JPH0738357B2 - Method of manufacturing perpendicular magnetic recording medium - Google Patents

Description

【発明の詳細な説明】Detailed Description of the Invention

【０００１】[0001]

【産業上の利用分野】本発明は垂直磁気記録方式におい
て使用する磁気記録媒体（特に磁気光記録媒体）の製造
方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a magnetic recording medium (particularly a magneto-optical recording medium) used in a perpendicular magnetic recording system.

【０００２】[0002]

【従来の技術及び発明が解決すべき課題】従来、薄膜面
と垂直な方向に磁化容易軸を有する強磁性薄膜としてＭ
ｎＢｉ、ＭｎＣｕＢｉ、ＣｏＣｒなどの多結晶金属薄
膜、ＧＩＧに代表される化合物単結晶薄膜、Ｇｄ−Ｃ
ｏ、Ｇｄ−Ｆｅ、Ｔｂ−Ｆｅ、Ｄｙ−Ｆｅなどの希土類
遷移金属非晶質薄膜などが知られている。2. Description of the Related Art Conventionally, M has been used as a ferromagnetic thin film having an easy axis of magnetization in a direction perpendicular to the thin film surface.
Polycrystalline metal thin films such as nBi, MnCuBi, and CoCr, compound single crystal thin films represented by GIG, Gd-C
Known are rare-earth transition metal amorphous thin films such as o, Gd-Fe, Tb-Fe, and Dy-Fe.

【０００３】本発明はこれら以外の特に希土類遷移金属
微細結晶合金薄膜に関するものである。非晶質膜は、多
結晶薄膜のようにノイズの原因となるような結晶粒界が
存在しない、広い膜を容易に製作できるなどの特長を有
し、光磁気記録材料として好都合である。The present invention relates to a rare-earth transition metal fine crystal alloy thin film other than the above. The amorphous film is advantageous as a magneto-optical recording material because it has features such as the absence of crystal grain boundaries that cause noise unlike a polycrystalline thin film, and that a wide film can be easily manufactured.

【０００４】希土類遷移金属非晶質合金が光磁気記録媒
体として使用される為には、磁化容易方向が膜面に対し
て垂直方向に向いていることが要求される。垂直磁気異
方性は、いかなる場合にも誘起できるものではなく、む
しろ、磁性薄膜の反磁界の発生により膜面に平行な方向
へ配向する傾向を示す。垂直磁化膜を得るためには、こ
の反磁界に打ち勝つだけの異方性エネルギーを付与する
ことが必要である。In order to use a rare-earth transition metal amorphous alloy as a magneto-optical recording medium, it is required that the easy magnetization direction be perpendicular to the film surface. Perpendicular magnetic anisotropy cannot be induced in any case, but rather tends to be oriented in a direction parallel to the film surface due to the generation of a demagnetizing field of the magnetic thin film. In order to obtain a perpendicularly magnetized film, it is necessary to give anisotropic energy sufficient to overcome this demagnetizing field.

【０００５】得られる薄膜の垂直磁気異方性の程度は、
一軸異方性定数Ｋｕの大きさによって表現でき、垂直磁
化膜となるためには、このＫｕと飽和磁化Ｍｓとの間に
Ｋｕ＞２πＭｓ²の関係を満足しなければならないとさ
れている。本発明において「垂直磁気異方性」とはかか
る条件を充足するものを少なくとも包含する。The degree of perpendicular magnetic anisotropy of the obtained thin film is
It can be expressed by the magnitude of the uniaxial anisotropy constant Ku, and it is said that the relationship of Ku> 2πMs ² must be satisfied between this Ku and the saturation magnetization Ms in order to form a perpendicular magnetization film. In the present invention, “perpendicular magnetic anisotropy” includes at least those satisfying such conditions.

【０００６】垂直磁気記録媒体では一般に高い記録密度
が要求され、微小な磁区が安定して保持されるためには
Ｍｓが大きく、かつ上記の関係を満足する十分に大きな
Ｋｕが得られることが大へん重要である。また、光磁気
ディスクではレーザ光を書込みパワーとして用いるが、
これを可能とするためには１００〜２００℃程度の十分
に低いキュリー温度Ｔｃとそれよりも十分に高い結晶化
温度Ｔｃｒｙを有し少なくともこの温度差は５０℃好ま
しくは１００℃以上であることが要求される。A perpendicular magnetic recording medium is generally required to have a high recording density, and in order to stably hold a minute magnetic domain, a large Ms and a sufficiently large Ku satisfying the above relationship are often obtained. Very important. Further, in the magneto-optical disk, laser light is used as the writing power,
In order to make this possible, it has a sufficiently low Curie temperature Tc of about 100 to 200 ° C. and a crystallization temperature Tcry sufficiently higher than that, and at least this temperature difference is 50 ° C., preferably 100 ° C. or more. Required.

【０００７】垂直磁化膜として最も良く知られている希
土類−遷移金属の組合せは重希土類元素と鉄である。代
表的なものにＴｂＦｅ、ＧｄＦｅ、ＤｙＦｅ、ＧｄＴｂ
Ｆｅ、ＴｂＤｙＦｅなどがある。例えばＴｂＦｅはキュ
リー温度Ｔｃ＝１４０〜２５０℃、カー回転角θ_k約0.3
°、飽和磁化Ｍｓ＝５０〜１００ｅｍｕ／ｃｃ、垂直磁
気異方性定数Ｋｕ＝１０⁵〜１０⁶ｅｒｇ／ｃｃなどの特
性を有する。The rare earth-transition metal combination best known as a perpendicular magnetization film is heavy rare earth element and iron. Typical ones are TbFe, GdFe, DyFe, GdTb
There are Fe, TbDyFe, and the like. For example, TbFe has a Curie temperature Tc of 140 to 250 ° C. and a Kerr rotation angle θ _{k of} about 0.3.
And the saturation magnetization Ms = 50 to 100 emu / cc, the perpendicular magnetic anisotropy constant Ku = 10 ⁵ to 10 ⁶ erg / cc, and the like.

【０００８】しかしこれらに用いられるＴｂ、Ｄｙ、Ｇ
ｄなどの重希土類元素は地殻中にわずかしか存在せず希
少資源であり、また複雑な分離工程を必要とし、大へん
高価である。However, Tb, Dy and G used for these
Heavy rare earth elements such as d are scarce resources because they are scarcely present in the crust, and require a complicated separation process, which is very expensive.

【０００９】また重希土類元素と鉄の原子磁気モーメン
トは反平行に結合しているので飽和磁化Ｍｓやキュリー
温度Ｔｃの組成依存性が大きく均質な製品を数多く生産
することが困難である。Further, since the heavy rare earth elements and the atomic magnetic moments of iron are coupled antiparallel to each other, it is difficult to produce many homogeneous products because the composition of saturation magnetization Ms and Curie temperature Tc is large.

【００１０】一方Ｎｄ、Ｐｒなどの軽希土類元素は地殻
中に重希土類元素よりもはるかに多く存在している。こ
のような希土類−鉄垂直磁化膜がＮｄ、Ｐｒなどの軽希
土類元素を用いて作製することができれば、資源的な問
題は一掃されるのである。On the other hand, light rare earth elements such as Nd and Pr are present in the crust much more than heavy rare earth elements. If such a rare earth-iron perpendicular magnetization film can be produced using a light rare earth element such as Nd or Pr, the resource problem will be eliminated.

【００１１】これまで軽希土類・鉄の非晶質合金の検討
は例えばJ.J.CroatがＦｅ_0.60Ｎｄ_0.40やＦｅ_0.60Ｐｒ
_0.40付近の組成で液体急冷法を用いてリボン合金を作製
し、高い保磁力が得られることから永久磁石としての可
能性を論じている(Appl.Phys.Lett.39(4).15.August.19
81)。しかしこのような方法で得られるリボンは合金全
体にわたって均質なものは得られず、実質的に等方性の
ものしか得られていない。またリボンの厚さは３３〜２
０８μｍであって記録媒体として用いられるものではな
い。Up to now, in the study of amorphous alloys of light rare earth / iron, for example, JJCroat showed that Fe _0.60 Nd _0.40 and Fe _0.60 Pr.
Ribbon alloys were prepared using a liquid quenching method with a composition near _0.40 , and the possibility as a permanent magnet was discussed because a high coercive force was obtained (Appl.Phys.Lett.39 (4) .15.August). .19
81). However, the ribbon obtained by such a method cannot obtain a homogeneous ribbon throughout the alloy, but only a substantially isotropic ribbon. The ribbon thickness is 33-2.
It is 08 μm and is not used as a recording medium.

【００１２】また最近では、K.Tsutsumi等がＦｅ_61.5−
Ｎｄ₃₄−Ｔｉ_4.5のスパッタ薄膜が垂直磁気異方性を有
することを報告している(Jpn.J.Appl.Phys.23(1984).L1
69〜L171頁)。しかしその特性はＭｓ＝４３０ｅｍｕ／
ｃｃ、Ｋｕ＝２×１０⁶ｅｒｇ／ｃｃであった。またＴ
ｉを含まないＦｅＮｄスパッタ薄膜については作製条件
は明らかでないが、薄膜の面内に異方性があるものしか
報告されていない。[0012] In recent years, K.Tsutsumi, etc. Fe _61.5 -
Sputtered film of Nd ₃₄ -Ti _4.5 is reported to have a perpendicular magnetic anisotropy (Jpn.J.Appl.Phys.23 (1984) .L1
69-L p. 171). However, the characteristic is Ms = 430 emu /
It was cc and Ku = 2 × 10 ⁶ erg / cc. See also T
Although the manufacturing conditions of the FeNd sputtered thin film not containing i are not clear, only those having in-plane anisotropy of the thin film have been reported.

【００１３】軽希土類元素及び鉄の非晶質薄膜は高い飽
和磁化を有するがそのために薄膜の反磁界による作用に
打ち勝つための垂直磁気異方性エネルギーを付与するこ
とはほとんど不可能とされてきた。Although amorphous thin films of light rare earth elements and iron have high saturation magnetization, it has been almost impossible to impart perpendicular magnetic anisotropy energy for overcoming the action due to the demagnetizing field of the thin films. .

【００１４】[0014]

【目的】本発明は、軽希土類及び鉄を中心とする新規な
垂直磁気記録媒体（特に光磁気記録媒体）の製造方法を
提供することを基本的目的とする。本発明はさらに上述
の従来法に比し優れた特性を有する垂直磁気記録媒体の
製造方法を提供することをも目的とする。An object of the present invention is to provide a novel method of manufacturing a perpendicular magnetic recording medium (particularly a magneto-optical recording medium) centered on light rare earth and iron. Another object of the present invention is to provide a method of manufacturing a perpendicular magnetic recording medium having excellent characteristics as compared with the above-mentioned conventional method.

【００１５】[0015]

【課題を解決するための手段】[Means for Solving the Problems]

【概要】すなわち、本発明は軽希土類及び鉄を中心とす
るまつたく新しい磁気記録媒体の製造方法を提供するも
のである。本発明における磁気記録媒体は鉄及び希土類
元素、又はこれらとＣｏ、を中心とし、希土類元素とし
てＮｄ、Ｐｒを主体とする軽希土類元素を用い、薄膜内
の非晶質マトリックスに数Å〜数１００Åの微細結晶を
含む垂直磁化薄膜である。[Outline] That is, the present invention provides a new method for manufacturing a magnetic recording medium comprising a rare rare earth element and iron. The magnetic recording medium in the present invention uses a light rare earth element mainly composed of iron and a rare earth element, or these and Co and mainly containing Nd and Pr as a rare earth element, and
Is a perpendicularly magnetized thin film containing several Å to several hundred Å fine crystals in the amorphous matrix of .

【００１６】本発明による垂直磁気記録媒体の製造方法
の第１の態様（請求の範囲第１項）は、基板上に金属ガ
ス凝集法により薄膜を形成する垂直磁気記録媒体の製造
方法において、基板上に金属ガス凝集法により薄膜を形
成する垂直磁気記録媒体の製造方法において、基板温度
を１８０℃〜合金の結晶化温度以下の温度に保持して、
式ＲＦｅにより本質上表わされ、希土類元素Ｒ２５〜６
０原子％、残部Ｆｅから成り、Ｒの内７０原子％以上が
Ｎｄ及びＰｒの１種又は２種、なおＲの残部はＹ、Ｌ
ａ、Ｃｅ、Ｓｍ、Ｇｄ、Ｔｂ、Ｄｙ、Ｈｏ、Ｅｒ及びＹ
ｂの一種以上とする組成から成り、膜厚を０．３〜３μ
ｍとし、かつ薄膜の非晶質マトリックスに数Å〜数１０
０Åの微細結晶相を少なくともを含むと共に垂直磁気異
方性定数Ｋｕが反磁界エネルギー２πＭｓ ^２ （Ｍｓは飽
和磁化）より大きな垂直磁気異方性を有し、さらに結晶
化温度Ｔｃｒｙとキュリー温度Ｔｃとの温度差Ｔｃｒｙ
−Ｔｃが１００℃以上である薄膜を形成することを特徴
とする。A first aspect (claim 1) of the method for manufacturing a perpendicular magnetic recording medium according to the present invention is the method for manufacturing a perpendicular magnetic recording medium, wherein a thin film is formed on a substrate by a metal gas aggregation method. In a method of manufacturing a perpendicular magnetic recording medium in which a thin film is formed on the upper surface by a metal gas aggregation method, the substrate temperature is maintained at 180 ° C. to a temperature equal to or lower than the crystallization temperature of the alloy,
Represented essentially by the formula RFe, rare earth elements R 25 to 6
0 atomic% and balance Fe, 70 atomic% or more of R is 1 or 2 kinds of Nd and Pr, and the balance of R is Y, L
a, Ce, Sm, Gd, Tb, Dy, Ho, Er and Y
The composition is one or more of b and the film thickness is 0.3 to 3 μm.
m, and several Å to several tens in the amorphous matrix of the thin film.
The perpendicular magnetic anisotropy constant Ku includes at least a fine crystal phase of 0Å, and the perpendicular magnetic anisotropy constant Ku has a demagnetizing field energy of 2πMs ² (Ms is
Has a larger perpendicular magnetic anisotropy than the sum magnetization) and further has a temperature difference Tcry between the crystallization temperature Tcry and the Curie temperature Tc.
It is characterized by forming a thin film having -Tc of 100 ° C or higher.

【００１７】本発明による垂直磁気記録媒体の製造方法
の第２の態様（請求の範囲第２項）として、前記Ｆｅ３
０原子％未満（全組成に対する）をＣｏにて置換した垂
直記録媒体が提供される（即ち全組成中Ｃｏ３０原子％
未満となる）。As a second aspect (claim 2) of the method for manufacturing a perpendicular magnetic recording medium according to the present invention, the Fe 3
Provided is a perpendicular recording medium in which less than 0 atomic% (relative to the total composition) is replaced with Co (that is, 30 atomic% Co in the total composition).
Less than).

【００１８】さらに本発明による垂直磁気記録媒体の製
造方法の別の態様（請求の範囲第３〜４項）として、Ｃ
ｏを含まない場合は所定量以外の他の元素Ｍ１０原子％
以下（但しＭはＮｉ、Ｖ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ｍ
ｎ、Ｂｉ、Ａｌ、Ｓｉ、Ｐｂ、Ｓｎ及びＳｂの一種以
上）を含むこともでき、３０原子％未満のＣｏを含む場
合はさらにＺｒを含むことができる。As another aspect (claims 3 to 4) of the method for manufacturing a perpendicular magnetic recording medium according to the present invention, C
When o is not included, other elements other than the specified amount M10 atom%
Below (however, M is Ni, V, Ta, Cr, Mo, W, M
One or more of n, Bi, Al, Si, Pb, Sn and Sb) may be contained, and when containing less than 30 atomic% Co, Zr may be further contained.

【００１９】以上は、式Ｒ（Ｆｅ、Ｃｏ）Ｍで表わさ
れ、Ｒ２５〜６０原子％、Ｍ０〜１０原子％、Ｃｏ３０
原子％未満及び残部Ｆｅから成る組成を成す。The above is represented by the formula R (Fe, Co) M, R 25 to 60 atom%, M 0 to 10 atom%, Co 30
It has a composition of less than atomic% and the balance Fe.

【００２０】[0020]

【作用効果概要】本発明者らは前述のような事情から微
細結晶質薄膜の作製条件を詳細に検討した。その結果資
源が豊富で安価なＮｄ、Ｐｒなどの軽希土類元素及び鉄
を用いてキュリー温度Ｔｃ＝７０〜２５０℃、飽和磁化
Ｍｓ約４５０ｅｍｕ／ｃｃ以上、垂直磁気異方性定数Ｋ
ｕ少くとも1.5×１０⁶ｅｒｇ／ｃｃ以上、さらに2.5〜
７×１０⁶ｅｒｇ／ｃｃ以上、カー回転角θ_k約0.3°以
上の特性、即ち前述の重希土類−鉄非晶質薄膜と同等ま
たはそれ以上の特性を有する垂直磁化膜が得られた。[Summary of Actions and Effects] The present inventors have studied in detail the conditions for producing a fine crystalline thin film from the above-mentioned circumstances. As a result, Curie temperature Tc = 70 to 250 ° C., saturation magnetization Ms of about 450 emu / cc or more, and perpendicular magnetic anisotropy constant K are obtained by using light rare earth elements such as Nd and Pr, which are rich in resources, and iron, and iron.
u At least 1.5 × 10 ⁶ erg / cc or more, further 2.5-
A perpendicular magnetization film having the characteristics of 7 × 10 ⁶ erg / cc or more and the Kerr rotation angle θ _{k of} about 0.3 ° or more, that is, the characteristics equal to or more than the above-mentioned heavy rare earth-iron amorphous thin film was obtained.

【００２１】既述の通り、垂直磁化膜となるためにはＫ
ｕ＞２πＭｓ²の関係が成立つことが必要とされてい
る。しかし本発明においては磁区が小さく分かれており
その場合には反磁界が見かけのそれよりも小さく、必ず
しも上記の条件を満足しなくとも垂直磁化膜となるが、
安定した垂直磁化膜を得るためには1.5×１０⁶ｅｒｇ／
ｃｃ以上とすることが必要である（大略、Ｋｕ≧0.6×
２πＭｓ²）。As described above, in order to form a perpendicular magnetization film, K
It is necessary that the relationship of u> 2πMs ² is established. However, in the present invention, the magnetic domains are divided into small regions, and in that case, the demagnetizing field is smaller than that apparently, and even if the above conditions are not always satisfied, a perpendicularly magnetized film is formed.
To obtain a stable perpendicular magnetic film, 1.5 × 10 ⁶ erg /
It is necessary to be cc or more (generally, Ku ≧ 0.6 ×
2πMs ² ).

【００２２】垂直磁化膜かどうかは図３のように、膜に
平行方向（//）と垂直方向（⊥）の磁化曲線を測定する
ことによって知ることができる。Whether the film is a perpendicular magnetization film can be known by measuring the magnetization curves in the direction parallel (//) and the direction perpendicular to the film (⊥) as shown in FIG.

【００２３】本発明において、ＮｄやＰｒと鉄との組合
せは各々の原子の磁気モーメントが平行に結合した場
合、重希土類元素・鉄の場合よりも高い飽和磁化が得ら
れ、記録の読み出し精度が向上する。熱磁気書込みを行
なう場合は、高い飽和磁化はもれ磁束が利用できて外部
から加えなければならない磁場が小さくても良い。さら
にＦｅの一部をＣｏで置換することはキュリー温度Ｔｃ
を上昇させさらにカー回転角θ_kを大きくし、θ_k約0.5
°以上のものが得られ、耐食性を改善する。In the present invention, when Nd or Pr and iron are combined in combination, when the magnetic moments of the respective atoms are coupled in parallel, higher saturation magnetization is obtained than in the case of heavy rare earth element / iron, and the reading accuracy of recording is improved. improves. In the case of performing thermomagnetic writing, high saturation magnetization and leakage magnetic flux can be used, and the magnetic field that must be applied from the outside may be small. Further, substituting a part of Fe with Co means that the Curie temperature is Tc.
To increase the Kerr rotation angle θ _k , and θ _{k is} about 0.5.
More than ° can be obtained to improve corrosion resistance.

【００２４】[0024]

【好適な実施の態様】本発明に用いる希土類元素Ｒとし
て、Ｒの内７０％以上はＮｄとＰｒを用い特にＮｄが望
ましい。Ｒの残部は入手上の事情などからＣｅ、Ｙ、Ｓ
ｍ、Ｄｙ、Ｔｂ、Ｈｏ、Ｇｄ、Ｌａ、Ｅｒ、Ｙｂなどそ
の他の希土類元素を含んだものを用いても良い。BEST MODE FOR CARRYING OUT THE INVENTION As the rare earth element R used in the present invention, Nd and Pr are used for 70% or more of R, and Nd is particularly desirable. The rest of R is Ce, Y, S due to availability reasons.
Those containing other rare earth elements such as m, Dy, Tb, Ho, Gd, La, Er, and Yb may be used.

【００２５】Ｒは全体組成中２５原子％以上含まれる
と、Ｋｕ≧１．５Ｘ１０^６ｅｒｇ／ｃｃかつＴｃｒｙ−
Ｔｃの温度差が約１００℃以上の垂直磁化膜となる。When R is 25 atomic% or more in the entire composition, Ku ≧ 1.5 × 10 ⁶ erg / cc and Tcry−
The perpendicular magnetization film has a Tc temperature difference of about 100 ° C. or more.

【００２６】Ｒは全体の組成の３１原子％（ａｔ％）以
上で薄膜面に垂直な磁気異方性定数Ｋｕが2.5×１０⁶ｅ
ｒｇ／ｃｃ以上となり十分に安定な垂直磁化膜となる。R is 31 atomic% (at%) or more of the total composition, and the magnetic anisotropy constant Ku perpendicular to the thin film surface is 2.5 × 10 ⁶ e.
The perpendicular magnetization film becomes rg / cc or more and is sufficiently stable.

【００２７】Ｒが６０ａｔ％以上では活性な希土類元素
を多く含むため薄膜作成後の安定性に欠ける。従ってＲ
の範囲は２５〜６０原子％（好ましくは３１〜６０原子
％）とする。Ｒが３３〜５０ａｔ％はＫｕ＝３×１０^６
ｅｒｇ／ｃｃ以上のさらに好ましい範囲であり、特に好
ましくは３５〜４５ａｔ％である（図８参照）。When R is 60 at% or more, a large amount of active rare earth elements are contained, and thus stability after forming a thin film is insufficient. Therefore R
The range is 25 to 60 atom% (preferably 31 to 60 atom%). When R is 33 to 50 at%, Ku = 3 × 10 ⁶
The range is more preferably erg / cc or more, and particularly preferably 35 to 45 at% (see FIG. 8).

【００２８】図２は飽和磁化Ｍｓ及びキュリー温度Ｔｃ
の組成（Ｎｄ量）依存性を示す図であるが広い組成（Ｎ
ｄ量）範囲にわたって飽和磁化Ｍｓ及びキュリー温度Ｔ
ｃの変化の割合が小さく、重希土類元素鉄の場合と較べ
て遥かに安定した品質の製品を容易に作製できる様子が
わかる。FIG. 2 shows the saturation magnetization Ms and the Curie temperature Tc.
It is a diagram showing the composition (Nd amount) dependence of the
d amount) saturation magnetization Ms and Curie temperature T over the range
It can be seen that the rate of change in c is small and that a product with much more stable quality can be easily produced as compared with the case of heavy rare earth element iron.

【００２９】Ｒの残りは鉄を主体とするがＦｅを全組成
中の３０％未満Ｃｏで置換することは磁気光記録媒体又
は垂直磁化膜としての特性を損なうことなく飽和磁化Ｍ
ｓ、キュリー温度Ｔｃの上昇、カー回転角の増加や薄膜
の耐食性を向上する効果がある。ＣｏをＦｅの５０％以
上置換することは結晶化温度Ｔｃｒｙとキュリー温度Ｔ
ｃの差が小さくなり、またカー回転角も小さくなる。さ
らにターゲットがもろくなり製作が困難となるため、Ｃ
ｏの上限は全組成中３０原子％未満とする。全Ｆｅに対
するＣｏ置換量は好ましくは、約８〜３０原子％未満
（θ_k0.45°以上）、最も好ましくは約１２〜約２７原
子％（θ_k0.5°以上）である。The rest of R mainly consists of iron, but substituting Fe by less than 30% of the total composition makes saturation magnetization M without impairing the characteristics as a magneto-optical recording medium or a perpendicular magnetization film.
s, the Curie temperature Tc is increased, the Kerr rotation angle is increased, and the corrosion resistance of the thin film is improved. Replacing Co by 50% or more of Fe means that crystallization temperature Tcry and Curie temperature T
The difference in c becomes smaller and the Kerr rotation angle also becomes smaller. Furthermore, the target becomes brittle and difficult to manufacture, so C
The upper limit of o is less than 30 atom% in the entire composition. The amount of Co substitution with respect to total Fe is preferably about 8 to less than 30 atom% (θ _k 0.45 ° or more), and most preferably about 12 to about 27 atom% (θ _k 0.5 ° or more).

【００３０】全体の組成の１０ａｔ％未満の元素Ｍ即
ち、Ｎｉ、Ｖ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ｍｎ、Ｂｉ、Ａ
ｌ、Ｐｂ、Ｓｎ、Ｓｂなどの添加も垂直磁化膜としての
特性を損なわない。前記所定量のＣｏを含有する場合に
は、さらにＺｒの添加によっても、その特性を損なわな
い。Element M less than 10 at% of the total composition, ie, Ni, V, Ta, Cr, Mo, W, Mn, Bi, A
The addition of 1, Pb, Sn, Sb, etc. does not impair the characteristics of the perpendicular magnetization film. When the predetermined amount of Co is contained, further addition of Zr does not impair the characteristics.

【００３１】さらに、本発明の組成には全体の組成の１
０ａｔ％未満のＴｉを含有させることもでき、本発明の
方法に従えばＫｕ３×１０⁶ｅｒｇ／ｃｃのものを得る
ことができる。Further, the composition of the present invention has one of the entire compositions.
Ti of less than 0 at% can be contained, and Ku3 × 10 ⁶ erg / cc can be obtained according to the method of the present invention.

【００３２】また本発明による薄膜は飽和磁化Ｍｓが高
いため、垂直磁気異方性定数が1.5×１０⁶ｅｒｇ／ｃｃ
より大きいことが必要である。一般に非晶質膜を作成す
るための基板を構成する基板材料は通常ガラス、Ａｌ、
ポリイミド系樹脂材、ポリエステル系樹脂材などを用い
るが、本発明の場合は垂直磁化膜を得るために基板の温
度を１８０℃以上、該合金組成の結晶化温度以下に保た
なければならないのでこの温度に耐えるものを用いる。
基板温度２００〜３００℃はＫｕ＝３×１０⁶ｅｒｇ／
ｃｃ以上が得られる好ましい範囲である（図４）。Since the thin film according to the present invention has a high saturation magnetization Ms, the perpendicular magnetic anisotropy constant is 1.5 × 10 ⁶ erg / cc.
It needs to be larger. Generally, the substrate material constituting the substrate for forming the amorphous film is usually glass, Al,
A polyimide resin material, a polyester resin material, or the like is used, but in the case of the present invention, the temperature of the substrate must be kept at 180 ° C. or higher and below the crystallization temperature of the alloy composition in order to obtain the perpendicular magnetization film. Use one that can withstand temperature.
When the substrate temperature is 200 to 300 ° C., Ku = 3 × 10 ⁶ erg /
It is a preferable range where cc or more is obtained (FIG. 4).

【００３３】薄膜の厚さは厚くなるに従ってＫｕが大き
くなり、垂直磁化膜を得るためには0.3μｍ以上必要で
あるが、３μｍをこえると均一な層が得難く、生産上好
ましくない（図６）。Ku increases as the thickness of the thin film increases, and 0.3 μm or more is required to obtain a perpendicularly magnetized film, but if it exceeds 3 μm, it is difficult to obtain a uniform layer, which is not preferable in production (FIG. 6). ).

【００３４】本発明による薄膜は金属ガス凝集法（いわ
ゆる気相析着法）により形成され、真空蒸着法、物理的
析着法（スパッタ法、イオンプレーティング法等）、Ｃ
ＶＤ法等いずれの方法においても作製できるが、スパッ
タ法の場合アルゴンの圧力は２×１０^-1Ｔｏｒｒ付近が
望ましい（図７）。The thin film according to the present invention is formed by a metal gas agglomeration method (so-called vapor deposition method), and is formed by vacuum vapor deposition method, physical deposition method (sputtering method, ion plating method, etc.), C
It can be formed by any method such as the VD method, but in the case of the sputtering method, the pressure of argon is preferably around 2 × 10 ⁻¹ Torr (FIG. 7).

【００３５】スパッタの際に基板には基板と垂直方向に
数〜数十Ｏｅの磁界が加わっていることが望ましい。こ
の磁界は基板下にとりつけた加熱用のシース線をソレノ
イド状に巻きつけ、加熱電流として直流を用いることに
よって容易に得ることができる。It is desirable that a magnetic field of several to several tens Oe is applied to the substrate in the direction perpendicular to the substrate during sputtering. This magnetic field can be easily obtained by winding a sheathing wire for heating attached under the substrate in a solenoid shape and using direct current as a heating current.

【００３６】本発明による薄膜の状態は薄膜の非晶質マ
トリックスに約数Å〜約１００Åの大きさの微細結晶相
を含むことが望ましい（図５）。The state of the thin film according to the present invention depends on the amorphous film of the thin film.
Fine crystalline phase with a size of about several Å to about 100 Å
Should be included (FIG. 5).

【００３７】また大きな飽和磁化を有することに基づ
き、光磁気ディスクとして熱磁気書込みを行う場合は囲
りの部分からのもれ磁束が利用できるため外部から加え
る磁場が小さくても良い。Further, since the leakage magnetic flux from the surrounding portion can be utilized when thermomagnetic writing is performed as a magneto-optical disk due to having a large saturation magnetization, a magnetic field applied from the outside may be small.

【００３８】[0038]

【実施例】以下に実施例を用いて詳細に説明する。薄膜
は高周波スパッタ法を用いてＡｒ雰囲気中でガラス基板
上に作成した。Embodiments will be described in detail below with reference to embodiments. The thin film was formed on a glass substrate in an Ar atmosphere by using the high frequency sputtering method.

【００３９】Ａｒガスを導入する前にスパッタ容器内を
５×１０^-7Ｔｏｒｒ以上の真空にした。スパッタの速度
は約２μｍ／ｈｒであった。スパッタ作成中は基板には
バイアス電圧を加えていない。Before introducing Ar gas, the inside of the sputtering container was evacuated to 5 × 10 ⁻⁷ Torr or more. The sputter rate was about 2 μm / hr. No bias voltage is applied to the substrate during sputtering production.

【００４０】基板の加熱は基板の下にとりつけた円筒状
の銅製ボビンの外周に巻回したシース線の電流を調整す
ることにより行った。The substrate was heated by adjusting the electric current of the sheath wire wound around the outer periphery of the cylindrical copper bobbin attached below the substrate.

【００４１】電流は直流を用いたため、基板上には数十
Ｏｅの磁界が発生している。試料の磁気特性は最大磁場
強さが２０ｋＯｅのトルク磁力計及び振動試料型磁力計
（ＶＳＭ）を用いた。薄膜の構造解析はＣｕ−Ｋα線を
用いたＸ線回折と、透過式電子顕微鏡によった。Since a direct current is used as the current, a magnetic field of several tens Oe is generated on the substrate. As the magnetic characteristics of the sample, a torque magnetometer having a maximum magnetic field strength of 20 kOe and a vibrating sample magnetometer (VSM) were used. The structure of the thin film was analyzed by X-ray diffraction using Cu-Kα ray and a transmission electron microscope.

【００４２】[0042]

【実施例１】図１にＦｅ_100-xＮｄ_x、ｘ＝１８、３０、
３５、３８、４０の組成でＡｒ圧が１〜２×１０^-1Ｔｏ
ｒｒ、基板温度２２０〜２９０℃、膜厚５０００Å〜1.
2μｍの条件で作成した薄膜の磁化の温度依存性を示
す。Example 1 In FIG. 1, Fe _100-x Nd _x , x = 18, 30,
The composition of 35, 38 and 40 has an Ar pressure of 1 to 2 × 10 ⁻¹ To.
rr, substrate temperature 220 to 290 ° C., film thickness 5000Å to 1.
The temperature dependence of the magnetization of the thin film formed under the condition of 2 μm is shown.

【００４３】ここで磁化は容易磁化軸方向に飽和磁化さ
せた後、ＶＳＭで１０ｋＯｅの磁場中で測定を行った。Here, the magnetization was subjected to saturation magnetization in the easy magnetization axis direction, and then measured with VSM in a magnetic field of 10 kOe.

【００４４】キュリー温度ＴｃはＭ²／Ｔ（Ｍ：磁化、
Ｔ：温度）曲線の外挿線が温度軸と交錯する点より求め
た。The Curie temperature Tc is M ² / T (M: magnetization,
It was determined from the point where the extrapolation line of the (T: temperature) curve intersects the temperature axis.

【００４５】図１中Ｔｃｒｙは結晶化温度を示す。In FIG. 1, Tcry represents the crystallization temperature.

【００４６】キュリー温度は３５０〜４００Ｋ（７７〜
１２７℃）でＤｙＦｅ（Ｔｃ約７０℃）、ＴｂＦｅ（Ｔ
ｃ約１４０℃）とほぼ同等であった。The Curie temperature is 350 to 400 K (77 to
DyFe (Tc about 70 ° C) at 127 ° C, TbFe (T
c about 140 ° C.).

【００４７】またキュリー温度（Ｔｃ）と結晶化温度
（Ｔｃｒｙ）の差がＮｄ≧３０原子％で約２００℃ある
ことからレーザ光による熱電気書込みが十分行えること
が判る。Further, since the difference between the Curie temperature (Tc) and the crystallization temperature (Tcry) is about 200 ° C. when Nd ≧ 30 atomic%, it can be understood that thermoelectric writing by laser light can be sufficiently performed.

【００４８】図２は図１のキュリー温度及び結晶化温度
を組成（Ｆｅ_{１００−ｘ}Ｎｄ_ｘ）と対比させたものであ
る。キュリー温度又はＭｓは広い組成範囲にわたってほ
とんど変化しないことが判る。Ｎｄ≧２１ａｔ％で温度
差（Ｔｃｒｙ−Ｔｃ）が約５０℃以上となり、Ｎｄ≧２
５ａｔ％で差≧１００℃となり、Ｎｄ≧３０ａｔ％で差
≧２００℃となる。[0048] FIG. 2 is obtained by comparing the Curie temperature and crystallization temperature of the 1 composition as _{(Fe 100-x Nd x)} . It can be seen that the Curie temperature or Ms changes little over a wide composition range. When Nd ≧ 21 at%, the temperature difference (Tcry−Tc) becomes about 50 ° C. or higher, and Nd ≧ 2
The difference is ≧ 100 ° C. at 5 at%, and the difference is ≧ 200 ° C. at Nd ≧ 30 at%.

【００４９】また図２にはまた７７Ｋ及び３００Ｋでの
飽和磁化のＦｅ−Ｎｄ組成依存性を示す。FIG. 2 also shows the Fe-Nd composition dependence of the saturation magnetization at 77K and 300K.

【００５０】[0050]

【実施例２】Ｆｅ₆₅Ｎｄ₃₅及びＦｅ₆₀Ｎｄ₄₀の組成で基
板温度が２４０〜２９０℃、Ａｒ圧が１〜２×１０^-1Ｔ
ｏｒｒの条件で作成したスパッタ薄膜を７７Ｋ及び３０
０Ｋで磁気特性を測定した。その結果を図３に示す。薄
膜の垂直方向（⊥）及び水平方向（//）の測定から７７
Ｋおよび３００Ｋにおいてこれらの薄膜が垂直磁化まく
である様子がわかる。Example 2 A composition of Fe ₆₅ Nd ₃₅ and Fe ₆₀ Nd ₄₀ having a substrate temperature of 240 to 290 ° C. and an Ar pressure of 1 to 2 × 10 ⁻¹ T
The sputtered thin film formed under the condition of orr is 77K and 30
The magnetic properties were measured at 0K. The result is shown in FIG. 77 from thin film vertical (⊥) and horizontal (//) measurements
It can be seen that at K and 300 K these films are vertically magnetized.

【００５１】これらの薄膜のカー回転各θ_kを求めたと
ころ、θ_k＝0.3°が得られた。これは前述の重希土類元
素−鉄非晶質垂直磁化膜と同等以上であった。When the Kerr rotations θ _k of these thin films were determined, θ _k = 0.3 ° was obtained. This was equal to or higher than that of the above-mentioned heavy rare earth element-iron amorphous perpendicular magnetization film.

【００５２】[0052]

【実施例３】Ｆｅ₆₅Ｎｄ₃₅の組成でＡｒ圧１〜２×１０
^-1Ｔｏｒｒ、厚さ６０００〜１２６５０Åの薄膜を作成
し、トルクメータで垂直磁気異方性定数Ｋｕを求めた。
スパッタ中の基板温度は７０〜３３０℃の間で変化させ
た。その結果を図４に示す。Example 3 A composition of Fe ₆₅ Nd ₃₅ and an Ar pressure of 1 to 2 × 10
A thin film of ^-1 Torr and a thickness of 6000 to 12650Å was prepared, and the perpendicular magnetic anisotropy constant Ku was determined with a torque meter.
The substrate temperature during sputtering was changed between 70 and 330 ° C. The result is shown in FIG.

【００５３】Ｋｕの値は基板温度が２６０〜２９０℃で
最大値を示す。図中黒丸は垂直磁化膜であることを示
し、白丸はそうでないことを表わす。基板温度Ｔｓが結
晶化温度Ｔｃｒｙ（≒３２０℃）よりも高い場合はもは
や垂直磁化膜の性質を示さない。（Ｋｕ≒０）The value of Ku shows the maximum value when the substrate temperature is 260 to 290 ° C. In the figure, a black circle indicates that it is a perpendicular magnetization film, and a white circle indicates that it is not. When the substrate temperature Ts is higher than the crystallization temperature Tcry (≈320 ° C.), the property of the perpendicular magnetization film is no longer exhibited. (Ku≈0)

【００５４】基板温度Ｔｓが２１２℃、２８７℃、３３
５℃の場合のスパッタ薄膜のＸ線回折パターンを図５に
示す。Ｔｓ=３３５℃及び２８７℃の場合には、Ｎｄ₂Ｆ
ｅ₁₇やＮｄに相当すると考えられる鋭いピークが現われ
ている。The substrate temperature Ts is 212 ° C., 287 ° C., 33
The X-ray diffraction pattern of the sputtered thin film at 5 ° C. is shown in FIG. When Ts = 335 ° C and 287 ° C, Nd ₂ F
Sharp peaks that are considered to correspond to e ₁₇ and Nd appear.

【００５５】電子顕微鏡の観察からもＴｓ＝２１２℃、
２８７℃の場合には微細結晶の粒子が存在し、Ｔｓ＝３
３５℃の場合には結晶かがかなり進んでいることが判っ
た。これらのことから垂直磁気異方性を有するためには
結晶粒径約数Å〜数１００Åの微細結晶相が不可欠であ
ることがわかる。From observation with an electron microscope, Ts = 212 ° C.,
In the case of 287 ° C., fine crystal grains are present, and Ts = 3
It was found that the crystallinity was considerably advanced at 35 ° C. From these facts, it is understood that a fine crystal phase having a crystal grain size of about several Å to several hundred Å is indispensable to have perpendicular magnetic anisotropy.

【００５６】[0056]

【実施例４】Ｆｅ₆₅Ｎｄ₃₅の組成のスパッタ膜を基板温
度２１０〜２９０℃、Ａｒ圧力１〜２×１０^-1Ｔｏｒｒ
の条件で膜厚を変化させて作成し、トルクメータで磁気
異方性定数Ｋｕを求めた結果を図６に示す。Example 4 A sputtered film having a composition of Fe ₆₅ Nd ₃₅ was formed at a substrate temperature of 210 to 290 ° C. and an Ar pressure of 1 to 2 × 10 ^-1 Torr.
FIG. 6 shows the results of obtaining the magnetic anisotropy constant Ku with the torque meter, which was prepared by changing the film thickness under the condition of.

【００５７】図６中黒丸は垂直磁化膜を示し、白丸は薄
膜の膜面内の異方性を有する場合である。図６中の添数
は基板の温度を示す。前述の条件Ｋｕ≧1.5×１０⁶ｅｒ
ｇ／ｃｃを満たすためには、Ｄ0.3μｍ以上、さらにＫ
ｕ≧2.5×１０⁶ｅｒｇ／ｃｃを満足させるためには、膜
厚Ｄ約0.7μｍ以上が必要であることが判る。In FIG. 6, black circles indicate perpendicularly magnetized films, and white circles indicate anisotropy in the film plane of the thin film. The index number in FIG. 6 indicates the temperature of the substrate. The above condition Ku ≧ 1.5 × 10 ⁶ er
To satisfy g / cc, D 0.3 μm or more, and further K
It can be seen that a film thickness D of about 0.7 μm or more is necessary to satisfy u ≧ 2.5 × 10 ⁶ erg / cc.

【００５８】[0058]

【実施例５】Ｆｅ₆₅Ｎｄ₃₅を基板温度２１０〜２９０
℃、膜厚６１４０〜１２６５０Åの条件でＡｒ圧を変化
させて作成したスパッタ膜の磁気異方性定数ＫｕのＡｒ
圧依存性を図７に示す。[Embodiment 5] Fe ₆₅ Nd ₃₅ was used at a substrate temperature of 210 to 290.
Ar of the magnetic anisotropy constant Ku of the sputtered film formed by changing the Ar pressure under the conditions of ℃ and film thickness of 6140 to 12650Å
The pressure dependence is shown in FIG.

【００５９】Ａｒ圧は２×１０^-1ＴｏｒｒあたりでＫｕ
は鈍いピークを示すが、相対的にＡｒ圧力依存性は他の
要因、すなわち基板温度や膜厚ほど顕著ではない。The Ar pressure is Ku around 2 × 10 ⁻¹ Torr.
Shows a dull peak, but the relative Ar pressure dependency is not so remarkable as other factors, that is, the substrate temperature and the film thickness.

【００６０】[0060]

【実施例６】Ｆｅ_100-xＮｄ_xにおいて、ｘ＝１８〜５０
の広い組成範囲において基板温度が２５０〜２８０℃、
Ａｒ圧１〜３×１０^-1Ｔｏｒｒ、膜厚６０００〜１３０
００Åのスパッタ薄膜を作成し、垂直磁気異方性定数Ｋ
ｕを求めた結果を図８に示す。Ｋｕの最大値はＮｄ４０
原子％辺りで得られ、１〜２×１０⁷ｅｒｇ／ｃｃにも
達する高い値を示す。Example 6 In Fe _100-x Nd _x , x = 18 to ₅₀
Substrate temperature of 250 to 280 ° C. in a wide composition range of
Ar pressure 1 to 3 × 10 ⁻¹ Torr, film thickness 6000 to 130
Create a 00 Å sputtered thin film and set the perpendicular magnetic anisotropy constant K
The result of obtaining u is shown in FIG. The maximum value of Ku is Nd40
It is obtained at around atomic% and shows a high value as high as 1-2 × 10 ⁷ erg / cc.

【００６１】Ｎｄ量がこれより減少する場合、Ｋｕは急
激に低下し、３１原子％未満では２．５×１０^６ｅｒｇ
／ｃｃ未満になるがＮｄ≧２５ａｔ％では製造条件に注
意すればＫｕ＞反磁界エネルギー２πＭｓ ^２ を満足し、
十分安定な垂直磁化膜となる。 When the amount of Nd is smaller than this, Ku decreases sharply, and when it is less than 31 atomic%, 2.5 × 10 ⁶ erg.
/ Cc but less than Nd ≧ 25at%
If desired, Ku> demagnetizing field energy 2πMs ² is satisfied,
It becomes a sufficiently stable perpendicular magnetic film.

【００６２】[0062]

【実施例７】Ｆｅ₆₀Ｎｄ₃₅Ｍ₅の組成でＭとしてＺｒ、
Ｈｆ、Ｂｉ、Ｖ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ｍｎ、
Ａｌ、Ｓｂ、Ｇｅ、Ｓｎ、Ｓｉ、Ｐｂ、ＮｉをＴｓ＝２
２０〜２９０℃、Ａｒ圧１〜２×１０^-1Ｔｏｒｒ、膜厚
６３００〜１１０００Åを作成し磁気特性を測定する。Example 7 A composition of Fe ₆₀ Nd ₃₅ M ₅ is Zr as M,
Hf, Bi, V, Nb, Ta, Cr, Mo, W, Mn,
Al, Sb, Ge, Sn, Si, Pb, Ni for Ts = 2
20 to 290 ° C., Ar pressure of 1 to 2 × 10 ⁻¹ Torr, and film thickness of 6300 to 11000Å are prepared and magnetic properties are measured.

【００６３】いずれもＫｕ≧2.5×１０⁶ｅｒｇ／ｃｃ、
カー回転角0.3°以上の垂直磁化膜が得られる。In all cases, Ku ≧ 2.5 × 10 ⁶ erg / cc,
A perpendicular magnetic film with a Kerr rotation angle of 0.3 ° or more can be obtained.

【００６４】[0064]

【実施例８】Ｆｅ₄₀Ｃｏ₂₅Ｎｄ₃₅の組成で、Ｔｓ＝２４
０℃、Ａｒ圧２×１０^-1Ｔｏｒｒ、膜厚７４００Åを作
成し、磁気特性を測定した。Example 8 A composition of Fe ₄₀ Co ₂₅ Nd ₃₅ and Ts = 24
A magnetic property was measured at 0 ° C., an Ar pressure of 2 × 10 ⁻¹ Torr, and a film thickness of 7400 Å.

【００６５】いずれもＫｕ≧2.5×１０⁶ｅｒｇ／ｃｃ以
上の垂直磁化膜が得られた。In all cases, a perpendicular magnetization film having a value of Ku ≧ 2.5 × 10 ⁶ erg / cc or more was obtained.

【００６６】[0066]

【実施例９】Ｆｅ₆₀Ｎｄ₂₅Ｐｒ₁₅の組成でＴｓ＝２６０
℃、Ａｒ圧1.5〜２×１０^-1Ｔｏｒｒ、膜厚７９００Å
のスパッタ薄膜を作成しＫｕ2.5×１０⁶ｅｒｇ／ｃｃ以
上の垂直磁化膜が得られた。Example 9 Composition of Fe ₆₀ Nd ₂₅ Pr ₁₅ and Ts = 260
℃, Ar pressure 1.5 to 2 × 10 ^-1 Torr, film thickness 7900Å
A sputtered thin film was prepared to obtain a perpendicular magnetization film of Ku2.5 × 10 ⁶ erg / cc or more.

【００６７】[0067]

【実施例１０】Ｆｅ₆₀Ｎｄ₃₂Ｄｙ₈、Ｆｅ₅₈Ｎｄ₃₂Ｃｅ
₁₀、Ｆｅ₅₇Ｎｄ₃₀Ｃｅ₁₀Ｖ₃の組成でＴｓ＝２４０〜２
９０℃、Ａｒ圧１〜２×１０^-1Ｔｏｒｒ、膜厚７３００
〜１１０００Åのスパッタ薄膜を作成し、Ｋｕ2.5×１
０⁶ｅｒｇ／ｃｃ以上の垂直磁化膜が得られた。Example 10 Fe ₆₀ Nd ₃₂ Dy ₈ and Fe ₅₈ Nd ₃₂ Ce
₁₀ , Fe ₅₇ Nd ₃₀ Ce ₁₀ V ₃ and Ts = 240-2
90 ° C., Ar pressure 1-2 × 10 ⁻¹ Torr, film thickness 7300
Create a sputtered thin film of ~ 11000Å, Ku2.5 × 1
A perpendicularly magnetized film of 0 ⁶ erg / cc or more was obtained.

【００６８】[0068]

【実施例１１】Ｆｅ₆₅Ｎｄ₃₅及びＦｅ₆₀Ｎｄ₄₀の組成
で、基板温度Ｔｓが各々２９０℃、２５０℃、Ａｒ圧２
×１０^-1Ｔｏｒｒ、膜厚が各々１２６５０Å、４８６０
Åのスパッタ膜を作成した。Ｆｅ₆₀Ｎｄ₄₀において4.2
〜３００Ｋで求めたトルク曲線を図９、図１０及び図１
１に示す。[Embodiment 11] Fe ₆₅ Nd ₃₅ and Fe ₆₀ Nd ₄₀ having a substrate temperature Ts of 290 ° C. and 250 ° C. and an Ar pressure of 2 respectively.
× 10 ^-1 Torr, film thickness 12650Å, 4860 respectively
A sputtered film of Å was created. 4.2 in Fe ₆₀ Nd ₄₀
The torque curves obtained at ˜300 K are shown in FIGS. 9, 10 and 1.
Shown in 1.

【００６９】また、１５ｋＯｅ磁界中での回転ヒステリ
シス損Ｗの低温での温度変化を図１１に示す。FIG. 11 shows the temperature change of the rotation hysteresis loss W at a low temperature in a magnetic field of 15 kOe.

【００７０】[0070]

【実施例１２】（Ｆｅ_1-yＣｏ_y）₆₀Ｎｄ₄₀、ｙ＝０、0.
075、0.15、0.25の組成でＡｒ圧が１〜２×１０^-1Ｔｏ
ｒｒ基板温度２３０〜２９０℃、膜厚７７００Å〜1.1
μｍの条件で作成した薄膜の結晶化温度Ｔｃｒｙ、キュ
リー温度Ｔｃ、垂直磁気異方性定数Ｋｕが最大値をとる
温度Ｔ₁、及び保磁力Ｈｃの変化を図１２に示す。Example 12 (Fe _1-y Co _y ) ₆₀ Nd ₄₀ , y = 0, 0.
075, 0.15, 0.25 composition with Ar pressure of 1-2 × 10 ^-1 To
rr substrate temperature 230 ~ 290 ℃, film thickness 7700Å ~ 1.1
FIG. 12 shows changes in the crystallization temperature Tcry, the Curie temperature Tc, the temperature T _{1 at} which the perpendicular magnetic anisotropy constant Ku takes the maximum value, and the coercive force Hc of the thin film formed under the condition of μm.

【００７１】Ｃｏの増加はＴｃｒｙを変化させないでＴ
ｃ、Ｈｃ、及びＴ₁の増加をもたらす。Increasing Co does not change Tcry but changes T
It results in an increase in c, Hc, and T ₁ .

【００７２】[0072]

【実施例１３】実施例１で得られたＮｄ₃₅Ｆｅ₆₅及び実
施例１２で得られた（Ｆｅ_1-yＣｏ_y）₆₀Ｎｄ₄₀の薄膜
に、入射角８０°の直線偏光した光（水銀ランプ光源、
波長λ＝２３０〜８３０ｎｍ、ハーフミラーは用いず）
を用いて、測定は薄膜表面側より行なった。測定装置は
日本分光株式会社製「磁気−光学測定装置Ｊ−２５０」
を用いてカー回転角θ_kの波長λ依存性を求めた（図１
３）。図中Ｃｏ５、Ｃｏ１０、Ｃｏ１５は夫々ｙ＝５／
６０（＝0.083）、１０／６０（＝0.17）、１５／６０
（＝0.25）に対応する。Example 13 A thin film of Nd ₃₅ Fe ₆₅ obtained in Example 1 and (Fe _1-y Co _y ) ₆₀ Nd ₄₀ obtained in Example 12 was linearly polarized with an incident angle of 80 ° (mercury). Lamp light source,
(Wavelength λ = 230-830 nm, half mirror not used)
Was measured from the thin film surface side. The measuring device is JASCO Corporation "Magnetic-optical measuring device J-250".
Was used to determine the wavelength λ dependence of the Kerr rotation angle θ _k (Fig. 1
3). In the figure, Co5, Co10, and Co15 are y = 5 /, respectively.
60 (= 0.083), 10/60 (= 0.17), 15/60
Corresponds to (= 0.25).

【００７３】低波長側で回転角は正、λ＝３４０ｎｍ付
近でθ_kはほぼ０、それ以上の波長領域では｜θ_k｜は急
に増加し、λ＞５００ｎｍではほぼ一定となるがすべて
の組成についてλ＝４００〜５００ｎｍで最大値をとっ
ている。λ＝５００及び６３３ｎｍにおける｜θ_k｜の
組成依存性を図１４に示す。Ｃｏ組成ｙの増加と共に｜
θ_k｜は増加しｙ＝0.25付近でほぼピークを示してい
る。λ＝５００及び６３３ｎｍでの値はｙ＝0.25で0.55
°及び0.45°である。これらの値は従来のＧｄ−Ｆｅ−
Ｃｏ系統の値よりはるかに大きいものである。The rotation angle is positive on the low wavelength side, θ _k is almost 0 in the vicinity of λ = 340 nm, and | θ _k | increases sharply in the wavelength region above λ> 500 nm, but becomes almost constant at all λ> 500 nm. The maximum value of the composition is taken at λ = 400 to 500 nm. FIG. 14 shows the composition dependence of | θ _k | at λ = 500 and 633 nm. With increase in Co composition y |
θ _k | increases and almost peaks near y = 0.25. The values at λ = 500 and 633 nm are 0.55 at y = 0.25.
And 0.45 °. These values are conventional Gd-Fe-
It is much larger than that of the Co system.

【００７４】[0074]

【実施例１４】実施例１３で用いたのと同じサンプルで
３００Ｋでの飽和磁化Ｍｓ及び垂直磁気異方性エネルギ
ー定数Ｋｕを求めた結果を図１５に示す。Ｆｅの一部に
対するＣｏによる置換量の増大と共に飽和磁化Ｍｓ及び
磁気異方性エネルギー定数Ｋｕを徐々に下げる。[Embodiment 14] FIG. 15 shows the results of determining the saturation magnetization Ms and the perpendicular magnetic anisotropy energy constant Ku at 300 K in the same sample used in Embodiment 13. The saturation magnetization Ms and the magnetic anisotropy energy constant Ku are gradually lowered with the increase of the substitution amount of Co for a part of Fe.

【００７５】[0075]

【実施例１５】実施例１と同じ条件で作成したＦｅ
_100-xＮｄ_xの組成の薄膜のカー回転角θ_k及び保磁力Ｈ
ｃを求め図１６に示す。Example 15 Fe prepared under the same conditions as in Example 1
Kerr rotation angle θ _k and coercive force H of a thin film having a composition of _100-x Nd _x
c is calculated and shown in FIG.

【００７６】Ｎｄ３５及び５０ａｔ％膜（膜作製直後に
厚さ約１００〜３００Å、表面を酸化させた膜）のカー
回転角は図１６の矢印で示すように増加することがわか
った。例えばＮｄ５０ａｔ％の場合θ_kは0.3°から約0.
6°（λ＝６３３ｎｍ）であり２倍近い増加を示してい
る。このことは表面を酸化させることにより多重干渉法
によりカー及びファラデー効果の両方の寄与を得て実効
的カー回転角が増加した為である。本方法は従来の重希
土類−鉄族垂直磁化膜ではＳｉＯ等の膜を表面上コーテ
ィングして回転角を増加させていた方法と異なり磁性膜
の表面をそのまま酸化させ回転角を増加することができ
る方法である。このことは本垂直磁化膜の特徴である。It was found that the Kerr rotation angle of the Nd35 and 50 at% film (a film having a thickness of about 100 to 300 Å immediately after film formation and having its surface oxidized) increased as shown by the arrow in FIG. For example, when Nd is 50 at%, θ _k is 0.3 ° to about 0.
The angle is 6 ° (λ = 633 nm), which is an almost double increase. This is because by oxidizing the surface, the contribution of both Kerr and Faraday effect is obtained by the multiple interference method, and the effective Kerr rotation angle is increased. This method can increase the rotation angle by oxidizing the surface of the magnetic film as it is, unlike the method of coating the surface of the conventional heavy rare earth-iron group perpendicular magnetization film with SiO or the like to increase the rotation angle. Is the way. This is a characteristic of this perpendicular magnetization film.

【００７７】薄膜表面の酸化皮膜はスパッタ後そのまま
装置内にて１００〜１５０℃で凡そ３０分〜１時間保持
することによって得られる。The oxide film on the surface of the thin film can be obtained by holding it in the apparatus at 100 to 150 ° C. for about 30 minutes to 1 hour after sputtering.

【００７８】ＳｉＯコーティングもｘ＝３５原子％の同
様なサンプルの表面に施した。その結果を図１６に示
す。ＳｉＯコーティングもカー回転角を増大させる。酸
化皮膜上にさらにＳｉＯコーティングを施すことによ
り、さらにθ_k、保護効果を増大できる。A SiO coating was also applied to the surface of a similar sample with x = 35 atomic%. The result is shown in FIG. The SiO coating also increases the Kerr rotation angle. By further applying SiO coating on the oxide film, θ _k and the protective effect can be further increased.

【００７９】[0079]

【実施例１６】実施例１５と同じ試料を用いて垂直磁気
異方性定数Ｋｕの温度依存性を求めた。（図１７）Example 16 The same sample as in Example 15 was used to determine the temperature dependence of the perpendicular magnetic anisotropy constant Ku. (Figure 17)

【００８０】Ｋｕは低温で増加し、ある温度Ｔ₁で最大
値をとった後、さらに低下する。Ku increases at a low temperature, reaches a maximum value at a certain temperature T ₁ , and then further decreases.

【００８１】[0081]

【実施例１７】レーザ光による書き込み実験 実施例１と同じ方法で得られた厚さ約４０００ÅのＮｄ
₃₈Ｆｅ₆₂膜についてレーザ光による書き込み実験を行な
った。Example 17 Writing Experiment by Laser Light Nd having a thickness of about 4000Å obtained by the same method as in Example 1
A writing experiment using a laser beam was performed on the ₃₈ Fe ₆₂ film.

【００８２】レーザ：半導体レーザ（パワー２０ｍＷ）
バイアス磁界〜１００Ｏｅ 線書込み方式 この結果幅約２〜１０μｍのビットが書き込めているこ
とがカー効果を利用した偏光顕微鏡により確認された。Laser: Semiconductor laser (power 20 mW)
Bias magnetic field to 100 Oe line writing system As a result, it was confirmed by a polarization microscope using the Kerr effect that bits having a width of about 2 to 10 μm could be written.

【００８３】[0083]

【実施例１８】図１８に本発明により２２０℃で作った
１５０Å厚のＦｅ₆₀Ｎｄ₄₀垂直磁化膜の微細結晶構造の
透過電子顕微鏡写真を矢印部分の領域の回折パターンと
共に示す。スペーシング0.2ｎｍ、クラスタ径２〜１０
ｎｍ、平均３〜５ｎｍを示す。EXAMPLE 18 FIG. 18 shows a transmission electron micrograph of a fine crystal structure of a 150Å-thick Fe ₆₀ Nd ₄₀ perpendicularly magnetized film produced at 220 ° C. according to the present invention, together with a diffraction pattern in a region indicated by an arrow. Spacing 0.2 nm, cluster diameter 2-10
nm, showing an average of 3 to 5 nm.

【００８４】[0084]

【実施例１９】Ｆｅ₄₅Ｃｏ₁₅Ｎｄ₃₅Ｍ₅の組成でＭとし
てＺｒ、Ｈｆ、Ｖ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ａｌ、Ｔ
ｉをＴｓ＝２１０〜２８５℃、Ａｒ圧１〜２×１０^-1Ｔ
ｏｒｒ、膜厚５３００〜１２０００Åの膜を作成し、磁
気特性を測定した。EXAMPLE 19 Zr, Hf, V, Nb, Ta, Cr, Mo, Al, and T are used as M in the composition of Fe ₄₅ Co ₁₅ Nd ₃₅ M _5.
i is Ts = 210 to 285 ° C., Ar pressure is 1 to 2 × 10 ⁻¹ T
A film having an orr and a film thickness of 5300 to 12000Å was formed, and the magnetic characteristics were measured.

【００８５】いずれもＫｕ≧2.5×１０⁶ｅｒｇ／ｃｃ以
上、カー回転角θ_kが0.4°以上の垂直磁化膜が得られ
た。In all cases, a perpendicular magnetic film having a value of Ku ≧ 2.5 × 10 ⁶ erg / cc or more and a Kerr rotation angle θ _k of 0.4 ° or more was obtained.

【００８６】[0086]

【実施例２０】実施例１、７、１２、１８と同様にして
得られたＦｅ₆₅Ｎｄ₃₅、Ｆｅ₆₀Ｎｄ₃₅Ｍ₅、（Ｍ＝Ｚ
ｒ、Ｈｆ、Ｖ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ａｌ、Ｂｉ、
Ｍｎ、Ｓｂ、Ｇｅ、Ｓｎ、Ｎｉ、Ｓｉ）、Ｆｅ₄₅Ｃｏ₁₅
Ｎｄ₄₀、Ｆｅ₄₅Ｃｏ₁₅Ｎｄ₃₅Ｍ₅（Ｍ＝Ｚｒ、Ｈｆ、
Ｖ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ａｌ、Ｔｉ、Ｎｉ、Ｓ
ｉ）の各薄膜を１規定食塩水中に２０分間浸漬後、８５
℃８５％ＲＨ（相対湿度）で２時間時効処理を行ない、
光学顕微鏡を用いて孔食の観察を行なった。孔食に対す
る耐食性はＦｅＣｏＮｄＭが最も優れており、次ぎにＦ
ｅＣｏＮｄ、ＦｅＮｄＭ（Ｍ＝Ｚｒ、Ｈｆ、Ｖ、Ｎｂ、
Ｔａ、Ｃｒ、Ｍｏ、Ａｌ、Ｎｉ、Ｓｉ）が良く、ＦｅＮ
ｄ及びＦｅＮｄＭ（Ｍ＝Ｂｉ、Ｍｎ、Ｓｂ、Ｇｅ、Ｓ
ｎ）は孔食が比較上最も進行していた。Example 20 Fe ₆₅ Nd ₃₅ , Fe ₆₀ Nd ₃₅ M ₅ and (M = Z obtained in the same manner as in Examples 1, 7, 12, and 18)
r, Hf, V, Nb, Ta, Cr, Mo, Al, Bi,
Mn, Sb, Ge, Sn, Ni, Si), Fe ₄₅ Co ₁₅
Nd ₄₀ , Fe ₄₅ Co ₁₅ Nd ₃₅ M ₅ (M = Zr, Hf,
V, Nb, Ta, Cr, Mo, Al, Ti, Ni, S
After dipping each thin film of i) in 1N saline for 20 minutes, 85
Aged at 85 ° C RH (relative humidity) for 2 hours,
The pitting corrosion was observed using an optical microscope. FeCoNdM has the best corrosion resistance against pitting corrosion, and then F
eCoNd, FeNdM (M = Zr, Hf, V, Nb,
Ta, Cr, Mo, Al, Ni, Si) is good, and FeN
d and FeNdM (M = Bi, Mn, Sb, Ge, S
In n), pitting corrosion was the most advanced in comparison.

【００８７】[0087]

【実施例２１】Ｆｅ_100-xＰｒ_x（ｘ＝２０、３０、４
０、５０原子％）の組成の薄膜を次の条件で作成した。
Ａｒ圧２×１０^-1Ｔｏｒｒ、Ｔｓは各々２９０℃と２７
０℃、Ｄは各々８２００Å（0.82μｍ）と９４００Å
（0.94μｍ）であった。Example 21 Fe _100-x Pr _x (x = 20, 30, 4
A thin film having a composition of 0, 50 atomic% was prepared under the following conditions.
Ar pressure 2 × 10 ⁻¹ Torr and Ts are 290 ° C. and 27, respectively.
0 ℃, D is 8200Å (0.82μm) and 9400Å respectively
(0.94 μm).

【００８８】この２種類の薄膜について、実施例１２と
同様の方法で入射光線の波長λを変えた場合のカー回転
角θ_kを調べた。その結果を図１９に示す。Ｆｅ₇₀Ｐｒ
₃₀ではλ＝５００ｎｍ付近でカー回転角θ_kは最大値0.3
5°を示す。With respect to these two kinds of thin films, the Kerr rotation angle θ _k when the wavelength λ of the incident light beam was changed was examined by the same method as in Example 12. The result is shown in FIG. Fe ₇₀ Pr
_{At 30} , the maximum Kerr rotation angle θ _k is 0.3 near λ = 500 nm.
Indicates 5 °.

【００８９】さらにＰｒ濃度ｘ（原子％）に対するカー
回転角の関係を入射光線λ＝５００、６３３ｎｍで測定
した結果を図２０に示す。カー回転角θ_kはＰｒ３０原
子％付近で最大値をとる。FIG. 20 shows the result of measurement of the relationship between the Kerr rotation angle and the Pr concentration x (atomic%) with the incident light beam λ = 500 and 633 nm. The Kerr rotation angle θ _k takes a maximum value in the vicinity of Pr30 atomic%.

【図面の簡単な説明】[Brief description of drawings]

【図１】本発明の一実施例、Ｆｅ_100-xＮｄ_xスパッタ薄
膜の磁化温度特性を示すグラフ。FIG. 1 is a graph showing a magnetization temperature characteristic of a Fe _100-x Nd _x sputtered thin film according to an example of the present invention.

【図２】Ｆｅ_100-xＮｄ_x薄膜のキュリー温度Ｔｃ、結晶
化温度Ｔｃｒｙ、及び飽和磁化Ｍｓ（７７Ｋ及び３００
Ｋ）を示すグラフ。FIG. 2 shows the Curie temperature Tc, crystallization temperature Tcry, and saturation magnetization Ms (77 K and 300) of the Fe _100-x Nd _x thin film.
Graph showing K).

【図３】（ａ）〜（ｂ）は、Ｆｅ_100-xＮｄ_x（ｘ＝３
５、４０）スパッタ薄膜の７７Ｋ及び３００Ｋでの各磁
化曲線を示すグラフ。3 (a) and (b) are Fe _100-x Nd _x (x = 3).
5, 40) Graphs showing the respective magnetization curves of the sputtered thin film at 77K and 300K.

【図４】Ｆｅ₆₅Ｎｄ₃₅スパッタ薄膜の基板温度と垂直磁
気異方性定数Ｋｕの関係を示すグラフ。FIG. 4 is a graph showing the relationship between the substrate temperature of an Fe ₆₅ Nd ₃₅ sputtered thin film and the perpendicular magnetic anisotropy constant Ku.

【図５】Ｆｅ₆₅Ｎｄ₃₅スパッタ薄膜の各基板温度による
Ｘ線回折パターンを示すグラフ。FIG. 5 is a graph showing an X-ray diffraction pattern of a Fe ₆₅ Nd ₃₅ sputtered thin film at each substrate temperature.

【図６】Ｆｅ₆₅Ｎｄ₃₅スパッタ薄膜の厚さとＫｕの関係
を示すグラフ。FIG. 6 is a graph showing the relationship between the thickness of an Fe ₆₅ Nd ₃₅ sputtered thin film and Ku.

【図７】Ｆｅ₆₅Ｎｄ₃₅スパッタ薄膜のＡｒ圧とＫｕの関
係を示すグラフ。FIG. 7 is a graph showing the relationship between Ar pressure and Ku of a Fe ₆₅ Nd ₃₅ sputtered thin film.

【図８】Ｆｅ_100-xＮｄ_xスパッタ薄膜のＮｄ量とＫｕの
関係を示すグラフ。FIG. 8 is a graph showing the relationship between Nd amount and Ku of a Fe _100-x Nd _x sputtered thin film.

【図９】Ｆｅ₆₀Ｎｄ₄₀において4.2〜３００Ｋで求めた
トルク曲線を示すグラフ。FIG. 9 is a graph showing a torque curve obtained at 4.2 to 300 K in Fe ₆₀ Nd ₄₀ .

【図１０】Ｆｅ₆₀Ｎｄ₄₀において4.2〜３００Ｋで求め
たトルク曲線を示すグラフ。FIG. 10 is a graph showing a torque curve obtained at 4.2 to 300 K in Fe ₆₀ Nd ₄₀ .

【図１１】Ｆｅ_100-xＮｄ_x（ｘ＝３５、４０）スパッタ
薄膜のヒステリシス損Ｗの温度変化を示すグラフ。FIG. 11 is a graph showing a temperature change of hysteresis loss W of a Fe _100-x Nd _x (x = 35, 40) sputtered thin film.

【図１２】（Ｆｅ_1-yＣｏ_y）₆₀Ｎｄ₄₀について、Ｃｏ濃
度ｙと結晶化温度Ｔｃｒｙ、キュリー温度Ｔｃ、Ｋｕが
最大値をとる温度Ｔ₁、及び保磁力Ｈｃの関係を示すグ
ラフ（実施例１２）。FIG. 12 is a graph showing the relationship between Co concentration y, crystallization temperature Tcry, Curie temperature Tc, temperature T _{1 at} which Ku takes the maximum value, and coercive force Hc for (Fe _1-y Co _y ) ₆₀ Nd ₄₀ ( Example 12).

【図１３】（Ｆｅ_1-yＣｏ_y）₆₀Ｎｄ₄₀について、各Ｃｏ
濃度ｙにおける入射光線の波長λ（ｎｍ）カー回転角θ
_k（度）の関係を示すグラフ（実施例１３）。FIG. 13 is a graph of (Fe _1-y Co _y ) ₆₀ Nd ₄₀ for each Co.
Wavelength λ (nm) of incident light at density y Kerr rotation angle θ
_The graph which shows the relationship of _k (degree) (Example 13).

【図１４】λ＝５００及び６３３ｎｍにおけるカー回転
角｜θ_k｜のＣｏ量（ｙ）に対する関係を示すグラフ
（実施例１３）。FIG. 14 is a graph showing the relationship between the Kerr rotation angle | θ _k | and the Co amount (y) at λ = 500 and 633 nm (Example 13).

【図１５】実施例１３のＣｏ濃度ｙと、飽和磁化Ｍｓ及
び垂直磁気異方性定数Ｋｕの関係を示すグラフ（実施例
１４）。FIG. 15 is a graph showing the relationship between Co concentration y in Example 13, saturation magnetization Ms, and perpendicular magnetic anisotropy constant Ku (Example 14).

【図１６】Ｆｅ_100-xＮｄ_xについて、ｘとカー回転角｜
θ_k｜（度）及び保磁力Ｈｃの関係を示すグラフ（実施
例１５）。FIG. 16: x and Kerr rotation angle for Fe _100-x Nd _x |
The graph which shows the relationship of (theta) _k | (degree) and coercive force Hc (Example 15).

【図１７】実施例１５と同じ試料についてのＫｕの温度
依存性を示すグラフ（実施例１６）。FIG. 17 is a graph showing the temperature dependence of Ku for the same sample as in Example 15 (Example 16).

【図１８】本発明の一実施例の結晶構造を示す透過電子
顕微鏡写真。FIG. 18 is a transmission electron micrograph showing a crystal structure of an example of the present invention.

【図１９】Ｆｅ_100-xＰｒ_xの各ｘ（２０、３０、４０、
５０原子％）について、入射光線のλとカー回転角θ_k
（度）との関係を示すグラフ（実施例２１）。FIG. 19: Fe _100-x Pr _x x (20, 30, 40,
50 atom%), the incident light λ and the Kerr rotation angle θ _k
The graph which shows the relationship with (degree) (Example 21).

【図２０】図１８と同じ系について、Ｐｒ濃度ｘとカー
回転角θ_kの関係を示すグラフ。20 is a graph showing the relationship between Pr concentration x and Kerr rotation angle θ _k for the same system as FIG. 18.

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.⁶ 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｇ１１Ｂ 11/10 ５０１ Ａ 9075−5Ｄ Ｇ１１Ｃ 13/06 Ａ Ｈ０１Ｆ 10/14 ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁶ Identification code Internal reference number FI Technical display location G11B 11/10 501 A 9075-5D G11C 13/06 A H01F 10/14

Claims (4)

【特許請求の範囲】[Claims] 【請求項１】基板上に金属ガス凝集法により薄膜を形成
する垂直磁気記録媒体の製造方法において、基板温度を
１８０℃〜合金の結晶化温度以下の温度に保持して、式
ＲＦｅにより本質上表わされ、希土類元素Ｒ２５〜６０
原子％、残部Ｆｅから成り、Ｒの内７０原子％以上がＮ
ｄ及びＰｒの１種又は２種、なおＲの残部はＹ、Ｌａ、
Ｃｅ、Ｓｍ、Ｇｄ、Ｔｂ、Ｄｙ、Ｈｏ、Ｅｒ及びＹｂの
一種以上とする組成から成り、膜厚を０．３〜３μｍと
し、かつ薄膜の非晶質マトリックスに数Å〜数１００Å
の微細結晶相を少なくとも含むと共に垂直磁気異方性定
数Ｋｕが反磁界エネルギー２πＭｓ ^２ （Ｍｓは飽和磁
化）より大きな垂直磁気異方性を有し、さらに結晶化温
度Ｔｃｒｙとキュリー温度Ｔｃとの温度差Ｔｃｒｙ−Ｔ
ｃが１００℃以上である薄膜を形成することを特徴とす
る垂直磁気記録媒体の製造方法。1. A method of manufacturing a perpendicular magnetic recording medium in which a thin film is formed on a substrate by a metal gas agglomeration method, the substrate temperature is kept at 180 ° C. to a temperature equal to or lower than the crystallization temperature of the alloy, and the formula RFe is used. represented, rare earth elements R 25 ~60
Atomic%, balance Fe, 70% or more of R is N
one or two of d and Pr, the remainder of R is Y, La,
Ce, Sm, Gd, Tb, Dy, Ho, Er, and Yb, which have a composition of one or more, and have a film thickness of 0.3 to 3 μm, and a thin film amorphous matrix of several Å to several hundred Å.
Of the diamagnetic field energy of 2πMs ² (Ms is a saturation magnetic field).
Has a larger perpendicular magnetic anisotropy, and a temperature difference Tcry-T between the crystallization temperature Tcry and the Curie temperature Tc.
A method of manufacturing a perpendicular magnetic recording medium, which comprises forming a thin film having c of 100 ° C. or higher. 【請求項２】基板上に金属ガス凝集法により薄膜を形成
する垂直磁気記録媒体の製造方法において、基板温度を
１８０℃〜合金の結晶化温度以下の温度に保持して、式
Ｒ（Ｆｅ、Ｃｏ）により本質上表わされ、希土類元素Ｒ
２５〜６０原子％、３０原子％未満のＣｏ及び残部Ｆｅ
から成り、Ｒの内７０原子％以上がＮｄ及びＰｒの１種
又は２種、なおＲの残部はＹ、Ｌａ、Ｃｅ、Ｓｍ、Ｇ
ｄ、Ｔｂ、Ｄｙ、Ｈｏ、Ｅｒ及びＹｂの一種以上とする
組成から成り、膜厚を０．３〜３μｍとし、かつ薄膜の
非昌質マトリックスに数Å〜数１００Åの微細結晶相を
少なくとも含むと共に垂直磁気異方性定数Ｋｕが反磁界
エネルギー２πＭｓ ^２ （Ｍｓは飽和磁化）より大きな垂
直磁気異方性を有し、さらに結晶化温度Ｔｃｒｙとキュ
リー温度Ｔｃとの温度差Ｔｃｒｙ−Ｔｃが１００℃以上
である薄膜を形成することを特徴とする垂直磁気記録媒
体の製造方法。2. A method of manufacturing a perpendicular magnetic recording medium in which a thin film is formed on a substrate by a metal gas agglomeration method, the substrate temperature is maintained at 180 ° C. to a temperature not higher than the crystallization temperature of the alloy, and the formula R (Fe, Co), essentially represented by the rare earth element R
25-60 atomic%, less than 30 atomic% Co and the balance Fe
70% by atom or more of R is one or two of Nd and Pr, and the balance of R is Y, La, Ce, Sm, G
d, Tb, Dy, Ho, Er, and Yb, and the composition is one or more, and the film thickness is 0.3 to 3 μm.
The non-matrix matrix contains at least a few Å to several hundred Å of a fine crystalline phase, and the perpendicular magnetic anisotropy constant Ku is a demagnetizing field.
A thin film having a perpendicular magnetic anisotropy larger than an energy of 2πMs ² (Ms is a saturation magnetization) and a temperature difference Tcry-Tc between the crystallization temperature Tcry and the Curie temperature Tc of 100 ° C. or more is formed. A method of manufacturing a perpendicular magnetic recording medium, comprising: 【請求項３】基板上に金属ガス凝集法により薄膜を形成
する垂直磁気記録媒体の製造方法において、基板温度を
１８０℃〜合金の結晶化温度以下の温度に保持して、式
ＲＦｅＭにより本質上表わされ、希土類元素Ｒ２５〜６
０原子％、ＭＯ〜１０原子％、及び残部Ｆｅから成り、
Ｒの内７０原子％以上がＮｄ及びＰｒの１種又は２種、
なおＲの残部はＹ、Ｌａ、Ｃｅ、Ｓｍ、Ｇｄ、Ｔｂ、Ｄ
ｙ、Ｈｏ、Ｅｒ及びＹｂの一種以上、ＭはＮｉ、Ｖ、Ｔ
ａ、Ｃｒ、Ｍｏ、Ｗ、Ｍｎ、Ｂｉ、Ａｌ、Ｓｉ、Ｐｂ、
Ｓｎ及びＳｂの少なくとも一種以上とする組成から成
り、膜厚を０．３μ〜３μｍとし、かつ薄膜の非晶質マ
トリックスに数Å〜数１００Åの微細結晶相を少なくと
も含むと共に垂直磁気異方性定数Ｋｕが反磁界エネルギ
ー２πＭｓ ^２ （Ｍｓは飽和磁化）より大きな垂直磁気異
方性を有し、さらに結晶化温度Ｔｃｒｙとキュリー温度
Ｔｃとの温度差Ｔｃｒｙ−Ｔｃが１００℃以上である薄
膜を形成することを特徴とする垂直磁気記録媒体の製造
方法。3. A method of manufacturing a perpendicular magnetic recording medium in which a thin film is formed on a substrate by a metal gas agglomeration method, the substrate temperature is maintained at 180 ° C. to a temperature equal to or lower than the crystallization temperature of the alloy, and is essentially expressed by the formula RFeM. represented, rare earth elements R 25 ~6
0 atomic%, MO-10 atomic%, and the balance Fe,
70% by atom or more of R is one or two of Nd and Pr,
The rest of R is Y, La, Ce, Sm, Gd, Tb, D.
One or more of y, Ho, Er and Yb, M is Ni, V, T
a, Cr, Mo, W, Mn, Bi, Al, Si, Pb,
It has a composition of at least one of Sn and Sb, a film thickness of 0.3 μm to 3 μm, and a thin film amorphous matrix.
The trick contains at least several Å to several hundred Å of a fine crystalline phase, and the perpendicular magnetic anisotropy constant Ku is demagnetizing field energy.
-2πMs ² (Ms is a saturation magnetization) , which has a larger perpendicular magnetic anisotropy, and further forms a thin film having a temperature difference Tcry-Tc of 100 ° C. or more between the crystallization temperature Tcry and the Curie temperature Tc. Method for manufacturing perpendicular magnetic recording medium. 【請求項４】基板上に金属ガス凝集法により薄膜を形成
する垂直磁気記録媒体の製造方法において、基板温度を
１８０℃〜合金の結晶化温度以下の温度に保持して、式
Ｒ（Ｆｅ、Ｃｏ）Ｍにより本質的に表わされ、希土類元
素Ｒ２５〜６０原子％、Ｍ０〜１０原子％、Ｃｏ３０原
子％未満、及び残部Ｆｅから成り、Ｒの内７０原子％以
上がＮｄ及びＰｒの１種又は２種、なおＲの残部はＹ、
Ｌａ、Ｃｅ、Ｓｍ、Ｇｄ、Ｔｂ、Ｄｙ、Ｈｏ、Ｅｒ及び
Ｙｂの一種以上、ＭはＮｉ、Ｚｒ、Ｖ、Ｔａ、Ｃｒ、Ｍ
ｏ、Ｗ、Ｍｎ、Ｂｉ、Ａｌ、Ｓｉ、Ｐｂ、Ｓｎ及びＳｂ
の少なくとも一種以上とする組成から成り、膜厚を０．
３μ〜３μｍとし、かつ薄膜の非晶質マトリックスに数
Å〜数１００Åの微細結晶相を少なくとも含むと共に垂
直磁気異方性定数Ｋｕが反磁界エネルギー２πＭｓ
^２ （Ｍｓは飽和磁化）より大きな垂直磁気異方性を有
し、さらに結晶化温度Ｔｃｒｙとキュリー温度Ｔｃとの
温度差Ｔｃｒｙ−Ｔｃが１００℃以上である薄膜を形成
することを特徴とする垂直磁気記録媒体の製造方法。4. A thin film is formed on a substrate by a metal gas aggregation method.
In the method of manufacturing the perpendicular magnetic recording medium,
Hold at a temperature of 180 ° C to the crystallization temperature of the alloy or lower,
Essentially represented by R (Fe, Co) M, a rare earth element
Elementary R25~ 60 atom%, M0-10 atom%, Co30 raw
Less than%, and the balance Fe, and 70% by atom or more of R
The top is one or two of Nd and Pr, and the rest of R is Y,
La, Ce, Sm, Gd, Tb, Dy, Ho, Er and
One or more types of Yb, M is Ni, Zr, V, Ta, Cr, M
o, W, Mn, Bi, Al, Si, Pb, Sn and Sb
Of at least one type and having a film thickness of 0.
3 μm to 3 μm, andFor thin film amorphous matrixnumber
Å to several hundred Å containing at least a fine crystalline phase
Direct magnetic anisotropy constant KuIs demagnetizing field energy 2πMs
^Two (Ms is saturation magnetization)With perpendicular magnetic anisotropy
Of the crystallization temperature Tcry and the Curie temperature Tc
The temperature difference Tcry-Tc is100Form a thin film above ℃
A method of manufacturing a perpendicular magnetic recording medium, comprising: