JP2003100515A - Soft magnetic thin film for magnetic core with high saturation magnetization - Google Patents
Soft magnetic thin film for magnetic core with high saturation magnetizationInfo
- Publication number
- JP2003100515A JP2003100515A JP2001331714A JP2001331714A JP2003100515A JP 2003100515 A JP2003100515 A JP 2003100515A JP 2001331714 A JP2001331714 A JP 2001331714A JP 2001331714 A JP2001331714 A JP 2001331714A JP 2003100515 A JP2003100515 A JP 2003100515A
- Authority
- JP
- Japan
- Prior art keywords
- film
- magnetic
- soft magnetic
- saturation magnetization
- magnetic core
- 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- Withdrawn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
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
- H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
- H01F10/12—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
- H01F10/14—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel
- H01F10/147—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel with lattice under strain, e.g. expanded by interstitial nitrogen
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は軟磁性膜に関し、特に５
０Ｇｂｐｉ以上の高密度磁気記録の記録用磁気ヘッドに
好適な高い飽和磁束密度、優れた高周波特性および熱的
安定性を有する磁心用軟磁性膜に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a soft magnetic film, especially 5
The present invention relates to a soft magnetic film for a magnetic core having a high saturation magnetic flux density suitable for a recording magnetic head of high density magnetic recording of 0 Gbpi or more, excellent high frequency characteristics and thermal stability.
【０００２】[0002]
【従来の技術】コンピュータの高性能化に伴い、主な記
録部であるハードディスクの高記録密度化が年４０％以
上の大きさで進んでおり、２，３年後には１００Ｇｂｐ
ｉを超えることが予測されている。このような高い記録
密度を有するハードディスクには大きな保磁力を示す媒
体とこれをオーバーライトするための高い飽和磁化を有
する記録ヘッド用軟磁性材料が要求される。しかし、十
分な特性を有する材料はまだ見出されていない。特に、
近未来の超高密度記録のハードディスク装置では、記録
用ヘッド材料の点で大きな問題になることが考えられ
る。2. Description of the Related Art As the performance of computers has increased, the recording density of hard disks, which are the main recording section, has been increasing at a rate of 40% or more per year, and 100 Gbp after a few years.
It is expected to exceed i. A hard disk having such a high recording density requires a medium having a large coercive force and a soft magnetic material for a recording head having a high saturation magnetization for overwriting the medium. However, a material having sufficient properties has not yet been found. In particular,
In the near future, ultra-high-density recording hard disk devices, it is conceivable that there will be a major problem in terms of recording head materials.
【０００３】一般に、ハードディスク装置の記録用ヘッ
ド材料の飽和磁化は、記録媒体の保磁力の約３倍の大き
さを保有しないと十分にオーバーライトすることが出来
ないことが知られている。１００Ｇｂｐｉの記録密度を
得るためには、７０００Ｏｅ以上の保磁力が媒体に求め
られ、その結果、記録用ヘッド材料には、２．１Ｔ以上
の飽和磁化を有することが求められる。It is generally known that the saturation magnetization of the recording head material of a hard disk drive cannot be sufficiently overwritten unless it has a coercive force of about 3 times the coercive force of the recording medium. In order to obtain a recording density of 100 Gbpi, a coercive force of 7,000 Oe or more is required for the medium, and as a result, the recording head material is required to have a saturation magnetization of 2.1 T or more.
【０００４】最近、大きな飽和磁化を有する高周波軟磁
性材料の研究が盛んに行われており、これまでに数多く
の磁性材料、例えば、Ｔ．Ｏｓａｋａ，Ｍ．Ｔａｋａ
ｉ，Ｋ．Ｈａｙａｓｈｉ，Ｋ．Ｏｈａｓｈｉ，Ｍ．Ｓａ
ｉｔｏ ａｎｄ Ｋ．Ｙａｍａｄａ：Ｎａｔｕｒｅ，３
９２，７９６（１９９８），大沼、李、小林、増本、藤
森：日本応用磁気学会誌、２４，６９１（２０００）が
提案されてきた。しかし、それらの材料のＢｓ値は高々
２．０Ｔであり、現状での書き込み容量には対応できて
いる。しかし、年約４０％の割合で記録密度が上昇して
いる昨今、数年後のハードディスクには、現状の軟磁性
材料では対応できなくなることが考えられ、さらなる大
きな飽和磁化を有する軟磁性材料が要望されている。Recently, high-frequency soft magnetic materials having a large saturation magnetization have been actively researched, and a large number of magnetic materials such as T.W. Osaka, M .; Taka
i, K. Hayashi, K .; Ohashi, M .; Sa
it and K. Yamada: Nature, 3
92, 796 (1998), Onuma, Lee, Kobayashi, Masumoto, Fujimori: Journal of Japan Society for Applied Magnetics, 24, 691 (2000). However, the Bs value of those materials is at most 2.0 T, which is sufficient for the current writing capacity. However, with the recent increase in recording density at a rate of about 40%, it is considered that the current soft magnetic materials will no longer be compatible with hard disks several years later, and soft magnetic materials with even higher saturation magnetization will be used. Is requested.
【０００５】[0005]
【発明が解決しようとする課題】磁性原子中最も大きな
磁化の値を示す材料が純Ｆｅで、その値は２．２Ｔであ
り、また合金ではＦｅ−Ｃｏで、２．４〜２．５Ｔであ
る。その他、Ｆｅにわずかの窒素が入った特殊な構造を
示す物質がさらに大きな磁化を示すとの報告がなされた
が、その真実性は定かではない。そのため、従来から多
くの研究者によって純ＦｅやＦｅＣｏの軟磁性化が試み
られてきたが、まだ成功していない。The material exhibiting the largest magnetization value among the magnetic atoms is pure Fe, which has a value of 2.2T, and the alloy Fe-Co, which has a value of 2.4 to 2.5T. is there. In addition, it was reported that a substance having a special structure, in which Fe contains a small amount of nitrogen, exhibits even larger magnetization, but the truth is not clear. Therefore, many researchers have tried to soften pure Fe and FeCo, but have not succeeded yet.
【０００６】軟磁性化を促進させるためには、材料の磁
気異方性を小さくすることにある。そのためには、結晶
粒径を制御させることと、結晶配向を制御することの２
つの方法が行われている。結晶粒径を制御し、磁気異方
性を分散消滅させた例がアモルファス材料であり、また
ナノ結晶材料である。しかし、これらの場合はいずれも
が微細化、または非晶質化させるために、かなりの量の
非磁性元素を混入させなければならず、そのために、磁
化の大きさが著しく減少してしまう。もう１つの優先結
晶配向を制御することによって異方性を小さくする方法
においても、非磁性元素の混入が必要であり、そのため
Ｂｓは減少し、また組成的に材料がかなり限定される。In order to promote soft magnetization, the magnetic anisotropy of the material should be reduced. For that purpose, it is necessary to control the crystal grain size and the crystal orientation.
One way is done. An example in which the crystal grain size is controlled and the magnetic anisotropy is dispersed and eliminated is an amorphous material or a nanocrystalline material. However, in each of these cases, a considerable amount of a non-magnetic element must be mixed in order to make the particles finer or amorphous, which significantly reduces the magnitude of magnetization. Another method for reducing anisotropy by controlling the preferential crystal orientation also requires the inclusion of a non-magnetic element, which reduces Bs and considerably limits the material compositionally.
【０００７】本発明は前記課題を解決するためになされ
たもので、２．２Ｔ以上の大きな飽和磁化を示す高周波
帯域まで、優れた軟磁性を示す膜を提供することを目的
としている。The present invention has been made to solve the above problems, and an object thereof is to provide a film exhibiting excellent soft magnetism up to a high frequency band exhibiting a large saturation magnetization of 2.2 T or more.
【０００８】[0008]
【課題を解決するための手段】本発明は、上記の事情を
鑑みて鋭意努力した結果、僅かな酸素を含む、極狭い組
成範囲の（Ｆｅ１−ＡＣｏＡ）１００−Ｘ−Ｙ−ＺＭＸ
ＲＹＯＺ膜に、２．２Ｔ以上の大きな飽和磁化を有し、
且つ高周波軟磁気特性をも示す膜が得られることを見出
し、本発明に至ったものである。The present invention has made intensive efforts in view of the above circumstances, and as a result, (Fe 1-A Co A ) 100-XYZ having a very narrow composition range containing a slight amount of oxygen. M X
The R Y O Z film has a large saturation magnetization of 2.2 T or more,
Moreover, they have found that a film exhibiting high-frequency soft magnetic properties can be obtained, and have reached the present invention.
【０００９】本発明の特徴とするところは次の通りであ
る。第１発明は、一般式（Ｆｅ１−ＡＣｏＡ）
１００−Ｘ−Ｙ−ＺＭＸＲＹＯＺで表され、ＭはＺｒ及
びＡｌの１種又は２種の元素であり、ＲはＲｕ，Ｐｄ，
Ｐｔのうちから選択された１種又は２種の元素であり、
Ｏは酸素を表し、且つ組成比Ａ，Ｘ，Ｙ，Ｚは原子比率
で、
０．２５≦Ａ≦０．５
１≦Ｘ≦３
０≦Ｙ≦１
６≦Ｚ≦１０
である組成からなり、体心立方構造の（１１０）面が優
先配向している粒径が４０ｎｍ以下の微結晶で、且つ飽
和磁化２．２Ｔ以上を有することを特徴とする磁心用軟
磁性膜に関する。The features of the present invention are as follows. The first invention is represented by a general formula (Fe 1-A Co A ).
100-X-Y-Z M X R Y O Z , M is one or two elements of Zr and Al, R is Ru, Pd,
One or two elements selected from Pt,
O represents oxygen, and the composition ratios A, X, Y, and Z are atomic ratios, and 0.25 ≦ A ≦ 0.5 1 ≦ X ≦ 3 0 ≦ Y ≦ 16 6 ≦ Z ≦ 10 The present invention relates to a soft magnetic film for a magnetic core, which is characterized in that the (110) plane of the body-centered cubic structure is preferentially oriented and has a crystallite size of 40 nm or less and a saturation magnetization of 2.2 T or more.
【００１０】第２発明は、一般式（Ｆｅ１−ＡＣｏＡ）
１００−Ｘ−Ｙ−ＺＺｒＸＲｕＹＯＺで表され、且つ組
成比Ａ，Ｘ，Ｙ，Ｚは原子比率で、
０．２５≦Ａ≦０．５
１≦Ｘ≦３
０≦Ｙ≦１
６≦Ｚ≦１０
である組成からなり、ＺｒとＯの原子比率が１：２より
も多い酸素を含み、体心立方構造の（１１０）面が優先
配向している粒径が４０ｎｍ以下の微結晶で、且つ飽和
磁化２．２Ｔ以上を有することを特徴とする磁心用軟磁
性膜に関する。The second invention is the general formula (Fe 1-A Co A )
100-X-Y-Z is represented by Zr X Ru Y O Z, and the composition ratio A, X, Y, Z is atomic ratio, 0.25 ≦ A ≦ 0.5 1 ≦ X ≦ 3 0 ≦ Y ≦ The composition is such that 16 ≦ Z ≦ 10, the atomic ratio of Zr and O is greater than 1: 2, and oxygen is included, and the (110) plane of the body-centered cubic structure is preferentially oriented and the particle size is 40 nm or less. The present invention relates to a soft magnetic film for a magnetic core, which is microcrystalline and has a saturation magnetization of 2.2 T or more.
【００１１】第３発明は、一般式（Ｆｅ１−ＡＣｏＡ）
１００−Ｘ−Ｙ−ＺＡｌＸＲｕＹＯＺで表され、且つ組
成比Ａ，Ｘ，Ｙ，Ｚは原子比率で、
０．２５≦Ａ≦０．５
１≦Ｘ≦２．４
０≦Ｙ≦１
２≦Ｚ≦６
である組成からなり、ＡｌとＯの原子比率が２：３より
も多い酸素を含み、体心立方構造の（１１０）面が優先
配向している粒径が４０ｎｍ以下の微結晶で、且つ飽和
磁化２．２Ｔ以上を有することを特徴とする磁心用軟磁
性膜に関する。The third aspect of the present invention is the general formula (Fe 1-A Co A )
100-X-Y-Z is represented by Al X Ru Y O Z, and the composition ratio A, X, Y, Z is atomic ratio, 0.25 ≦ A ≦ 0.5 1 ≦ X ≦ 2.4 0 ≦ The composition is such that Y ≦ 12 ≦ Z ≦ 6, the atomic ratio of Al to O is larger than 2: 3, and oxygen is included, and the (110) plane of the body-centered cubic structure has a preferentially oriented grain size of 40 nm. The present invention relates to a soft magnetic film for a magnetic core, which is characterized by the following crystallites and having a saturation magnetization of 2.2 T or more.
【００１２】第４発明は、５０Ｏｅ以上の一方向磁界中
で成膜することにより、５Ｏｅ以上の一軸磁気異方性を
付与したことを特徴とする請求項１ないし３のいずれか
１項に記載の磁心用軟磁性膜に関する。The fourth invention is characterized in that uniaxial magnetic anisotropy of 5 Oe or more is imparted by forming the film in a unidirectional magnetic field of 50 Oe or more. The present invention relates to a soft magnetic film for magnetic core.
【００１３】第５発明は、１００℃以上６００℃以下の
温度で、且つ一方向磁界中で焼鈍することを特徴とする
請求項１ないし４のいずれか１項に記載の磁心用軟磁性
膜に関する。A fifth aspect of the present invention relates to a soft magnetic film for a magnetic core according to any one of claims 1 to 4, which is annealed at a temperature of 100 ° C. or more and 600 ° C. or less and in a unidirectional magnetic field. .
【００１４】[0014]
【作用】本発明の軟磁性膜は、粒径が４０ｎｍ以下のＦ
ｅＣｏＲの金属粒子で構成されており、その中に微細な
Ｍ−Ｏ酸化物が少量分散している形態になっている。そ
のために、個々の粒子が持っている結晶磁気異方性が大
きくとも、ランダムに配向しているために膜全体の磁気
異方性は小さくなる。ＦｅＣｏ合金においてＦｅとＣｏ
との組成比（原子％）が（７５：２５）〜（５０：５
０）の範囲のときに２．４Ｔ以上の大きなＢｓを示す。
Ｍ−Ｏ酸化物が１３％（原子％）より多くなると軟磁性
は促進するが、Ｂｓは２．２Ｔ以下となる。一方、７％
より少ない膜では、Ｂｓは２．４Ｔに近い値を示すが、
金属粒子径が大きくなり、保磁力が大きくなってしま
う。Ｒ量が１％を超えるとＢｓの減少をもたらすが、そ
れ以内であれば、成膜中にまたは熱処理中に一方向の磁
界を印加することにより、膜に一軸磁気異方性を付与さ
せ、高周波軟磁気特性を向上させることが出来る。Ｍ元
素がＦｅＣｏ中に存在するとＢｓが小さくなるばかり
か、粒子の結晶配向をも変え、軟磁気特性を示さなくな
る。そのため、Ｍ−Ｏ中の酸素濃度がＭ−Ｏの化合物の
化学量論比、例えばＺｒ−Ｏ系ではＺｒＯ２ 、またＡ
ｌ−Ｏ系ではＡｌ２Ｏ３、よりも多いことが望まれ、そ
の組成ではマトリックス中にＭは含まなくなる。The soft magnetic film of the present invention has an F particle size of 40 nm or less.
It is composed of eCoR metal particles, in which a small amount of fine MO oxide is dispersed. Therefore, even if the crystal magnetic anisotropy of each grain is large, the magnetic anisotropy of the entire film is small because the grains are randomly oriented. Fe and Co in FeCo alloy
The composition ratio (atomic%) of (75:25) to (50: 5)
In the range of 0), a large Bs of 2.4 T or more is shown.
When the M-O oxide content is more than 13% (atomic%), soft magnetism is promoted, but Bs is 2.2T or less. On the other hand, 7%
For smaller films, Bs is close to 2.4T,
The metal particle diameter becomes large and the coercive force also becomes large. When the amount of R exceeds 1%, Bs is reduced, but if the amount is less than 1%, a uniaxial magnetic anisotropy is imparted to the film by applying a unidirectional magnetic field during film formation or during heat treatment, The high frequency soft magnetic characteristics can be improved. When the M element is present in FeCo, not only Bs becomes small, but also the crystal orientation of the particles is changed and the soft magnetic property is not exhibited. Therefore, the stoichiometric ratio of the compound in which the oxygen concentration in M-O is M-O, such as ZrO 2 in the Zr-O system, or A
More than Al 2 O 3 is desired in the l-O system, and the composition does not include M in the matrix.
【００１５】一方、基板ホールダー付近に５０Ｏｅ以上
の一方向磁界が印加するように、例えば永久磁石等をセ
ットし成膜すると、膜中に５Ｏｅ以上の異方性磁界を付
与させることが出来、膜の高周波軟磁気特性が向上する
のである。同様の効果は成膜した膜を一方向磁界中で焼
鈍することによっても得られる。ただし、このときの温
度が１００℃以下では低すぎて、異方性磁界が充分付与
されず、６００℃以上では結晶粒が成長してしまい、軟
磁性膜が得られなくなってしまうので、好ましくない。
また熱処理することにより、内部応力が緩和し、磁気特
性の改善が同時になされる。On the other hand, when a permanent magnet or the like is set and deposited so that a unidirectional magnetic field of 50 Oe or more is applied near the substrate holder, an anisotropic magnetic field of 5 Oe or more can be imparted to the film. The high frequency soft magnetic characteristics of are improved. The same effect can be obtained by annealing the formed film in a unidirectional magnetic field. However, if the temperature at this time is 100 ° C. or lower, the anisotropic magnetic field is not sufficiently applied, and if the temperature is 600 ° C. or higher, crystal grains grow and a soft magnetic film cannot be obtained. .
The heat treatment also relaxes the internal stress and improves the magnetic properties at the same time.
【００１６】（Ｆｅ１−ＡＣｏＡ）１００−Ｘ−Ｙ−Ｚ
ＭＸＲＹＯＺ体心立方構造の薄膜においては、（１１
０）面配向膜は面内磁化膜となり、（１１１）面配向膜
は垂直磁化膜となる。本発明においては、粒径が４０ｎ
ｍ以下の（１１０）面を優先配向とする薄膜を意図的に
作製し、この（１１０）面薄膜の成膜中または熱処理中
に、５０Ｏｅ以上の一方向磁界を印加することにより、
磁界方向が容易磁化方向となり、一軸異方性を有した
（１１０）面配向の薄膜となり、飽和磁化が２．２Ｔ以
上で優れた高周波特性の磁心用軟磁性膜が得られたので
ある。(Fe 1-A Co A ) 100-XYZ
In the thin film of the M X R Y O Z body-centered cubic structure, (11
The (0) plane orientation film becomes an in-plane magnetization film, and the (111) plane orientation film becomes a perpendicular magnetization film. In the present invention, the particle size is 40n
By intentionally producing a thin film in which the (110) plane of m or less is preferentially oriented and applying a unidirectional magnetic field of 50 Oe or more during film formation or heat treatment of the (110) plane thin film,
The magnetic field direction was the easy magnetization direction, a (110) plane oriented thin film having uniaxial anisotropy was obtained, and a soft magnetic film for a magnetic core having a saturation magnetization of 2.2 T or more and excellent high frequency characteristics was obtained.
【００１７】[0017]
【実施例】本発明を具体的に図を用いてさらに詳しく説
明する。
〔実施例〕薄膜の作製と評価
ＲＦマグネトロンスパッタ装置を用い、（Ｆｅ．６５Ｃ
ｏ．３５）９６Ｚｒ４（原子％）ターゲットを用いて、
（Ａｒ＋Ｏ２）混合ガス雰囲気中での反応スパッタ法に
より、ＦｅＣｏ−Ｚｒ−Ｏ薄膜を作製した。膜厚の制御
は成膜時間を加減することによって行い、約１μｍにな
るように調整した。基板には、約０．５ｍｍ厚のコーニ
ング社製＃７０５９ガラスを用いた。成膜時のスパッタ
圧力は２〜８ｍＴｏｒｒで、スパッタ電力は１００〜５
００Ｗである。また成膜時の基板ホールダーには、１０
０Ｏｅの一方向の磁界が試料に印加されるように、一対
の永久磁石をセットした。作製した薄膜試料には、１０
０〜６００℃の温度で種々の熱処理を施した。The present invention will be described in more detail with reference to the drawings. [Example] Fabrication and evaluation of thin film Using an RF magnetron sputtering device, (Fe .65 C
o . 35 ) 96 Zr 4 (atomic%) target,
The (Ar + O 2) reactive sputtering in a mixed gas atmosphere to prepare a FeCo-Zr-O thin film. The film thickness was controlled by adjusting the film forming time, and was adjusted to be about 1 μm. Corning # 7059 glass having a thickness of about 0.5 mm was used for the substrate. The sputtering pressure during film formation is 2 to 8 mTorr, and the sputtering power is 100 to 5
It is 00W. Also, the substrate holder during film formation has 10
A pair of permanent magnets was set so that a unidirectional magnetic field of 0 Oe was applied to the sample. The thin film sample produced has 10
Various heat treatments were performed at a temperature of 0 to 600 ° C.
【００１８】前記のようにして作製した薄膜試料は、試
料振動型磁力計を用いて磁化曲線を、また直流４端子法
により電気比抵抗を測定した。膜組成は、エネルギー分
散型分光分析法（ＥＤＳ）と（ＥＰＭＡ）によって決定
した。膜の構造は、Ｃｕ−Ｋα線を用いたＸ線回折法に
よって決定した。前記の方法で作製した薄膜とその飽和
磁化（Ｂｓ）の値を図１に示す。With respect to the thin film sample manufactured as described above, the magnetization curve was measured using a sample vibrating magnetometer, and the electrical resistivity was measured by the direct current 4-terminal method. The film composition was determined by energy dispersive spectroscopy (EDS) and (EPMA). The structure of the film was determined by the X-ray diffraction method using Cu-Kα ray. FIG. 1 shows the thin film produced by the above method and its saturation magnetization (Bs) value.
【００１９】図中、白丸は面内磁化膜を表し、黒丸は面
内磁化成分と面に垂直な方向に容易磁化を示す成分とが
混在する膜を表す。図から明らかなように、磁気特性は
ＦｅＣｏ−ＺｒＯ２線で２分割される。ＺｒＯ２よりも
酸素の少ない組成の膜では垂直磁化膜が、酸素の多い組
成の膜では面内膜が実現する。膜中の酸素量の増加とと
もにＺｒは選択的に酸化される。ＺｒＯ２よりも酸素の
少ない組成域では、マトリックスはＦｅＣｏＺｒになっ
ており、またその粒界に微小なＺｒＯが析出している構
造になっており、且つＦｅＣｏＺｒが（１１１）面に優
先配向している（図２−Ａ）ために、垂直磁化成分が現
れる。一方、ＺｒＯ２よりも酸素の多い組成の膜では、
全てのＺｒは酸化されるため、マトリックスはＦｅＣｏ
のみになり、膜構造はＦｅＣｏ中に微小なＺｒＯが析出
している構造になり、且つＦｅＣｏが（１１０）面に優
先配向する（図２−Ｂ）ために面内磁化膜が実現する。
さらに酸素濃度の高い組成域ではＦｅＣｏも酸化されて
しまうために、垂直磁化膜になってしまうのである。In the figure, white circles represent in-plane magnetized films, and black circles represent films in which in-plane magnetized components and components exhibiting easy magnetization in the direction perpendicular to the plane are mixed. As is clear from the figure, the magnetic characteristic is divided into two by the FeCo-ZrO 2 line. A perpendicularly magnetized film is realized with a film having a composition with less oxygen than ZrO 2 , and an in-plane film is realized with a film having a composition with more oxygen. Zr is selectively oxidized as the amount of oxygen in the film increases. In the composition range in which oxygen is smaller than that of ZrO 2 , the matrix is FeCoZr, and the structure is such that minute ZrO is precipitated in the grain boundaries, and FeCoZr is preferentially oriented in the (111) plane. (FIG. 2-A), a perpendicular magnetization component appears. On the other hand, for a film having a composition with more oxygen than ZrO 2 ,
Since all Zr is oxidized, the matrix is FeCo
The film structure becomes a structure in which minute ZrO is precipitated in FeCo, and FeCo is preferentially oriented to the (110) plane (FIG. 2-B), so that an in-plane magnetized film is realized.
Further, FeCo is also oxidized in the composition region where the oxygen concentration is high, so that it becomes a perpendicular magnetization film.
【００２０】Ｚｒ濃度の高い領域の飽和磁化はＺｒ量と
ともに減少し、一方酸素濃度の少ない領域では、酸素濃
度の増加とともに減少するような組成依存性を示す。そ
のため、ＦｅＣｏ−ＺｒＯ２組成付近にＢｓのピークを
持つような組成依存性を示し、低Ｚｒ濃度の組成域では
９０（原子％）ＦｅＣｏでも２．２Ｔ以上のＢｓを示す
膜が得られる。The saturation magnetization in the high Zr concentration region decreases with the Zr amount, while in the low oxygen concentration region, the saturation magnetization decreases with the increase in the oxygen concentration. Therefore, a film having a composition dependency such that a Bs peak is present in the vicinity of the FeCo-ZrO 2 composition, and a Bs of 2.2 T or more can be obtained even with 90 (atomic%) FeCo in the low Zr concentration composition range.
【００２１】図３には、ＦｅＣｏ−Ｚｒ−Ｏ膜の保磁力
の組成依存性を示す。図から明らかなように、ＦｅＣｏ
−ＺｒＯ２組成に沿ってＨｃの小さな組成域が存在する
ことを見出した。Ｈｃが小さくなる原因は、面配向、粒
径および交換結合の大きさに起因しているものと考えら
れる。ただし、ＦｅＣｏ濃度が高くなると、粒径が大き
くなるため、膜の結晶配向が（１１０）面になっていて
も、Ｈｃは大きくなる。FIG. 3 shows the composition dependence of the coercive force of the FeCo-Zr-O film. As is clear from the figure, FeCo
Small composition range of Hc found that lie along the -ZrO 2 compositions. It is considered that the reason why Hc becomes small is due to the plane orientation, the particle size and the size of the exchange coupling. However, since the grain size increases as the FeCo concentration increases, Hc increases even if the crystal orientation of the film is the (110) plane.
【００２２】図１と３とを重ね合わせると明らかなよう
に、Ｚｒ濃度が１（原子％）以上、３（原子％）以下、
ＦｅＣｏ濃度が８８（原子％）以上９２（原子％）以
下、そしてＯ濃度が６（原子％）以上１０（原子％）以
下の組成域に飽和磁化が２．２Ｔ以上の軟磁性膜を見出
すことが出来た。As is apparent from the superposition of FIGS. 1 and 3, the Zr concentration is not less than 1 (at%) and not more than 3 (at%),
To find a soft magnetic film having a saturation magnetization of 2.2 T or more in a composition range in which the FeCo concentration is 88 (atomic%) or more and 92 (atomic%) or less, and the O concentration is 6 (atomic%) or more and 10 (atomic%) or less. Was completed.
【００２３】本発明膜の典型的な磁化曲線の結果を図４
に示す。図４−Ａは成膜したままの膜の結果であり、図
４−Ｂは７７３Ｋ（５００℃）で熱処理した後の膜の結
果である。なお、熱処理は真空中で、１ｋＯｅの静磁界
中で行った。いずれも２．２Ｔ以上のＢｓを示し、面内
磁化膜になっている。注目すべき結果は熱処理後のＨｃ
の値である。熱処理を施すことにより、Ｈｃの大きさは
約１／３に小さくなる。ここでＨｃｅは容易磁化方向
の、Ｈｃｈは困難磁化方向の保磁力を示す。このよう
に、熱処理により軟磁性が改善することがわかったの
で、熱処理温度とＨｃとの関係を詳細に検討した（図
５）。Ｈｃは熱処理温度の上昇とともに小さくなり、７
７３Ｋ付近で最小値を示し、それ以上の温度では増加し
始める。熱処理によるＨｃの減少は、成膜時の歪が緩和
したことによるものであり、高温での増大はＦｅＣｏ粒
子の粒径の増加に起因しているものと考えられる。これ
らの結果は、本合金薄膜の耐熱性が比較的大きいことを
も示唆している。The typical magnetization curve results for the inventive film are shown in FIG.
Shown in. FIG. 4-A shows the result of the as-deposited film, and FIG. 4-B shows the result of the film after heat treatment at 773K (500 ° C.). The heat treatment was performed in vacuum in a static magnetic field of 1 kOe. Both show Bs of 2.2 T or more, and are in-plane magnetized films. Notable result is Hc after heat treatment
Is the value of. By performing the heat treatment, the size of Hc is reduced to about 1/3. Here, Hce represents the coercive force in the easy magnetization direction, and Hch represents the coercive force in the difficult magnetization direction. As described above, it was found that the heat treatment improves the soft magnetism. Therefore, the relationship between the heat treatment temperature and Hc was examined in detail (FIG. 5). Hc decreases with increasing heat treatment temperature,
It shows a minimum value around 73K, and begins to increase at higher temperatures. The decrease in Hc due to heat treatment is due to the relaxation of strain during film formation, and the increase at high temperature is considered to be due to the increase in the particle size of FeCo particles. These results also suggest that the alloy thin film has relatively high heat resistance.
【００２４】種々の温度で熱処理した試料の透磁率の周
波数依存性を評価した結果が、図６に示してある。一軸
磁気異方性が付与されているために、試料は成膜直後の
膜でも、６００ＭＨｚまでほぼ平らである。図中の６９
３Ｋの結果から明らかなように、熱処理温度を上げる
と、透磁率ばかりでなく、周波数依存性も向上する。最
小のＨｃの値を示した７７３Ｋで処理された膜は透磁率
は大きいが、渦電流損失の影響で３００ＭＨｚ付近から
減少する。The results of evaluating the frequency dependence of the magnetic permeability of the samples heat-treated at various temperatures are shown in FIG. Since the uniaxial magnetic anisotropy is imparted, the sample is almost flat up to 600 MHz even in the film immediately after film formation. 69 in the figure
As is clear from the result of 3K, increasing the heat treatment temperature improves not only the magnetic permeability but also the frequency dependence. The film treated at 773K, which showed the minimum Hc value, has a high magnetic permeability, but decreases from around 300 MHz due to the effect of eddy current loss.
【００２５】表１に示した試料は、いずれも請求項記載
の範囲の膜である。これらの膜はいずれもＢｓは２．２
Ｔ以上の値を示し、面内磁化膜になっており、軟磁性を
示す。Ｒｕの添加は軟磁性とＨｋの向上に奇与し、Ｐ
ｄ，ＰｔはＨｋを増大させる効果が大きい。All the samples shown in Table 1 are films within the scope of the claims. In all of these films, Bs is 2.2.
It exhibits a value of T or more, is an in-plane magnetized film, and exhibits soft magnetism. The addition of Ru has an adverse effect on the improvement of soft magnetism and Hk.
d and Pt have a large effect of increasing Hk.
【００２６】[0026]
【表１】 [Table 1]
【００２７】本発明の高飽和磁化を有する軟磁性薄膜
は、Ｂｓが大きいばかりでなく、高周波軟磁気特性が優
れているので、磁気記録ヘッド用磁心のみならず、１Ｍ
Ｈｚ以上の高周波帯域で用いるトランス用磁心やインダ
クタ、フィルタなどの磁心としても好適である。また高
周波ＥＭＩ材料としても適している。The soft magnetic thin film having a high saturation magnetization of the present invention has not only a large Bs but also excellent high frequency soft magnetic characteristics, so that not only the magnetic core for a magnetic recording head but also 1M.
It is also suitable as a magnetic core for transformers, inductors, filters, etc. used in a high frequency band of Hz or higher. It is also suitable as a high frequency EMI material.
【００２８】[0028]
【発明の効果】本発明の高飽和磁化を有する磁心用軟磁
性膜は、（１１０）面に優先配向した４０ｎｍ以下の粒
径を有するＦｅＣｏマトリックス中に、微小なＺｒ−Ｏ
粒子が分散している構造からなり、２．２Ｔ以上のＢｓ
を有するばかりでなく、その透磁率は約１ＧＨｚ付近ま
で伸びている。そのため、磁気ヘッド用磁心材料のみな
らず、各種の高周波磁気デバイス用磁心材料として好適
で、その工業的意義は大きい。The soft magnetic film for a magnetic core having a high saturation magnetization of the present invention has a fine Zr-O in a FeCo matrix having a grain size of 40 nm or less preferentially oriented in the (110) plane.
It has a structure in which particles are dispersed and has a Bs of 2.2 T or more.
Not only that, but its magnetic permeability extends to around 1 GHz. Therefore, it is suitable not only as a magnetic core material for a magnetic head but also as a magnetic core material for various high-frequency magnetic devices, and its industrial significance is great.
【図１】（Ｆｅ．６５Ｃｏ．３５）−Ｚｒ−Ｏ３元系薄
膜の組成と、膜の容易磁化方向と飽和磁化の等値曲線を
示す特性図である。[1] (Fe .65 Co .35) the composition of -Zr-O3 ternary thin film, a characteristic diagram showing the equality curves of the easy magnetization direction as the saturation magnetization of the film.
【図２】成膜したままの（Ｆｅ．６３Ｃｏ．３７）
９５．２Ｚｒ２．０Ｏ２．８膜（Ａ）と（Ｆｅ．６５Ｃ
ｏ．３５）９２．７Ｚｒ２．２Ｏ５．１膜（Ｂ）とのＸ
線回折図形。FIG. 2 As-deposited (Fe .63 Co .37 )
95.2 Zr 2.0 O 2.8 film (A) and (Fe .65 C
o . 35 ) X with 92.7 Zr 2.2 O 5.1 film (B)
Line diffraction pattern.
【図３】（Ｆｅ．６５Ｃｏ．３５）−Ｚｒ−Ｏ３元系薄
膜の組成と、膜の容易磁化方向と保磁力の等値曲線を示
す特性図である。[3] the composition of the (Fe .65 Co .35) -Zr- O3 ternary thin film, a characteristic diagram showing the equality curves of the easy magnetization direction and the coercive force of the film.
【図４】（Ｆｅ．６５Ｃｏ．３５）９２．７Ｚｒ２．２
Ｏ５．１薄膜の成膜したままの膜と、７７３Ｋで熱処理
した膜の磁化と印加磁場との関係を示す特性図である。[4] (Fe .65 Co .35) 92.7 Zr 2.2
FIG. 6 is a characteristic diagram showing the relationship between the magnetization and applied magnetic field of an as-deposited O 5.1 thin film and a film heat-treated at 773K.
【図５】（Ｆｅ．６５Ｃｏ．３５）９２．７Ｚｒ２．２
Ｏ５．１薄膜の保磁力と熱処理温度との関係を示す特性
図である。FIG. 5: (Fe .65 Co .35 ) 92.7 Zr 2.2
It is a characteristic view which shows the relationship between the coercive force of an O5.1 thin film, and heat processing temperature.
【図６】（Ｆｅ．６５Ｃｏ．３５）９２．７Ｚｒ２．２
Ｏ５．１薄膜の成膜したままの膜と６９３Ｋと７７３Ｋ
で熱処理した膜の透磁率と周波数の関係を示す特性図で
ある。FIG. 6 is (Fe .65 Co .35 ) 92.7 Zr 2.2.
As-deposited O 5.1 thin film and 693K and 773K
FIG. 6 is a characteristic diagram showing the relationship between magnetic permeability and frequency of the film heat-treated in Step 1.
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4G002 AA06 AA10 AB01 AD02 AD04 AE03 5D033 BA03 CA01 DA03 5D093 AA05 BB18 BC18 FA09 HA17 JA01 JC03 JC06 5E049 AA01 AA04 AA09 AC05 BA12 ─────────────────────────────────────────────────── ─── Continued front page F-term (reference) 4G002 AA06 AA10 AB01 AD02 AD04 AE03 5D033 BA03 CA01 DA03 5D093 AA05 BB18 BC18 FA09 HA17 JA01 JC03 JC06 5E049 AA01 AA04 AA09 AC05 BA12
Claims (5)
１００−Ｘ−Ｙ−ＺＭＸＲＹＯＺで表され、ＭはＺｒ及
びＡｌの１種又は２種の元素であり、ＲはＲｕ，Ｐｄ，
Ｐｔのうちから選択された１種又は２種の元素であり、
Ｏは酸素を表し、且つ組成比Ａ，Ｘ，Ｙ，Ｚは原子比率
で、 ０．２５≦Ａ≦０．５ １≦Ｘ≦３ ０≦Ｙ≦１ ６≦Ｚ≦１０ である組成からなり、体心立方構造の（１１０）面が優
先配向している粒径が４０ｎｍ以下の微結晶で、且つ飽
和磁化２．２Ｔ以上を有することを特徴とする磁心用軟
磁性膜。 1. A general formula (Fe 1-A Co A )
100-X-Y-Z M X R Y O Z , M is one or two elements of Zr and Al, R is Ru, Pd,
One or two elements selected from Pt,
O represents oxygen, and the composition ratios A, X, Y, and Z are atomic ratios, and 0.25 ≦ A ≦ 0.5 1 ≦ X ≦ 3 0 ≦ Y ≦ 16 6 ≦ Z ≦ 10 A soft magnetic film for a magnetic core, characterized in that the (110) plane of the body-centered cubic structure is microcrystalline with a grain size of 40 nm or less and has a saturation magnetization of 2.2 T or more.
１００−Ｘ−Ｙ−ＺＺｒＸＲｕＹＯＺで表され、且つ組
成比Ａ，Ｘ，Ｙ，Ｚは原子比率で、 ０．２５≦Ａ≦０．５ １≦Ｘ≦３ ０≦Ｙ≦１ ６≦Ｚ≦１０ である組成からなり、ＺｒとＯの原子比率が１：２より
も多い酸素を含み、体心立方構造の（１１０）面が優先
配向している粒径が４０ｎｍ以下の微結晶で、且つ飽和
磁化２．２Ｔ以上を有することを特徴とする磁心用軟磁
性膜。2. A general formula (Fe 1-A Co A ).
100-X-Y-Z is represented by Zr X Ru Y O Z, and the composition ratio A, X, Y, Z is atomic ratio, 0.25 ≦ A ≦ 0.5 1 ≦ X ≦ 3 0 ≦ Y ≦ The composition is such that 16 ≦ Z ≦ 10, the atomic ratio of Zr and O is greater than 1: 2, and oxygen is included, and the (110) plane of the body-centered cubic structure is preferentially oriented and the particle size is 40 nm or less. A soft magnetic film for a magnetic core, which is microcrystalline and has a saturation magnetization of 2.2 T or more.
１００−Ｘ−Ｙ−ＺＡｌＸＲｕＹＯＺで表され、且つ組
成比Ａ，Ｘ，Ｙ，Ｚは原子比率で、 ０．２５≦Ａ≦０．５ １≦Ｘ≦２．４ ０≦Ｙ≦１ ２≦Ｚ≦６ である組成からなり、ＡｌとＯとの原子比率が２：３よ
りも多い酸素を含み、体心立方構造の（１１０）面が優
先配向している粒径が４０ｎｍ以下の微結晶で、且つ飽
和磁化２．２Ｔ以上を有することを特徴とする磁心用軟
磁性膜。3. A general formula (Fe 1-A Co A )
100-X-Y-Z is represented by Al X Ru Y O Z, and the composition ratio A, X, Y, Z is atomic ratio, 0.25 ≦ A ≦ 0.5 1 ≦ X ≦ 2.4 0 ≦ The composition is such that Y ≦ 12 ≦ Z ≦ 6, the atomic ratio of Al to O is larger than 2: 3, and oxygen is included, and the (110) plane of the body-centered cubic structure has a preferentially oriented grain size. A soft magnetic film for a magnetic core, which is a microcrystal of 40 nm or less and has a saturation magnetization of 2.2 T or more.
とにより、５Ｏｅ以上の一軸磁気異方性を付与したこと
を特徴とする請求項１ないし３のいずれか１項に記載の
磁心用軟磁性膜。4. The magnetic core according to any one of claims 1 to 3, wherein uniaxial magnetic anisotropy of 5 Oe or more is imparted by forming the film in a unidirectional magnetic field of 50 Oe or more. Soft magnetic film.
一方向の磁界中で焼鈍することを特徴とする請求項１な
いし４のいずれか１項に記載の磁心用軟磁性膜。5. The soft magnetic film for a magnetic core according to claim 1, wherein the soft magnetic film is annealed at a temperature of 100 ° C. or more and 600 ° C. or less and in a magnetic field in one direction.
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| Application Number | Title | Priority Date | Filing Date |
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| JP2001331714A Withdrawn JP2003100515A (en) | 2001-09-21 | 2001-09-21 | Soft magnetic thin film for magnetic core with high saturation magnetization |
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| Country | Link |
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| JP (1) | JP2003100515A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004097806A1 (en) * | 2003-04-30 | 2004-11-11 | Fujitsu Limited | Magnetic head |
| JP2005025890A (en) * | 2003-07-04 | 2005-01-27 | Fujitsu Ltd | Magnetic film for magnetic head |
| US20100201469A1 (en) * | 2006-08-09 | 2010-08-12 | General Electric Company | Soft magnetic material and systems therewith |
| JP2012132095A (en) * | 2010-10-29 | 2012-07-12 | General Electric Co <Ge> | Article formed using nanostructured ferritic alloy |
| JP2019534562A (en) * | 2016-10-27 | 2019-11-28 | ザ ボード オブ トラスティーズ オブ ザ ユニヴァーシティ オブ アラバマ | Fe-Al alloy magnetic thin film |
-
2001
- 2001-09-21 JP JP2001331714A patent/JP2003100515A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004097806A1 (en) * | 2003-04-30 | 2004-11-11 | Fujitsu Limited | Magnetic head |
| JPWO2004097806A1 (en) * | 2003-04-30 | 2006-07-13 | 富士通株式会社 | Magnetic head |
| US7372666B2 (en) | 2003-04-30 | 2008-05-13 | Fujitsu Limited | Magnetic head with alternately laminated (110)-orientation-inducing non-magnetic underlayers, magnetic layers, and discontinuous insulating layers |
| JP2005025890A (en) * | 2003-07-04 | 2005-01-27 | Fujitsu Ltd | Magnetic film for magnetic head |
| US20100201469A1 (en) * | 2006-08-09 | 2010-08-12 | General Electric Company | Soft magnetic material and systems therewith |
| JP2012132095A (en) * | 2010-10-29 | 2012-07-12 | General Electric Co <Ge> | Article formed using nanostructured ferritic alloy |
| JP2019534562A (en) * | 2016-10-27 | 2019-11-28 | ザ ボード オブ トラスティーズ オブ ザ ユニヴァーシティ オブ アラバマ | Fe-Al alloy magnetic thin film |
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