JPS62271226A - Production of magnetic recording medium - Google Patents
Production of magnetic recording mediumInfo
- Publication number
- JPS62271226A JPS62271226A JP11646386A JP11646386A JPS62271226A JP S62271226 A JPS62271226 A JP S62271226A JP 11646386 A JP11646386 A JP 11646386A JP 11646386 A JP11646386 A JP 11646386A JP S62271226 A JPS62271226 A JP S62271226A
- Authority
- JP
- Japan
- Prior art keywords
- film
- thin
- thin film
- layer
- heat treatment
- 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.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 238000005546 reactive sputtering Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000000151 deposition Methods 0.000 claims abstract description 5
- 239000010409 thin film Substances 0.000 claims description 37
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 23
- 239000010408 film Substances 0.000 claims description 17
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 3
- 229910003145 α-Fe2O3 Inorganic materials 0.000 abstract 1
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 abstract 1
- 238000004544 sputter deposition Methods 0.000 description 8
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 241001191378 Moho Species 0.000 description 1
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
３、発明の詳細な説明
〔概要〕
磁気記録媒体の製造方法であって、非磁性の基板上に、
Ｆｅ （鉄）を母材とする反応性スパッタリングにより
α−Ｆｅｔｅ＞膜を被着した後、還元熱処理を行って下
地膜となるＦｅＪＯＶ膜を形成し、更に該Ｆｑ％膜（下
地膜）上にＦｅ母材の反応性スパッタリングを用いて、
Ｆｅ、７０−膜（第二層）を形成することにより、良好
な磁気特性を有するｒ−Ｆｅユ０３磁性薄膜を安定に形
成することを可能にしたものであＺる・
〔産業上の利用分野〕
本発明は、磁気ディスク装置に用いられる６ｉ１気記録
媒体の製造方法に関する。[Detailed Description of the Invention] 3. Detailed Description of the Invention [Summary] A method for manufacturing a magnetic recording medium, comprising:
After depositing an α-Fete film by reactive sputtering using Fe (iron) as a base material, reduction heat treatment is performed to form a FeJOV film as a base film, and further on the Fq% film (base film). Using reactive sputtering of Fe matrix,
By forming a Fe,70- film (second layer), it is possible to stably form an r-Fe Yu-03 magnetic thin film with good magnetic properties. Field] The present invention relates to a method of manufacturing a 6I1 recording medium used in a magnetic disk device.
磁気ディスク装置における記憶容量の増大化に伴い、磁
気記録媒体に対してより一層の記録の高密度化が要望さ
れている。これに対応して、近年従来のスピンコーティ
ングに代わって、薄膜化の容易なスパッタリング法によ
り磁気記録媒体を製造する研究開発が盛んに行われ、特
に膜自身が硬く、かつ化学的にも安定なγ−ＦｅｚＯｉ
ｌｄｆ性薄膜が注目されている。As the storage capacity of magnetic disk devices increases, there is a demand for higher recording densities in magnetic recording media. In response to this, in recent years there has been much research and development into manufacturing magnetic recording media using sputtering, which can easily produce thin films, instead of conventional spin coating. γ-FezOi
ldf thin films are attracting attention.
従来、スパッタリング法を用いてｒ −ＦｅＡＱ３１性
薄膜を有する磁気記録媒体の製造方法としては、第４図
に示すように例えば、アルマイト処理を施した層合金か
らなる円板状非磁性基板１上に、Ｆｅ（鉄）母材をＡｒ
−０１（アルゴン−酸素）雰囲気中で、反応スパックリ
ングしてＦｅ５０？薄膜２を形成した後、このｌ’ｅ３
０≠膜を大気中にて熱処理を行い、Ｔ−ＦｅＬＯ３磁性
薄膜３を得る直接酸化法等が一般に知られた方法である
。Conventionally, as a method for manufacturing a magnetic recording medium having an r -FeAQ31 thin film using a sputtering method, as shown in FIG. , Fe (iron) base material is Ar
-01 (Argon-Oxygen) atmosphere, reaction sputtering to Fe50? After forming the thin film 2, this l'e3
A generally known method is a direct oxidation method in which the T-FeLO3 magnetic thin film 3 is obtained by heat-treating the 0≠ film in the atmosphere.
従来の直接酸化法では、ｌ？ｃ（鉄）から中間酸化状態
であるＦｅ３Ｏ４の生成が、非磁性基板１へ飛来中、若
しくは非磁性基板１上で行われるため、スパッタパワー
、スパッタガス圧等といったスパッタリング条件に対す
る許容度が極めて狭く、かつ非磁性基板１表面の状態（
基板表面荒れ、清浄度）の影啓を受は易いと云う欠点が
ある。その為γ−ＦｅよＯＪ膜を形成する上で、その安
定性が大きな問題となっていた。In the conventional direct oxidation method, l? Since Fe3O4, which is in an intermediate oxidation state, is generated from c (iron) while flying to or on the nonmagnetic substrate 1, the tolerance for sputtering conditions such as sputtering power and sputtering gas pressure is extremely narrow. , and the state of the surface of the nonmagnetic substrate 1 (
The drawback is that it is easily affected by substrate surface roughness and cleanliness. Therefore, when forming an OJ film using γ-Fe, its stability has been a major problem.
第１図は本発明に係る磁気記録媒体の製造方法を工程順
に示す要部拡大断面図である。FIG. 1 is an enlarged cross-sectional view of a main part showing the method of manufacturing a magnetic recording medium according to the present invention in order of steps.
本問題点は、円板状非磁性基板１上に、Ｆｅ （鉄）を
母材とする反応性スパッタリングよりα−Ｆｅ・０コ薄
膜４を被着した後、還元熱処理を行って第一層のＰｅＪ
Ｏす薄膜５を形成し、該Ｆｅ３Ｏ４薄膜５ （第一層）
上にＦｅ母材の反応性スパッタリングにより、Ｆｅ５０
−薄膜６を被着することにより解決される。This problem is solved by depositing an α-Fe.O thin film 4 on a disc-shaped nonmagnetic substrate 1 by reactive sputtering using Fe (iron) as a base material, and then performing a reduction heat treatment to form the first layer. PeJ of
An O thin film 5 is formed, and the Fe3O4 thin film 5 (first layer)
By reactive sputtering of Fe matrix on top, Fe50
- solved by applying a thin film 6;
即ち、円板状非磁性基板１上にα−Ｆｅ、０３ 薄膜４
を還元熱処理して形成したＦｅ１Ｏ＠からなる下地薄膜
５を予め被着しておき、この下地膜＋１’Ｊ ５上に反
応性スパッタリングによりＦｅＪＯｓ薄膜６を形成すれ
ば、基板表面の形容を除去することができ、かつ第２層
のＦｅＪＯ＋薄膜６が、下地膜となる第一層のＦｅ３０
ｙ薄膜５の結晶性を受は継いだ形で形成されるので、反
応性スパッタリングの制御マージンを広げることができ
る゛。これらのＦｅＪ０４薄膜を大気中にて熱処理すれ
ば、良好な磁気特性ををするＴ−ＦｅユＯ８薄膜７を安
定に形成することが可能となる。That is, a thin film 4 of α-Fe, 03 is deposited on a disc-shaped nonmagnetic substrate 1.
If a base thin film 5 made of Fe1O@ formed by reduction heat treatment is deposited in advance, and a FeJOs thin film 6 is formed on the base film +1'J 5 by reactive sputtering, the shape of the substrate surface can be removed. and the second layer of FeJO+ thin film 6 is the first layer of Fe30 which serves as the base film.
Since it is formed in a manner that inherits the crystallinity of the y-thin film 5, it is possible to widen the control margin of reactive sputtering. If these FeJ04 thin films are heat-treated in the atmosphere, it becomes possible to stably form a T-FeO8 thin film 7 having good magnetic properties.
〔実施例］ 第１図を用いて本発明について説明する。〔Example] The present invention will be explained using FIG.
第１図に示すように、直径８インチの表面硬化されたガ
ラス基板（非磁性基板Ｉ）に、Ｔｉ、Ｃｏ、Ｃｕが微少
添加されたＦｅターゲノｌ−（２５０Ｘ１２５ ＊：）
を用いて、Ａｒ−０１雰囲気圧１．ＯＸ １０ Ｔｏ
ｒｒ。As shown in Fig. 1, a surface-hardened glass substrate (non-magnetic substrate I) with a diameter of 8 inches is coated with Fe target material (250X125*:) to which Ti, Co, and Cu are slightly added.
Using Ar-01 atmospheric pressure 1. OX 10 To
rr.
スパッタ電力２ＫＷ 、 ｌ板回転１０ｒｐｍにて反応
スパッタリングを行い、膜厚５００人のα−Ｆｅ工ｏ３
薄膜４を形成した。Reactive sputtering was performed at a sputtering power of 2 KW and a plate rotation of 10 rpm to form a film with a thickness of 500 mm.
A thin film 4 was formed.
その後α−Ｆｅ工Ｏ３薄膜を湿潤Ｈユ雰囲気中で還元熱
処理を行い、下地膜となるＦＯＪＯチ薄膜５ （第１層
）を形成した。Thereafter, the α-Fe-treated O3 thin film was subjected to a reduction heat treatment in a humid H atmosphere to form a FOJO thin film 5 (first layer) serving as a base film.
次に、上記Ｆｅ、Ｏい薄膜５下地上に、Ｃｏを微量含む
トｃターゲットをＡｒ−０Ｌ雰囲気圧０．５×耐Ｔｏｒ
ｒ、スパッタ電力１．ＯＫＷ 、基板温度２５０ ’Ｃ
の条件にて反応性スパッタリングして、１０００人のＦ
ｅ）Ｏｓ 薄膜６ （第２層）を形成し、その後節１、
第２層のＦｅ５０≠薄膜５．６を大気中にて熱処理を行
い、γ−ＦｅｚＯ５薄膜７を形成した。Next, a target containing a small amount of Co was placed on the Fe, O thin film 5 substrate at an Ar-0L atmospheric pressure of 0.5×Tor resistance.
r, sputtering power 1. OKW, substrate temperature 250'C
Reactive sputtering was performed under the conditions of 1000 F.
e) Form the Os thin film 6 (second layer), and then the nodes 1,
The second layer of Fe50≠thin film 5.6 was heat-treated in the atmosphere to form a γ-FezO5 thin film 7.
本実施例で得られたｒ−Ｆｅよ０３薄膜７の磁気特性（
Ｂ−Ｈ特性）を、第２図の表に示す。また比較のために
、下地のＦｅ３０１＋３膜５を形成せずに、ガラス基板
（非磁性基板１）上に直接酸化法で形成したＴ−Ｆｅ□
０３薄膜（膜厚１５００人）の磁気特性を併記しておく
。なお、第２図の表において、試料Ｉ、■、■はＡ ｒ
／ ０２の混合ガス比を変えて成膜したものである。Magnetic properties of the r-Fe 03 thin film 7 obtained in this example (
B-H characteristics) are shown in the table of FIG. For comparison, T-Fe
The magnetic properties of the 03 thin film (thickness: 1500 mm) are also listed below. In addition, in the table of Fig. 2, samples I, ■, and ■ are A r
The film was formed by changing the mixed gas ratio of /02.
−ＩｉＣにｒ−ＦｅｚＯ３薄膜の磁気特性としては、残
留磁束密度８ｒが２０００Ｇａｕｓｓ Ｊソ上、角形比
Ｓ（＝！４ｒ／Ｂｓ） 、Ｓ＊（＝ｌＩｘ／１ｌｃ）が
０．７以上が望ましい。As for the magnetic properties of the -IiC r-FezO3 thin film, it is desirable that the residual magnetic flux density 8r be 2000 Gauss J or higher, the squareness ratio S (=!4r/Bs), and S* (=lIx/1lc) be 0.7 or more.
第２図の表をみると、従来法で作成したサンプルは、流
量が５〜７ ｓｅｃｍの間で変化しただけで、モホ気特
性が著しく変化して劣化するものもあるが、本実施例に
より作成したサンプルは全て良好な６’ｔｌ気特性を示
している。Looking at the table in Figure 2, it can be seen that in some samples prepared using the conventional method, the moho characteristics significantly change and deteriorate even when the flow rate changes between 5 and 7 seconds, but with this example, All the prepared samples showed good 6'tl characteristics.
本発明は下地膜を入れることで、下地膜を引き継いた形
でその上にＦｅｊＯ≠薄膜が形成されるので、基板表面
の影響が除去され、且つ」二記表のように酸素流量をか
えても、良好な磁気特性が得られるので、反応性スパッ
タリングの制御マージンが広いことは明らかである。従
って、良好な磁気特性を有するγ−Ｆｅ２０３薄膜を安
定して形成することが可能となる。In the present invention, by inserting a base film, a FejO≠ thin film is formed on the base film in a manner that takes over the base film, so the influence of the substrate surface is removed, and the oxygen flow rate can be changed as shown in Table 2. It is clear that the control margin for reactive sputtering is wide because good magnetic properties can also be obtained. Therefore, it is possible to stably form a γ-Fe203 thin film having good magnetic properties.
以上説明したように本発明によれば、非磁性の円板状基
板表面の影響を下地膜を入れることにより除去すること
ができ、かつ、Ｆｅを母材とする反応性スパッタリング
の制御マージンを広げることが可能となることから、磁
気特性の優れたγ−Ｆ６λ０、薄膜を安定に形成するこ
とが出来る。As explained above, according to the present invention, the influence of the non-magnetic disk-shaped substrate surface can be removed by adding an underlayer, and the control margin for reactive sputtering using Fe as a base material can be expanded. This makes it possible to stably form a γ-F6λ0 thin film with excellent magnetic properties.
第１図は本発明に係る磁気記録媒体の製造方法を工程順
に示す要部拡大断面図、
第２図は磁気特性の比較表、
第３図はＢ−８曲線、
第４図は従来の磁気記録媒体の製造方法を説明するため
の要部拡大断面図である。
図において、
１は非磁性基板、
４はα−Ｆｅ、０３薄膜、
５．６はＦ切回薄膜、Fig. 1 is an enlarged sectional view of main parts showing the manufacturing method of the magnetic recording medium according to the present invention in order of steps, Fig. 2 is a comparison table of magnetic properties, Fig. 3 is the B-8 curve, and Fig. 4 is a conventional magnetic recording medium. FIG. 2 is an enlarged sectional view of a main part for explaining a method of manufacturing a recording medium. In the figure, 1 is a non-magnetic substrate, 4 is α-Fe, 03 thin film, 5.6 is F-cut thin film,
Claims (1)
性スパッタリングによりα−Ｆｅ＿２Ｏ＿３薄膜（４）
を被着した後、還元熱処理を行って第一層のＦｅ＿３Ｏ
＿４薄膜（５）を形成し、 更に該Ｆｅ＿３Ｏ＿４膜（第一層）（５）上に、Ｆｅを
母材にて反応性スパッタリングを行って第二層のＦｅ＿
３Ｏ＿４薄膜（６）を被着した後、 これら両薄膜（５、６）を酸化処理してγ−Ｆｅ＿２Ｏ
＿３磁性薄膜（７）を形成したことを特徴とする磁気記
録媒体の製造方法。[Claims] An α-Fe_2O_3 thin film (4) is formed on a non-magnetic substrate (1) by reactive sputtering using Fe (iron) as a base material.
After depositing Fe_3O, a reduction heat treatment is performed to form the first layer of Fe_3O.
A _4 thin film (5) is formed, and then reactive sputtering is performed on the Fe_3O_4 film (first layer) (5) using a base material to form a second layer of Fe_
After depositing the 3O_4 thin film (6), both these thin films (5, 6) are oxidized to form γ-Fe_2O.
_3 A method for manufacturing a magnetic recording medium, characterized in that a magnetic thin film (7) is formed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11646386A JPS62271226A (en) | 1986-05-20 | 1986-05-20 | Production of magnetic recording medium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11646386A JPS62271226A (en) | 1986-05-20 | 1986-05-20 | Production of magnetic recording medium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62271226A true JPS62271226A (en) | 1987-11-25 |
Family
ID=14687733
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11646386A Pending JPS62271226A (en) | 1986-05-20 | 1986-05-20 | Production of magnetic recording medium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62271226A (en) |
-
1986
- 1986-05-20 JP JP11646386A patent/JPS62271226A/en active Pending
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