JP2668470B2 - Method for manufacturing soft magnetic film - Google Patents

Method for manufacturing soft magnetic film

Info

Publication number
JP2668470B2
JP2668470B2 JP3266818A JP26681891A JP2668470B2 JP 2668470 B2 JP2668470 B2 JP 2668470B2 JP 3266818 A JP3266818 A JP 3266818A JP 26681891 A JP26681891 A JP 26681891A JP 2668470 B2 JP2668470 B2 JP 2668470B2
Authority
JP
Japan
Prior art keywords
film
soft magnetic
substrate
amorphous
amorphous film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
JP3266818A
Other languages
Japanese (ja)
Other versions
JPH0582379A (en
Inventor
治 清水
寛次 中西
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujifilm Holdings Corp
Original Assignee
Fuji Photo Film Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Fuji Photo Film Co Ltd filed Critical Fuji Photo Film Co Ltd
Priority to JP3266818A priority Critical patent/JP2668470B2/en
Publication of JPH0582379A publication Critical patent/JPH0582379A/en
Application granted granted Critical
Publication of JP2668470B2 publication Critical patent/JP2668470B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15308Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni

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  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Thin Magnetic Films (AREA)
  • Magnetic Heads (AREA)
  • Soft Magnetic Materials (AREA)

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、磁気ヘッドのコア材料
等に好適な軟磁性膜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 producing a soft magnetic film suitable for a core material of a magnetic head.

【0002】[0002]

【発明の背景】例えばオーディオテープレコーダやVT
R(ビデオテープレコーダ)等の磁気記録再生装置にお
いては、記録信号の高密度化や高品質化等が進められて
おり、この高記録密度化に対応して、磁気記録媒体とし
て磁性粉にFe、Co、Ni等の金属あるいは合金から
なる粉末を用いた、いわゆるメタルテープや、強磁性金
属材料を真空薄膜形成技術によりベースフィルム上に直
接被着した、いわゆる蒸着テープ等が開発され、各分野
で実用化されている。
BACKGROUND OF THE INVENTION For example, audio tape recorders and VTs
In magnetic recording / reproducing apparatuses such as R (video tape recorder), recording signals have been increased in density and quality, and in response to this increase in recording density, Fe has been added to magnetic powder as a magnetic recording medium. So-called metal tapes using powders of metals or alloys such as Co, Ni, etc., and so-called vapor-deposited tapes in which a ferromagnetic metal material is directly applied on a base film by a vacuum thin film forming technique have been developed. Has been put to practical use.

【0003】[0003]

【従来の技術】ところで、このような所定の保磁力を有
する磁気記録媒体の特性を発揮せしめるためには、磁気
ヘッドのコア材料の特性として、高い飽和磁束密度Bs
を有するとともに、同一の磁気ヘッドで再生を行なおう
とする場合においては、高透磁率を併せて有することが
要求される。
2. Description of the Related Art In order to exhibit the characteristics of a magnetic recording medium having such a predetermined coercive force, the core material of a magnetic head must have a high saturation magnetic flux density Bs.
In addition, in the case where reproduction is to be performed with the same magnetic head, it is required to have high magnetic permeability.

【0004】このような要求を満足するものとして、特
開平2−275605号公報には、Feabc(但
し、a、b、cは各々原子%を示し、BはZr、Hf、
Ti、Nb、Ta、V、Mo、Wの少なくとも1種以上
を表わす。)なる組成式で示され、その組成範囲は 0<b≦20 0<c≦22 の範囲(但し、b≦7.5かつc≦5を除く)であるこ
とを特徴とする軟磁性薄膜、が記載され、そして、この
軟磁性薄膜は、例えばRFスパッタ法等の気相析着法に
より前記特定組成の非晶質薄膜を得て、この非晶質薄膜
を例えば350〜650℃で熱処理し前記非晶質薄膜の
一部ないし全部を結晶化させて製造することができる点
が記載されている。
In order to satisfy such a requirement, Japanese Patent Laid-Open No. 2-275605 discloses Fe a B b N c (where a, b and c each represent atomic%, B represents Zr, Hf,
It represents at least one of Ti, Nb, Ta, V, Mo, and W. ), The composition range is 0 <b ≦ 20 0 <c ≦ 22 (provided that b ≦ 7.5 and c ≦ 5 are excluded), a soft magnetic thin film, This soft magnetic thin film is obtained by, for example, vapor deposition method such as RF sputtering method to obtain an amorphous thin film having the above-mentioned specific composition, and the amorphous thin film is heat treated at 350 to 650 ° C., for example. It is described that a part or all of the amorphous thin film can be manufactured by crystallization.

【0005】[0005]

【発明が解決しようとする課題】しかし、前記軟磁性薄
膜の製造方法により、一定の膜厚以上の軟磁性膜を形成
したところ、軟磁性膜が、基板から剥離した状態で形成
される場合があった。そのため、一定の膜厚以上の前記
軟磁性膜をコアとして用いた磁気ヘッドを製造する際に
は、磁気ヘッドの歩留を低下させていた。
However, when a soft magnetic film having a certain thickness or more is formed by the method for manufacturing a soft magnetic thin film, the soft magnetic film may be formed in a state of being separated from the substrate. there were. Therefore, when manufacturing a magnetic head using the soft magnetic film having a certain film thickness or more as a core, the yield of the magnetic head is reduced.

【0006】本発明の目的は、特開平2−275605
号公報に記載の軟磁性薄膜及びその一部を他の元素で置
き換えて得られる軟磁性薄膜を、膜厚を厚くして基板上
に形成した場合に発生する上記問題点を解決する軟磁性
膜の製造方法を提供することにある。
[0006] An object of the present invention is to solve the problem described in JP-A-2-275605.
Patent application title: Soft magnetic thin film described in Japanese Patent Application Laid-Open Publication No. H10-15095 and a soft magnetic thin film obtained by replacing a part thereof with another element and forming the soft magnetic thin film on a substrate with a large thickness It is to provide a manufacturing method of.

【0007】[0007]

【課題を解決するための手段】本発明によれば、次の軟
磁性膜の製造方法により上記目的を達成することができ
る。
According to the present invention, the above object can be achieved by the following method for manufacturing a soft magnetic film.

【0008】(a)Fea-mmbc(但し、a、b、
c、mは各々原子%を示し、mは0の場合もあり、Mは
Co、Ru、Cr、V、Ni、Mn、Pd、Ir、Pt
の少なくとも1種以上を表わし、BはZr、Hf、T
i、Nb、Ta、Mo、Wの少なくとも1種以上を表わ
す。)なる組成式で示される非晶質膜を減圧下で基板上
に形成する工程 b)引続き減圧下で、かつ、前記非晶質膜の製膜温度よ
り高温で前記非晶質膜を保持する工程 c)その後前記非晶質膜を微結晶化するための熱処理工
程、を含み、生成軟磁性膜の組成範囲を前記組成式にお
いて、 0≦m/a<0.3 0<b≦20 0<c≦22 の範囲(但し、b≦7.5かつc≦5を除く)に制御す
る軟磁性膜の製造方法。
[0008] (a) Fe am M m B b N c ( where, a, b,
c and m each represent atomic%, m may be 0, and M is Co, Ru, Cr, V, Ni, Mn, Pd, Ir, Pt.
Of at least one of Br is represented by Zr, Hf, T
represents at least one of i, Nb, Ta, Mo, and W. B) a step of forming an amorphous film represented by the composition formula on a substrate under reduced pressure b) continuing to hold the amorphous film under reduced pressure and at a temperature higher than the film forming temperature of the amorphous film And a heat treatment step for microcrystallizing the amorphous film, wherein the composition range of the soft magnetic film to be formed is 0 ≦ m / a <0.3 0 <b ≦ 200 <C ≦ 22 (however, b ≦ 7.5 and c ≦ 5 are excluded), a method for producing a soft magnetic film.

【0009】なお、上記組成式において、a+b+c=
100である。
In the above composition formula, a + b + c =
100.

【0010】前記(a)の工程において、好ましくは基
板を水冷する。
In the step (a), the substrate is preferably water-cooled.

【0011】前記(b)の保持工程の後に、好ましくは
非晶質膜を冷却する。
After the holding step (b), the amorphous film is preferably cooled.

【0012】また、前記(b)の保持工程において、好
ましくは非晶質膜を結晶化温度以下、より好ましくは結
晶化温度より50℃以上低い温度で保持する。
In the holding step (b), the amorphous film is preferably held at a crystallization temperature or lower, more preferably at a temperature 50 ° C. or higher lower than the crystallization temperature.

【0013】本発明者が軟磁性膜の基板からの剥離につ
いて鋭意調査したところ、RFスパッタ法等の減圧下に
おける気相析着法により非晶質膜を製膜した後に、前記
非晶質膜を製膜したスパッタ装置のチャンバーを大気解
放すると、前記非晶質膜が基板から一定の割合で剥離す
ることがわかった。
The inventor of the present invention has made a diligent study on the peeling of the soft magnetic film from the substrate. As a result, the amorphous film is formed by the vapor deposition method under reduced pressure such as the RF sputtering method. It was found that when the chamber of the sputtering apparatus in which the film was formed was opened to the atmosphere, the amorphous film was separated from the substrate at a constant rate.

【0014】そこで、チャンバーを大気解放する前にチ
ャンバー内をさらに減圧しそのままアニール(150
℃)したところ、アニール後の非晶質薄膜は基板から剥
離しないということを見い出し、本発明を完成するに至
った。
Therefore, before the chamber is opened to the atmosphere, the inside of the chamber is further reduced in pressure and annealed as it is (150
° C), it was found that the annealed amorphous thin film did not peel off from the substrate, and the present invention was completed.

【0015】[0015]

【好適な実施態様】前記特定の組成式で示される非晶質
膜は、例えばRFスパッタ法等の減圧下における気相析
着法で形成することができる。RFスパッタ法により形
成する場合の雰囲気(例えばN2を含有したアルゴンガ
ス)の圧力は0.1〜0.6Paにすることができる。
Preferred Embodiment The amorphous film represented by the above specific composition formula can be formed by a vapor deposition method under reduced pressure such as an RF sputtering method. The pressure of the atmosphere (for example, argon gas containing N 2 ) when forming by RF sputtering can be set to 0.1 to 0.6 Pa.

【0016】RFスパッタ法においては、基板は一般に
水冷して行なうが、基板温度は150℃まで上昇させて
行なうこともできる。しかし、基板温度はより低温のほ
うが、組成がずれても安定して成膜できる。従って、好
ましくは基板を水冷する。
In the RF sputtering method, the substrate is generally cooled with water, but the substrate temperature can be raised to 150 ° C. However, when the substrate temperature is lower, a stable film can be formed even if the composition is shifted. Therefore, the substrate is preferably water cooled.

【0017】前記非晶質膜を形成する基板としては、例
えば、一般のフェライト基板、MnZn単結晶フェライ
ト基板、結晶化ガラス基板、単結晶サファイア基板等を
用いることができ、また、これらの基板表面にSiO2
膜等を有するものでもよい。
As the substrate on which the amorphous film is formed, for example, a general ferrite substrate, a MnZn single crystal ferrite substrate, a crystallized glass substrate, a single crystal sapphire substrate or the like can be used, and the surface of these substrates can be used. On SiO 2
It may have a film or the like.

【0017】前記非晶質膜を減圧下で基板上に形成した
後も、引続き減圧下で、かつ前記非晶質膜の製膜温度よ
り高温で前記非晶質膜を保持する。この際の非晶質膜の
保持圧力は、好ましくは製膜時の圧力以下にし、例えば
10-5Pa程度にする。また、非晶質膜の保持温度は、
結晶が生じない温度範囲であって、かつ、応力を緩和で
きる温度範囲で保持する。好ましくは結晶化温度以下、
より好ましくは結晶化温度より50〜100℃以上低い
温度で保持する。例えば300℃以下で保持する。保持
温度の下限は好ましくは100℃にする。なお、上記圧
力及び温度で前記非晶質膜を保持する時間は、約30分
〜1時間程度でよい。
Even after the amorphous film is formed on the substrate under reduced pressure, the amorphous film is kept under reduced pressure and at a temperature higher than the film forming temperature of the amorphous film. At this time, the holding pressure of the amorphous film is preferably equal to or lower than the pressure at the time of film formation, for example, about 10 -5 Pa. The holding temperature of the amorphous film is
The temperature is maintained in a temperature range where crystals are not generated and stress can be relaxed. Preferably below the crystallization temperature,
More preferably, the temperature is maintained at a temperature 50 to 100 ° C. lower than the crystallization temperature. For example, it is held at 300 ° C. or lower. The lower limit of the holding temperature is preferably 100 ° C. The time for holding the amorphous film at the above pressure and temperature may be about 30 minutes to 1 hour.

【0018】減圧下で基板上に形成した前記非晶質膜
を、引続き減圧下で、かつ前記特定の温度で保持する
と、大気圧下においても基板から前記非晶質膜が剥離し
ない。従って、前記(b)の工程を経た非晶質膜を例え
ば350〜650℃で熱処理して非晶質膜の一部ないし
全部を微結晶化して(例えば結晶粒径300オングスト
ローム以下)、前記組成式において前記特定組成範囲の
軟磁性薄膜を基板からの剥離なしに製造することができ
る。
When the amorphous film formed on the substrate under reduced pressure is continuously kept under reduced pressure and at the specific temperature, the amorphous film does not peel off from the substrate even under atmospheric pressure. Therefore, the amorphous film that has undergone the step (b) is heat-treated at, for example, 350 to 650 ° C. to microcrystallize a part or all of the amorphous film (for example, a crystal grain size of 300 Å or less), and the composition described above. In the formula, the soft magnetic thin film having the specific composition range can be manufactured without peeling from the substrate.

【0019】なお、生成する軟磁性膜の組成は、前記各
工程を経るので(例えば(C)の熱処理工程)その条件
(例えば温度及び時間)に応じて窒素が減少し、非晶質
膜の組成から変化することが多いが、最終的には前記特
定の組成範囲に制御する。
Since the composition of the soft magnetic film to be formed passes through each of the above steps (for example, the heat treatment step of (C)), nitrogen is reduced according to the conditions (for example, temperature and time), and the composition of the amorphous film is reduced. Although the composition often changes, the final composition range is controlled.

【0020】[0020]

【実施例】【Example】

【実施例1】Fe90Zr10の組成のターゲットを用い
て、6モル%のN2を含む窒素含有アルゴンガス雰囲気
中(圧力0.15Pa)で、陰極電力1KW(ターゲット直
径6インチ)、基板を水冷するという条件で、RFスパ
ッタ法により約7μmの厚さのFe−Zr−N非晶質薄
膜を基板上に形成した。
Example 1 A substrate having a composition of Fe 90 Zr 10 was used in a nitrogen-containing argon gas atmosphere containing 6 mol% N 2 (pressure 0.15 Pa), a cathode power of 1 kW (target diameter 6 inches), and a substrate. Under the condition of cooling with water, an Fe-Zr-N amorphous thin film having a thickness of about 7 μm was formed on the substrate by RF sputtering.

【0021】前記非晶質膜を形成後もRFスパッタ装置
の製膜用チャンバーを大気解放せずにそのままさらに減
圧して圧力5×10-5Paにし、その圧力を維持したま
ま150℃で1時間保持し、その後常温まで冷却してか
らチャンバーを大気解放した。基板としてはMIGヘッ
ド用に溝加工されたMnZn結晶フェライトを用いた。
After the amorphous film is formed, the film forming chamber of the RF sputtering apparatus is not further exposed to the atmosphere but further depressurized to a pressure of 5 × 10 −5 Pa, and the pressure is maintained at 150 ° C. for 1 hour. The chamber was held for a time and then cooled to room temperature, and then the chamber was exposed to the atmosphere. As the substrate, MnZn crystal ferrite grooved for the MIG head was used.

【0022】[0022]

【参考例1〜2】前記実施例1において、非晶質膜を基
板上に形成した後、ただちに前記チャンバーを大気解放
した(参考例1)。
Reference Examples 1 and 2 In Example 1, the amorphous film was formed on the substrate, and immediately thereafter, the chamber was exposed to the atmosphere (Reference Example 1).

【0023】参考例1の工程に引き続いて非晶質膜をそ
の後別の熱処理装置内で減圧下(圧力5×10-5Pa)
150℃で1時間保持し、常温まで冷却してから大気解
放した(参考例2)。
Subsequent to the process of Reference Example 1, the amorphous film is then subjected to reduced pressure (pressure 5 × 10 −5 Pa) in another heat treatment apparatus.
It was kept at 150 ° C. for 1 hour, cooled to room temperature, and then released to the atmosphere (Reference Example 2).

【0017】参考例1〜2の基板としては、実施例1と
同様のものを用いた。
The same substrates as in Example 1 were used as the substrates in Reference Examples 1 and 2.

【0024】[0024]

【基板からの非晶質膜の剥離試験】前記実施例1及び参
考例1〜2をそれぞれ10回ずつ行ない、最終的にギャ
ップ面になる面の非晶質膜の剥離の割合について調べ
た。その結果を表1に示す。前記実施例によれば、非晶
質膜の剥離が全く発生しないということが表1からわか
る。
[Peeling Test of Amorphous Film from Substrate] The above-mentioned Example 1 and Reference Examples 1 and 2 were carried out 10 times each, and the rate of peeling of the amorphous film on the surface to finally become the gap surface was examined. Table 1 shows the results. It can be seen from Table 1 that no peeling of the amorphous film occurs according to the embodiment.

【0025】[0025]

【表1】 [Table 1]

【0017】[0017]

【発明の効果】本発明の軟磁性膜の製造方法は、前記特
定の組成式で示される非晶質膜を減圧下で基板上に形成
した後も、さらに引続き減圧下で、かつ、前記非晶質膜
の製膜温度よりも高い温度で前記非晶質膜を保持するの
で、例えば膜厚10μmまでの前記非晶質膜の大気圧下
における基板からの剥離を防止することができる。その
ため、前記特定の組成式において前記特定の組成範囲の
軟磁性膜を基板から剥離させることなく形成することが
できる。
According to the method of manufacturing a soft magnetic film of the present invention, even after the amorphous film represented by the above specific composition formula is formed on the substrate under reduced pressure, it is further continuously reduced pressure and Since the amorphous film is held at a temperature higher than the film forming temperature of the crystalline film, it is possible to prevent the amorphous film having a film thickness of up to 10 μm from peeling from the substrate under atmospheric pressure. Therefore, the soft magnetic film having the specific composition range in the specific composition formula can be formed without peeling from the substrate.

【0026】従って、前記特定の組成式において前記特
定の組成範囲の軟磁性膜をコアとして用いた磁気ヘッド
を製造する際の歩留を上昇させることができる。
Therefore, it is possible to increase the yield in manufacturing a magnetic head using the soft magnetic film having the specific composition range as the core in the specific composition formula.

Claims (5)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 (a)Fea-mmbc(但し、a、b、c、mは各々
原子%を示し、mは0の場合もあり、MはCo、Ru、
Cr、V、Ni、Mn、Pd、Ir、Ptの少なくとも
1種以上を表わし、BはZr、Hf、Ti、Nb、T
a、Mo、Wの少なくとも1種以上を表わす。)なる組
成式で示される非晶質膜を減圧下で基板上に形成する工
程 (b)引続き減圧下で、かつ、前記非晶質膜の製膜温度
より高温で前記非晶質膜を保持する工程 (c)その後前記非晶質膜を微結晶化するための熱処理
工程、を含み、生成軟磁性膜の組成範囲を前記組成式に
おいて、 0≦m/a<0.3 0<b≦20 0<c≦22 の範囲(但し、b≦7.5かつc≦5を除く)に制御す
ることを特徴とする軟磁性膜の製造方法。
1. (a) Fe am M m B b N c (provided that a, b, c and m each represent atomic%, m may be 0, M may be Co, Ru,
Represents at least one of Cr, V, Ni, Mn, Pd, Ir, and Pt, and B represents Zr, Hf, Ti, Nb, T
and represents at least one of a, Mo, and W. (B) forming an amorphous film represented by the composition formula on the substrate under reduced pressure (b) maintaining the amorphous film under reduced pressure and at a temperature higher than the film forming temperature of the amorphous film. (C) a heat treatment step for microcrystallizing the amorphous film, and the composition range of the soft magnetic film to be formed is represented by the following composition formula: 0 ≦ m / a <0.3 0 <b ≦ A method for producing a soft magnetic film, wherein the soft magnetic film is controlled in a range of 200 <c ≦ 22 (however, excluding b ≦ 7.5 and c ≦ 5).
【請求項2】前記(a)の工程において、基板を水冷す
ることを特徴とする請求項1記載の軟磁性膜の製造方
法。
2. The method according to claim 1, wherein the substrate is water-cooled in the step (a).
【請求項3】前記(b)の保持工程の後に、非晶質膜を
冷却することを特徴とする請求項1又は2記載の軟磁性
膜の製造方法。
3. The method for producing a soft magnetic film according to claim 1, wherein the amorphous film is cooled after the holding step (b).
【請求項4】前記(b)の保持工程において、非晶質膜
を結晶化温度以下で保持することを特徴とする請求項1
〜3の一に記載の軟磁性膜の製造方法。
4. The method according to claim 1, wherein in the holding step (b), the amorphous film is held at a crystallization temperature or lower.
3. The method for manufacturing a soft magnetic film as described in 1 above.
【請求項5】前記(b)の保持工程において、非晶質膜
を結晶化温度より50℃以上低い温度で保持することを
特徴とする請求項1〜4の一に記載の軟磁性膜の製造方
法。
5. The soft magnetic film according to claim 1, wherein in the holding step (b), the amorphous film is held at a temperature lower than the crystallization temperature by 50 ° C. or more. Production method.
JP3266818A 1991-09-19 1991-09-19 Method for manufacturing soft magnetic film Expired - Fee Related JP2668470B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3266818A JP2668470B2 (en) 1991-09-19 1991-09-19 Method for manufacturing soft magnetic film

Publications (2)

Publication Number Publication Date
JPH0582379A JPH0582379A (en) 1993-04-02
JP2668470B2 true JP2668470B2 (en) 1997-10-27

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