化アン
モニウム等の通常の電気めっき浴に添加する成分を適宜
含有させてもよい。また、適宜、安定化剤として有機酸
イオン、還元剤、キレート剤等を添加してもよい。な
お、一般の条件では３価のＦｅイオンは沈澱を生じ好ま
しくないが、クエン酸、酒石酸等の安定剤ないしキレー
ト剤（錯体形成剤）を添加した場合は沈澱を生じないば
かりでなく、Ｈc 低下に効果があるため、むしろ３価の
Ｆｅイオンを浴中に存在させる方が好ましい。An organic brightener may be contained in the plating bath. Saccharin is preferred as the organic brightener. Although it is sufficient to add 0.5 g / liter or more, it is preferably 1 to 6 g / liter in consideration of consumption during use. In addition to the above, the plating bath may appropriately contain a surfactant such as sodium lauryl sulfate and the like, and components such as boric acid and ammonium chloride to be added to a usual electroplating bath. Further, an organic acid ion, a reducing agent, a chelating agent or the like may be added as a stabilizer as appropriate. Under normal conditions, trivalent Fe ions cause precipitation, which is not preferable. However, when a stabilizer such as citric acid or tartaric acid or a chelating agent (complex forming agent) is added, precipitation does not occur and the Hc is lowered. It is more preferable to allow trivalent Fe ions to be present in the bath because it has an effect on.
【００３８】なお、連続フィルタリングによりめっき浴
中の微粒子や水酸化物を取り除いてもよい。Fine particles and hydroxides in the plating bath may be removed by continuous filtering.
【００３９】陽極は、微粒子除去の観点からは不溶性の
ＴｉＰｔ、フェライト電極が好ましい。しかし、陽極に
おいて酸化反応が起こるので、例えばイオン交換膜によ
り陰極部と分離することが望ましい。The anode is preferably an insoluble TiPt or ferrite electrode from the viewpoint of removing fine particles. However, since an oxidation reaction occurs at the anode, it is desirable to separate it from the cathode part by, for example, an ion exchange membrane.
【００４０】成膜時の電流密度は、０．５〜４．０A/dm
2 とすることが好ましく、さらには０．５〜２A/dm2 と
することが好ましい。電流密度を上記範囲とすることに
よって、良好なめっき膜を得ることができる。これに対
し、電流密度が小さくなると金属の析出速度が低下し、
電流密度が大きくなると膜中の金属粒子の粒子サイズが
増大しＨc が低下する。直流以外にもパルス電解や陰極
溶解まで行なう交流併用型も可能である。The current density during film formation is 0.5 to 4.0 A / dm.
It is preferably 2 and more preferably 0.5 to 2 A / dm 2 . By setting the current density within the above range, a good plated film can be obtained. On the other hand, when the current density decreases, the metal deposition rate decreases,
When the current density increases, the particle size of the metal particles in the film increases and Hc decreases. In addition to direct current, it is also possible to use an alternating current combined type that performs pulse electrolysis and cathode dissolution.
【００４１】めっき浴の溶媒としては、通常の水の他に
非水系溶媒、例えばメチルアルコール、ジメチルホルム
アミド、エチルアルコール、プロピレンカーバイド、溶
融塩等も使用可能である。As the solvent for the plating bath, in addition to ordinary water, non-aqueous solvents such as methyl alcohol, dimethylformamide, ethyl alcohol, propylene carbide and molten salt can be used.
【００４２】本発明の軟磁性薄膜では、Ｃｏ、Ｆｅ、Ｎ
ｉの一部を置換する形で、Ｃｕ、Ｃｒ、Ｓｎ、Ｒｈ、Ｐ
ｄ、Ｍｎ、Ｐ、Ｂ、Ｚｎ、Ｓｎ、Ｐｔ等から選択された
１種以上の元素を含有させてもよい。含有量は全体の３
wt% 以下とすることが好ましい。In the soft magnetic thin film of the present invention, Co, Fe, N
Cu, Cr, Sn, Rh, P by substituting a part of i
One or more elements selected from d, Mn, P, B, Zn, Sn, Pt and the like may be contained. The total content is 3
It is preferably set to wt% or less.
【００４３】なお、膜中にはＣ、Ｓが微量含有されるこ
とがあるが、これらのものは磁気特性に大きな影響を与
えるので注意が必要となる。具体的には共に１０００pp
m 以下であることが望ましい。Although a small amount of C and S may be contained in the film, it should be noted that these substances have a great influence on the magnetic characteristics. Specifically, both are 1000pp
It is desirable to be less than m.
【００４４】本発明の軟磁性薄膜には、目的とする方向
に一軸異方性を付与することが好ましい。一軸異方性付
与の方法としては、磁界中成膜や成膜後の磁界中アニー
ルを用いることができる。磁界中成膜としては、一定の
直流磁界中で成膜する方法が一般的である。しかし、本
発明の軟磁性薄膜では異方性磁界Ｈｋが大きくなりすぎ
ることが多く、高透磁率を得るためにはＨｋの適正化が
要求される場合も多い。Ｈｋの適正化方法としては直交
磁界中成膜や回転磁界中アニール、あるいは直流磁界中
成膜時と直流磁界中アニール時の磁界方向を面内直交さ
せる等の方法が有効である。直交磁界中成膜は、磁場を
コイルで発生させ交互に電流を印加することで可能であ
る。また、永久磁石を用いる場合には陰極を９０°回転
させることで可能となる。アニールの際には飽和磁歪値
が正の方向に増加することが多いので、アニール後の飽
和磁歪値が所望の値となるように成膜を行なうことが好
ましい。薄膜磁気ヘッドのバルクハウゼンノイズを低減
するためには、軟磁性薄膜の飽和磁歪値を小さな負の値
に保つ必要があるとされている。この目的のためには、
成膜時にはやや大きな負の磁歪とし、アニール後に小さ
な負の値となるように設計を行なう。また、複数回の面
内直交方向磁界印加熱処理を行ない、異方性制御を行な
うことも透磁率の向上や磁区構造制御等に有効である。
磁区構造の適性化によりデバイス化した場合のバルクハ
ウセンノイズの低減が可能となる。The soft magnetic thin film of the present invention is preferably provided with uniaxial anisotropy in a desired direction. As a method for imparting uniaxial anisotropy, film formation in a magnetic field or magnetic field annealing after film formation can be used. As the film formation in a magnetic field, a method of forming a film in a constant DC magnetic field is generally used. However, in the soft magnetic thin film of the present invention, the anisotropic magnetic field Hk is often too large, and it is often necessary to optimize Hk in order to obtain high magnetic permeability. As a method of optimizing Hk, it is effective to perform film formation in a perpendicular magnetic field, annealing in a rotating magnetic field, or to make the magnetic field directions at the time of film formation in a DC magnetic field and the annealing in a DC magnetic field in-plane orthogonal. Film formation in an orthogonal magnetic field can be performed by generating a magnetic field with a coil and alternately applying a current. When a permanent magnet is used, it is possible to rotate the cathode by 90 °. Since the saturation magnetostriction value often increases in the positive direction during annealing, it is preferable to form the film so that the saturation magnetostriction value after annealing becomes a desired value. In order to reduce the Barkhausen noise of the thin film magnetic head, it is said that it is necessary to keep the saturation magnetostriction value of the soft magnetic thin film at a small negative value. For this purpose,
The film is designed to have a slightly large negative magnetostriction during film formation and a small negative value after annealing. It is also effective to improve the magnetic permeability and control the magnetic domain structure by performing heat treatment by applying a magnetic field in the in-plane orthogonal direction a plurality of times to control the anisotropy.
By optimizing the magnetic domain structure, it is possible to reduce Barkhausen noise in the device.
【００４５】本発明では、成膜時にｆｃｃ相と微量のｂ
ｃｃ相とを共析させてもよいが、上記した組成範囲にお
いて微量のｂｃｃ相を共析させることは困難なので、通
常、ｆｃｃ単相の薄膜を形成した後、熱処理により微量
のｂｃｃ相を析出させることが好ましい。この熱処理に
は、上記した磁界中アニールを利用することができる。
熱処理の際の保持温度は、好ましくは２４０〜３７０
℃、より好ましくは２８０〜３５０℃である。熱処理温
度が低すぎるとｂｃｃ相が析出せず、高すぎるとｂｃｃ
相の析出量が多くなりすぎて保磁力が高くなってしま
う。熱処理時間は、０．１〜１０時間とすることが好ま
しい。In the present invention, the fcc phase and a small amount of b are deposited during film formation.
Although it may be co-deposited with the cc phase, it is difficult to co-deposit a small amount of bcc phase within the above composition range. Therefore, usually, a small amount of bcc phase is deposited by heat treatment after forming a thin film of fcc single phase. Preferably. The annealing in the magnetic field described above can be used for this heat treatment.
The holding temperature during the heat treatment is preferably 240 to 370.
C., more preferably 280 to 350.degree. If the heat treatment temperature is too low, bcc phase will not precipitate, and if it is too high, bcc
The coercive force becomes high due to the excessive amount of phase precipitation. The heat treatment time is preferably 0.1 to 10 hours.
【００４６】本発明の軟磁性薄膜の厚さは、目的に応じ
て適宜決定すればよく、特に制限はないが、低い保磁力
を得るためには、通常、０．５〜１０μm 程度とするこ
とが好ましく、また、薄膜磁気ヘッドに適用する場合は
０．５〜４．５μm 程度、薄膜トランスに適用する場合
は３〜７μm 程度とすることが好ましい。The thickness of the soft magnetic thin film of the present invention may be appropriately determined according to the purpose and is not particularly limited, but it is usually about 0.5 to 10 μm in order to obtain a low coercive force. Preferably, the thickness is about 0.5 to 4.5 μm when applied to a thin film magnetic head, and about 3 to 7 μm when applied to a thin film transformer.
【００４７】本発明の軟磁性薄膜は、薄膜磁気ヘッドや
薄膜トランスのほか、各種磁気デバイスへの適用が可能
である。また、低保磁力で磁歪（λｓ）が大きいことを
利用した用途が期待される。The soft magnetic thin film of the present invention can be applied to various magnetic devices as well as a thin film magnetic head and a thin film transformer. Further, it is expected to be used for the purpose of utilizing low coercive force and large magnetostriction (λs).
【００４８】[0048]
【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.
【００４９】＜実施例１＞１０mm×１０mm×０．７mm厚
のコーニング７０５９ガラス上に、スパッタ法によりチ
タンを５０A 、さらにパーマロイを５００A 成膜した基
板を使用した。めっき前処理として１Ｎ−塩酸（常温）
に３０秒浸漬し、水洗した後、以下のめっき条件にて軟
磁性薄膜サンプルを成膜した。なお、飽和磁歪値測定用
の試料には、別途０．１mm厚のガラス板に上記基板と同
様の処理を施した基板を使用した。Example 1 A substrate having a thickness of 50 mm of titanium and 500 A of permalloy deposited on a Corning 7059 glass having a thickness of 10 mm × 10 mm × 0.7 mm by a sputtering method was used. 1N-hydrochloric acid (normal temperature) as a pretreatment for plating
After immersing in, for 30 seconds and washing with water, a soft magnetic thin film sample was formed under the following plating conditions. As a sample for measuring the saturation magnetostriction value, a glass plate having a thickness of 0.1 mm was subjected to the same treatment as the above-mentioned substrate.
【００５０】めっき浴中の基板の周囲には銅板で補助カ
ソードを設けた。陰極全体の形状は３インチの円盤状で
あり、陽極には４インチ径のＴｉＰｔ板を使用した。攪
拌には断面が三角形のパドルを用い、６０回／分間の周
期で陰極から２mmの場所でパドル攪拌を行なった。めっ
き液は下記組成とし、その総量は約７リットルとした。Around the substrate in the plating bath, an auxiliary cathode was provided with a copper plate. The whole cathode had a disk shape of 3 inches, and a TiPt plate having a diameter of 4 inches was used for the anode. A paddle having a triangular cross section was used for stirring, and paddle stirring was performed at a position 2 mm from the cathode at a cycle of 60 times / minute. The plating solution had the following composition, and the total amount was about 7 liters.
【００５１】めっき浴組成（１リットル中） 硫酸コバルト・７水塩 ０〜２０g 硫酸ニッケル・６水塩 ０〜５０g 硫酸第一鉄・７水塩 ０〜２０g ホウ酸 ２５g 塩化アンモニウム １５g サッカリン ２g 界面活性剤 微量 Plating bath composition (in 1 liter) Cobalt sulfate heptahydrate 0-20 g Nickel sulfate hexahydrate 0-50 g Ferrous sulfate heptahydrate 0-20 g Boric acid 25 g Ammonium chloride 15 g Saccharin 2 g Surface active Agent
【００５２】めっき浴温度は４０℃、めっき浴のｐＨは
２．８、電流密度は１．５A/dm2 、めっき時間は５分間
とし、３００Oeの直流磁界を印加しながら電気めっきを
行ない、厚さ１．２μm の軟磁性薄膜サンプルを得た。
この場合、浴中の金属イオンの濃度比を変化させること
により種々の組成のものを得た。また一部のサンプルに
ついては、異方性磁界制御を目的に、膜面内でかつ成膜
時の磁界印加方向と直交する方向に２kOe の磁場を印加
しながら、真空熱処理炉にて３００℃で３０分間のアニ
ールを行なった。The plating bath temperature was 40 ° C., the pH of the plating bath was 2.8, the current density was 1.5 A / dm 2 , the plating time was 5 minutes, and electroplating was performed while applying a DC magnetic field of 300 Oe. A soft magnetic thin film sample having a thickness of 1.2 μm was obtained.
In this case, various compositions were obtained by changing the concentration ratio of the metal ions in the bath. In addition, for some samples, in order to control the anisotropic magnetic field, while applying a magnetic field of 2 kOe in the film plane and in the direction orthogonal to the magnetic field application direction during film formation, at 300 ° C in a vacuum heat treatment furnace. Annealing was performed for 30 minutes.
【００５３】得られた各サンプルについて、下記の測定
を行った。The following measurements were performed on each of the obtained samples.
【００５４】（組成）蛍光Ｘ線分析装置、ＩＣＰを用い
て測定した。(Composition) The composition was measured using a fluorescent X-ray analyzer and ICP.
【００５５】（保磁力Ｈc ）交流Ｂ−Ｈトレーサーによ
り６０Hzにて測定した。(Coercive force Hc) Measured at 60 Hz with an AC BH tracer.
【００５６】（飽和磁束密度Ｂs ）ＶＳＭにより測定し
た。(Saturation magnetic flux density Bs) Measured by VSM.
【００５７】（飽和磁歪値）光てこ法により３Hz、１０
０Oeの磁界中で測定した。(Saturation magnetostriction value) 3 Hz, 10 by optical lever method
It was measured in a magnetic field of 0 Oe.
【００５８】（透磁率）８の字コイル法により５MHz 、
３mOe にて測定した。(Permeability) 5 MHz by the figure-eight coil method,
It was measured at 3 mOe.
【００５９】（Ｘ線回折）Ｃｕ−Ｋα線（５０kV，４０
mA）を用い、各面のピークの強度を求めた。(X-ray diffraction) Cu-Kα ray (50 kV, 40
mA) was used to determine the intensity of the peak on each surface.
【００６０】晶相および面配向比とＨc との関係を説明
するために選択したサンプルを、図１に示す。図１か
ら、ｆｃｃ単相で、かつＩ（２００）／Ｉ（１１１）が
０．１〜０．２では、すべて０．５Oe以下のＨc を示
し、０．１５以上ではほとんどが０．３Oe以下のＨc を
示すことがわかる。これに対し、ｂｃｃ相が混在してい
るものや、Ｉ（２００）／Ｉ（１１１）が０．１未満の
サンプルではＨc が高くなっている。なお、図１におい
てＩ（２００）／Ｉ（１１１）が０．１〜０．２のサン
プルは、すべて図２の領域ＡＢＣＤ内の組成を有する。
これらのサンプルにおいて、ｂｃｃ相は、（１１０）
面、（２１１）面および（２２０）面の回折ピークの出
現により確認した。図１にｆｃｃ＋ｂｃｃと表示してあ
るものは、Ｉ（１１０）／Ｉ（１１１）＞０．１であ
る。また、図１にｆｃｃと表示してあるものは、Ｉ（１
１０）／Ｉ（１１１）＝０である。A sample selected for explaining the relationship between the crystal phase and the plane orientation ratio and Hc is shown in FIG. From FIG. 1, it is shown that when the fcc single phase and I (200) / I (111) are 0.1 to 0.2, Hc is 0.5 Oe or less, and most of 0.15 or more is 0.3 Oe or less. It can be seen that the Hc of On the other hand, Hc is high in the case where the bcc phase is mixed and the sample in which I (200) / I (111) is less than 0.1. Note that, in FIG. 1, all the samples with I (200) / I (111) of 0.1 to 0.2 have the composition in the region ABCD of FIG.
In these samples, the bcc phase is (110)
This was confirmed by the appearance of diffraction peaks of the (211) plane and the (211) plane. What is shown as fcc + bcc in FIG. 1 is I (110) / I (111)> 0.1. In addition, what is indicated as fcc in FIG. 1 is I (1
10) / I (111) = 0.
【００６１】また、組成とＨc との関係を説明するため
に選択したサンプルを、図２および図３に示す。図２の
三元組成図には、Ｈc が０．３ Oe 以下のサンプルをプ
ロットし、図２にプロットしたサンプルのうちＨc が
０．２ Oe 以下のものを、図３の三元組成図にプロット
した。図２および図３にはＣｏ＝０のサンプルもプロッ
トされているが、これらはパーマロイ組成であり、Ｂs
が１０kG未満と低かった。一方、３成分系である本発明
のサンプルは、Ｂs が１３〜２０kGと極めて高かった。Samples selected to explain the relationship between composition and Hc are shown in FIGS. 2 and 3. In the ternary composition diagram of FIG. 2, a sample having Hc of 0.3 Oe or less is plotted. Of the samples plotted in FIG. 2, one having Hc of 0.2 Oe or less is plotted in the ternary composition diagram of FIG. Plotted. The Co = 0 sample is also plotted in FIGS. 2 and 3, but these have a permalloy composition and Bs
Was as low as less than 10 kG. On the other hand, the sample of the present invention, which is a three-component system, had an extremely high Bs of 13 to 20 kG.
【００６２】図３にプロットした本発明のサンプルの一
例について、詳しい特性を以下に示す。Detailed characteristics of an example of the sample of the present invention plotted in FIG. 3 are shown below.
【００６３】膜組成 Ｃｏ＝４０wt% 、Ｆｅ＝２８wt%
、Ｎｉ＝３２wt%結晶相 ｆｃｃ相＋微量のｂｃｃ相面配向比 Ｉ（２００）／Ｉ（１１１）＝０．１９、Ｉ
（１１０）／Ｉ（１１１）＝０アニール後の磁気特性 Ｈc ＝０．０５Oe、Ｂs ＝１７
kG、Ｈｋ＝５Oe、μ＝３５００ なお、ｂｃｃ相は、加速電圧２００kV、制限視野５μm
の電子線回折により確認した。 Film composition Co = 40 wt%, Fe = 28 wt%
, Ni = 32 wt% crystalline phase fcc phase + bcc phase plane orientation ratio I (200) of the trace / I (111) = 0.19, I
(110) / I (111) = 0 Magnetic property after annealing Hc = 0.05 Oe, Bs = 17
kG, Hk = 5 Oe, μ = 3500 Note that the bcc phase has an acceleration voltage of 200 kV and a limited field of view of 5 μm.
Was confirmed by electron diffraction.
【００６４】上記サンプル中のＣ含有量は８５０ppm 、
Ｓ含有量は５５０ppm であった。The C content in the above sample was 850 ppm,
The S content was 550 ppm.
【００６５】＜実施例２＞Ｃｏ＝３８wt% 、Ｆｅ＝２８
wt% 、Ｎｉ＝３４wt% を含む薄膜サンプルを実施例１と
同様にして形成した。次いで、表１に示す保持温度でア
ニールを施した。保持温度以外のアニール条件は、実施
例１と同様とした。アニール後の各サンプルについてＸ
線回折を行ない、Ｉ（２００）／Ｉ（１１１）およびＩ
（１１０）／Ｉ（１１１）を求め、また、電子線回折を
行なって、ｂｃｃ相の有無を調べた。Ｘ線回折および電
子線回折の条件は、実施例１と同様とした。さらに、こ
れらのサンプルのＨc を測定した。なお、比較のため
に、アニールを施さなかったサンプルについても同様な
測定を行なった。結果を表１に示す。<Example 2> Co = 38 wt%, Fe = 28
A thin film sample containing wt% and Ni = 34 wt% was formed in the same manner as in Example 1. Then, annealing was performed at the holding temperature shown in Table 1. The annealing conditions other than the holding temperature were the same as in Example 1. X for each sample after annealing
Line diffraction was performed and I (200) / I (111) and I
(110) / I (111) was determined, and electron diffraction was performed to examine the presence or absence of the bcc phase. The conditions of X-ray diffraction and electron diffraction were the same as in Example 1. Furthermore, Hc of these samples was measured. For comparison, the same measurement was performed on a sample that was not annealed. The results are shown in Table 1.
【００６６】[0066]
【表１】 [Table 1]
【００６７】表１から、Ｘ線回折においてＩ（１１０）
／Ｉ（１１１）＝０となりｆｃｃ単相と判断されるもの
でも、電子線回折によりｆｃｃ＋ｂｃｃであることが確
認できることがわかる。そして、ｂｃｃ相が存在し、か
つＩ（１１０）／Ｉ（１１１）≦０．１である場合、極
めて低いＨc が得られることがわかる。From Table 1, I (110) in X-ray diffraction
It can be seen that electron diffraction also confirms that fcc + bcc is obtained even when the / f (111) = 0 and fcc single phase is determined. It can be seen that when the bcc phase is present and I (110) / I (111) ≦ 0.1, an extremely low Hc is obtained.
【００６８】[0068]
【発明の効果】本発明によれば、低Ｈc で高Ｂs の軟磁
性薄膜が得られる。According to the present invention, a soft magnetic thin film having low Hc and high Bs can be obtained.
【図１】結晶相および面配向比に対するＨc の依存性を
示すグラフである。FIG. 1 is a graph showing the dependence of Hc on the crystal phase and the plane orientation ratio.
【図２】低Ｈc が得られる膜組成の範囲を示す三元組成
図である。FIG. 2 is a ternary composition diagram showing a range of film composition that can obtain low Hc.
【図３】低Ｈc が得られる膜組成の範囲を示す三元組成
図である。FIG. 3 is a ternary composition diagram showing a range of film composition that can obtain low Hc.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 佐藤 雄一 東京都中央区日本橋一丁目13番１号 ティ ーディーケイ株式会社内 ─────────────────────────────────────────────────── ─── Continued Front Page (72) Inventor Yuichi Sato 1-13-1 Nihonbashi, Chuo-ku, Tokyo TDC Corporation
Claims (13)
晶相からなり、Ｘ線回折における面心立方晶（２００）
面のピーク強度および面心立方晶（１１１）面のピーク
強度をそれぞれＩ（２００）およびＩ（１１１）とした
とき、 ０．１≦Ｉ（２００）／Ｉ（１１１）≦０．２ であることを特徴とする軟磁性薄膜。1. A face-centered cubic crystal (200) in X-ray diffraction, which contains Co, Ni, and Fe and has a face-centered cubic phase.
When the peak intensity of the plane and the peak intensity of the face-centered cubic (111) plane are I (200) and I (111), respectively, 0.1 ≦ I (200) / I (111) ≦ 0.2 A soft magnetic thin film characterized by the above.
晶相を主とし、微量の体心立方晶相を含み、Ｘ線回折に
おける面心立方晶（２００）面のピーク強度、面心立方
晶（１１１）面のピーク強度および体心立方晶（１１
０）面のピーク強度をそれぞれＩ（２００）、Ｉ（１１
１）およびＩ（１１０）としたとき、 Ｉ（２００）／Ｉ（１１１）≧０．１かつ Ｉ（１１０）／Ｉ（１１１）≦０．１ であることを特徴とする軟磁性薄膜。2. A peak intensity of a face-centered cubic (200) plane in X-ray diffraction, containing Co, Ni and Fe, mainly containing a face-centered cubic phase, and containing a trace amount of a body-centered cubic phase, Face-centered cubic (111) plane peak intensity and body-centered cubic (11)
The peak intensities of the 0) plane are I (200) and I (11
1) and I (110), I (200) / I (111) ≧ 0.1 and I (110) / I (111) ≦ 0.1.
には面心立方晶単相であり、熱処理により体心立方晶相
を共析したものである請求項２または３の軟磁性薄膜。4. The soft magnetic thin film according to claim 2, wherein the soft magnetic thin film is formed by electroplating, has a face-centered cubic single phase immediately after formation, and has a body-centered cubic phase co-deposited by heat treatment.
℃である請求項４の軟磁性薄膜。5. The temperature during the heat treatment is 240 to 370.
The soft magnetic thin film according to claim 4, wherein the soft magnetic thin film has a temperature of ° C.
ｂおよびｃは、それぞれＣｏ、ＮｉおよびＦｅの比率
（wt% ）を表し、 ａ＝２８〜７５wt% 、 ｂ＝１６〜６０wt% 、 ｃ＝９〜４２wt% 、および ａ＋ｂ＋ｃ＝１００wt% の関係を満足する。］で表される組成を有する請求項１
ないし５のいずれかの軟磁性薄膜。6. aCo-bNi-cFe [where a,
b and c represent the ratio (wt%) of Co, Ni and Fe, respectively, and satisfy the relations of a = 28 to 75 wt%, b = 16 to 60 wt%, c = 9 to 42 wt%, and a + b + c = 100 wt%. To do. ] The composition represented by
The soft magnetic thin film according to any one of 1 to 5.
ｂおよびｃは、それぞれＣｏ、ＮｉおよびＦｅの比率
（wt% ）を表し、 ａ＝３０〜６０wt% 、 ｂ＝２０〜５０wt% 、 ｃ＝１０〜４０wt% 、および ａ＋ｂ＋ｃ＝１００wt% の関係を満足する。］で表される組成を有する請求項６
の軟磁性薄膜。7. aCo-bNi-cFe [where a,
b and c represent the ratio (wt%) of Co, Ni and Fe, respectively, and satisfy the relationships of a = 30 to 60 wt%, b = 20 to 50 wt%, c = 10 to 40 wt%, and a + b + c = 100 wt%. To do. ] The composition represented by
Soft magnetic thin film.
ｂおよびｃは、それぞれＣｏ、ＮｉおよびＦｅの比率
（wt% ）を表し、 ａ＝３５〜４５wt% 、 ｂ＝２５〜３５wt% 、 ｃ＝２５〜３５wt% 、および ａ＋ｂ＋ｃ＝１００wt% の関係を満足する。］で表される組成を有する請求項７
の軟磁性薄膜。8. aCo-bNi-cFe [where a,
b and c represent the proportions (wt%) of Co, Ni and Fe, respectively, and satisfy the relationships of a = 35-45 wt%, b = 25-35 wt%, c = 25-35 wt%, and a + b + c = 100 wt%. To do. ] It has a composition represented by these.
Soft magnetic thin film.
ンを含有し、ｐＨ２〜１０、温度１０〜８０℃のめっき
浴を用い、電流密度０．５〜４．０A/dm2 の条件で電気
めっき法により作製した請求項１ないし８のいずれかの
軟磁性薄膜。9. An electroplating method using a plating bath containing Co ions, Ni ions and Fe ions and having a pH of 2 to 10 and a temperature of 10 to 80 ° C. and a current density of 0.5 to 4.0 A / dm 2. 9. The soft magnetic thin film according to claim 1, which is produced by.
求項９の軟磁性薄膜。10. The soft magnetic thin film according to claim 9, which is made of permalloy as a base film.
度が１３kG以上である請求項１ないし１０のいずれかの
軟磁性薄膜。11. The soft magnetic thin film according to claim 1, which has a coercive force of 0.5 Oe or less and a saturation magnetic flux density of 13 kG or more.
１の軟磁性薄膜。12. A coercive force of 0.3 Oe or less.
1. Soft magnetic thin film.
２の軟磁性薄膜。13. A coercive force of 0.2 Oe or less.
2. Soft magnetic thin film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23553793A JP3201892B2 (en) | 1993-04-23 | 1993-08-27 | Soft magnetic thin film and magnetic inductive MR head using the same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12084793 | 1993-04-23 | ||
| JP5-120847 | 1993-04-23 | ||
| JP23553793A JP3201892B2 (en) | 1993-04-23 | 1993-08-27 | Soft magnetic thin film and magnetic inductive MR head using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH073489A true JPH073489A (en) | 1995-01-06 |
| JP3201892B2 JP3201892B2 (en) | 2001-08-27 |
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ID=26458353
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23553793A Expired - Fee Related JP3201892B2 (en) | 1993-04-23 | 1993-08-27 | Soft magnetic thin film and magnetic inductive MR head using the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3201892B2 (en) |
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| US6466416B1 (en) | 1999-08-11 | 2002-10-15 | Nec Corporation | Magnetic head, method for making the same and magnetic recording/reproducing device using the same |
| JP2003034891A (en) * | 2001-05-18 | 2003-02-07 | Headway Technologies Inc | Method for manufacturing cobalt iron alloy and plated magnetic thin-film of cobalt iron alloy, and method for manufacturing quaternary alloy and plated magnetic thin-film of cobalt iron molybdenum alloy |
| US6661606B2 (en) | 1995-02-03 | 2003-12-09 | Hitachi, Ltd. | Magnetic disk apparatus with magnetic head having upper and lower magnetic cores of an electroplated thin film |
| US6723449B2 (en) | 2000-12-07 | 2004-04-20 | Hitachi, Ltd. | Structure and plating method of thin film magnetic head and magnetic storage apparatus |
| US6791794B2 (en) | 2000-09-28 | 2004-09-14 | Nec Corporation | Magnetic head having an antistripping layer for preventing a magnetic layer from stripping |
| US6795271B2 (en) | 2000-01-05 | 2004-09-21 | Nec Corporation | Recording head, recording head manufacturing method, combined head and magnetic recording/reproduction apparatus |
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| JP2006210744A (en) * | 2005-01-31 | 2006-08-10 | Alps Electric Co Ltd | Soft magnetic film and magnetic head using it |
| US7267757B2 (en) | 2002-11-01 | 2007-09-11 | Hitachi Global Storage Technologies Japan, Ltd. | Magnetic head utilizing a CoNiFe alloy with 60-80 weight percent Fe and method for production therefor |
| US7679860B2 (en) | 2005-03-09 | 2010-03-16 | Hitachi Global Storage Technologies Netherlands B.V. | Thin film magnetic head with layer having high saturation magnetic flux density, and magnetic storage apparatus |
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| US6661606B2 (en) | 1995-02-03 | 2003-12-09 | Hitachi, Ltd. | Magnetic disk apparatus with magnetic head having upper and lower magnetic cores of an electroplated thin film |
| US6466416B1 (en) | 1999-08-11 | 2002-10-15 | Nec Corporation | Magnetic head, method for making the same and magnetic recording/reproducing device using the same |
| US7023659B2 (en) | 1999-09-30 | 2006-04-04 | Nec Corporation | Magnetic head having an antistripping layer for preventing a magnetic layer from stripping |
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| US7150819B2 (en) | 2000-12-07 | 2006-12-19 | Hitachi Global Storage Technologies Japan, Ltd. | Structure and plating method of thin film magnetic head and magnetic storage apparatus |
| JP2003034891A (en) * | 2001-05-18 | 2003-02-07 | Headway Technologies Inc | Method for manufacturing cobalt iron alloy and plated magnetic thin-film of cobalt iron alloy, and method for manufacturing quaternary alloy and plated magnetic thin-film of cobalt iron molybdenum alloy |
| US7267757B2 (en) | 2002-11-01 | 2007-09-11 | Hitachi Global Storage Technologies Japan, Ltd. | Magnetic head utilizing a CoNiFe alloy with 60-80 weight percent Fe and method for production therefor |
| JP2006210744A (en) * | 2005-01-31 | 2006-08-10 | Alps Electric Co Ltd | Soft magnetic film and magnetic head using it |
| JP4635626B2 (en) * | 2005-01-31 | 2011-02-23 | Ｔｄｋ株式会社 | Method for manufacturing soft magnetic film and method for manufacturing magnetic head |
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