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JP2552799B2 - Manufacturing method of magnetic storage medium - Google Patents
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JP2552799B2 - Manufacturing method of magnetic storage medium - Google Patents

Manufacturing method of magnetic storage medium

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Publication number
JP2552799B2
JP2552799B2 JP4232064A JP23206492A JP2552799B2 JP 2552799 B2 JP2552799 B2 JP 2552799B2 JP 4232064 A JP4232064 A JP 4232064A JP 23206492 A JP23206492 A JP 23206492A JP 2552799 B2 JP2552799 B2 JP 2552799B2
Authority
JP
Japan
Prior art keywords
storage medium
magnetic storage
protective film
manufacturing
hydrocarbon
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 - Lifetime
Application number
JP4232064A
Other languages
Japanese (ja)
Other versions
JPH05217160A (en
Inventor
敏弘 安東
修一 平井
博 竹野
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.)
Mitsubishi Chemical Corp
Original Assignee
Mitsubishi Chemical Corp
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 Mitsubishi Chemical Corp filed Critical Mitsubishi Chemical Corp
Priority to JP4232064A priority Critical patent/JP2552799B2/en
Publication of JPH05217160A publication Critical patent/JPH05217160A/en
Application granted granted Critical
Publication of JP2552799B2 publication Critical patent/JP2552799B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Manufacturing Of Magnetic Record Carriers (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】本発明は録画用、録音用又は電算
機に用いられるテープ状、ドラム状又はディスク状の磁
気記憶媒体の製造方法に関し、特に高湿度条件下に暴露
された後でも優れた耐摩耗性を有する磁気記憶媒体の製
造方法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a tape-shaped, drum-shaped or disk-shaped magnetic recording medium used for recording, recording or computer, and particularly excellent even after being exposed to high humidity conditions. And a method of manufacturing a magnetic storage medium having wear resistance.

【0002】[0002]

【従来の技術】近年、記録密度の向上の目的のもとに、
鉄、コバルト、ニッケル又はこれらの合金からなる強磁
性金属薄膜を真空蒸着、スパッタリング又はメッキ法で
基体上に設けた磁気記憶媒体が提案されている。これら
の金属磁気記憶媒体は高密度記録性に優れているが、記
録再生装置に使用すると磁気ヘッド等と物理的に接触し
ながら高速度走行をするので、実用上、耐摩耗性も優れ
ていることが必要である。
2. Description of the Related Art In recent years, for the purpose of improving recording density,
A magnetic storage medium has been proposed in which a ferromagnetic metal thin film made of iron, cobalt, nickel or an alloy thereof is provided on a substrate by vacuum deposition, sputtering or plating. These metal magnetic storage media are excellent in high-density recording property, but when used in a recording / reproducing apparatus, they run at high speed while physically contacting a magnetic head or the like, so they are also practically excellent in wear resistance. It is necessary.

【0003】この耐摩耗性を向上させるために、強磁性
体金属の表面に液体又は固体のパラフィン等の炭化水素
類からなる潤滑剤を塗布するか、又は真空蒸着法により
薄膜を形成することが提案されている。
In order to improve the abrasion resistance, a lubricant made of a hydrocarbon such as liquid or solid paraffin or the like is applied to the surface of the ferromagnetic metal, or a thin film is formed by a vacuum vapor deposition method. Proposed.

【0004】[0004]

【発明が解決しようとする課題】これらの塗布法又は真
空蒸着法で形成された炭化水素保護膜は、溶剤に可溶で
あるので、常態での耐摩耗性は優れているものの、高湿
度条件下に暴露した後ではその耐摩耗性が著しく劣化す
るという欠点がある。
Since the hydrocarbon protective film formed by these coating methods or vacuum deposition methods is soluble in a solvent, it is excellent in wear resistance under normal conditions, but under high humidity conditions. After being exposed to the bottom, it has the drawback that its wear resistance deteriorates significantly.

【0005】本発明者等は、これらの欠点を改善するた
めに種々の研究を行った結果、磁気記憶媒体の保護被膜
として炭化水素膜が高湿度条件下に暴露しても耐摩耗性
が劣化しないという知見に基づいて本発明に到達したも
のである。
The inventors of the present invention have conducted various studies in order to remedy these drawbacks, and as a result, the hydrocarbon film as a protective film of the magnetic storage medium deteriorates in wear resistance even when exposed to high humidity conditions. The present invention has been achieved based on the finding that it does not.

【0006】即ち、本発明の目的は、常態及び高湿度条
件下に暴露した後のいずれにおいても、耐摩耗性が優れ
た磁気記憶媒体の製造方法を提供することにある。
That is, it is an object of the present invention to provide a method of manufacturing a magnetic storage medium which is excellent in wear resistance both under normal conditions and after being exposed to high humidity conditions.

【0007】[0007]

【課題を解決するための手段】本発明に係る磁気記憶媒
体の製造方法は、基体の上に設けた強磁性金属薄膜の表
面上に、炭化水素を含むガスのイオン化プラズマ分解重
合反応により、形成すべき炭化水素質保護膜の炭素/水
素の割合を原子比で50/50から98/2の範囲にす
ることを特徴とする。
A method of manufacturing a magnetic storage medium according to the present invention comprises forming on a surface of a ferromagnetic metal thin film provided on a substrate by an ionization plasma decomposition polymerization reaction of a gas containing a hydrocarbon. It is characterized in that the ratio of carbon / hydrogen of the hydrocarbon protective film to be made is in the range of 50/50 to 98/2 in atomic ratio.

【0008】[0008]

【作用】本発明においては、基体の上に設けた強磁性金
属薄膜の表面上に、炭化水素保護膜を形成する。炭化水
素保護膜(以下、保護膜という)とは、炭素/水素の割
合が50/50から98/2の範囲にあるものである。
このような保護膜は、炭化水素ガスを含むガスのイオン
化プラズマ分解重合反応により形成することができる。
In the present invention, the hydrocarbon protective film is formed on the surface of the ferromagnetic metal thin film provided on the substrate. A hydrocarbon protective film (hereinafter referred to as a protective film) has a carbon / hydrogen ratio of 50/50 to 98/2.
Such a protective film can be formed by an ionization plasma decomposition polymerization reaction of a gas containing a hydrocarbon gas.

【0009】このようにして形成した保護膜は溶剤に不
溶であり、その赤外分光分析によるとC−H結合の吸収
ピークが存在し、その元素分析ではC/Hの原子比で5
0/50以下の水素が含有されているものである。水素
の含有量が少なくなると、膜の硬度は増加すると共に、
その内部応力及び動摩擦係数も増加する。従って、磁気
記憶媒体の保護膜としては、C/Hの原子比で50/5
0から98/2の範囲にすることが必要であるが、特に
好ましい範囲としては60/40から90/10であ
る。
The protective film thus formed is insoluble in a solvent and has an absorption peak of C--H bond according to its infrared spectroscopic analysis. Its elemental analysis shows that the atomic ratio of C / H is 5%.
It contains 0/50 or less hydrogen. As the hydrogen content decreases, the hardness of the film increases and
Its internal stress and dynamic coefficient of friction also increase. Therefore, as the protective film of the magnetic storage medium, the atomic ratio of C / H is 50/5.
It is necessary to set it in the range of 0 to 98/2, and a particularly preferable range is 60/40 to 90/10.

【0010】保護膜は高湿度条件下に暴露した後でも極
めて硬く、なおかつ極めて小さな摩擦係数をもっている
ので、磁気記憶媒体上に積層する保護膜として特に有益
で優れた特性を有する。従って、本発明方法により製造
した磁気記憶媒体は、高湿度条件下で使用する場合に極
めて実用性が高い。
Since the protective film is extremely hard even after being exposed to high humidity conditions and has a very small friction coefficient, it is particularly useful and has excellent properties as a protective film to be laminated on a magnetic storage medium. Therefore, the magnetic storage medium manufactured by the method of the present invention is extremely practical when used under high humidity conditions.

【0011】保護膜の厚さとしては、好ましくは2000Å
以下、特に好ましくは1000Å以下であり、それ以上の厚
さになるとスペーシングロスが大きくなる。
The thickness of the protective film is preferably 2000Å
The thickness is particularly preferably 1000 L or less, and the spacing loss becomes large when the thickness is more than 1000 L.

【0012】[0012]

【実施例】次に、本発明の実施例に係る磁気記憶媒体の
製造方法について、添付の図面を参照して具体的に説明
する。
Next, a method of manufacturing a magnetic storage medium according to an embodiment of the present invention will be specifically described with reference to the accompanying drawings.

【0013】図1は、本実施例方法において、保護膜を
作成するために使用するイオン化プラズマ分解重合装置
の一例を示す模式図である。反応容器4は反応容器台5
の上に気密が保持されるように装着される。この反応容
器台5には炭化水素を含むガスの供給口6及び排気ポン
プに接続された排気管7が設けられている。また、反応
容器4内には電極2、3が設けられていて、この電極
2,3間に電圧を印加することによって両者間にプラズ
マを発生させることができる。電極2上には、保護膜を
被着すべき磁気ディスク1が設置されるようになってお
り、これにより磁気ディスク1には電極2と同じ電位が
印加され、この磁気ディスク1上でイオン化プラズマ分
解重合により保護膜が形成されるように構成されてい
る。
FIG. 1 is a schematic view showing an example of an ionization plasma decomposition polymerization apparatus used for forming a protective film in the method of this embodiment. The reaction container 4 is a reaction container base 5
It is installed so that airtightness is maintained on the top of the. The reaction vessel base 5 is provided with a supply port 6 for a gas containing hydrocarbon and an exhaust pipe 7 connected to an exhaust pump. Further, electrodes 2 and 3 are provided in the reaction container 4, and plasma can be generated between the electrodes 2 and 3 by applying a voltage between them. A magnetic disk 1 to be coated with a protective film is arranged on the electrode 2, and thereby the same potential as that of the electrode 2 is applied to the magnetic disk 1, and an ionized plasma is generated on the magnetic disk 1. The protective film is formed by decomposition polymerization.

【0014】本実施例方法においては、反応容器4内に
磁性層を備えた磁気ディスク1を設置し、排気管7を介
して反応容器4内を排気する。次いで、この排気を継続
しつつ、供給口6を介して反応容器4内に原料ガスとし
て、C22、C24、C26,CH4,C410等の飽和
若しくは不飽和の炭化水素、C66,C612等の常温
・常圧で液体の炭化水素をガス化したもの、又はこれら
のガス状炭化水素とAr、He、Ne、H2等の炭化水
素以外のガスとの混合ガスを供給する。このようにし
て、反応容器4内を所定の圧力の原料ガス雰囲気にお
き、電極2,3間に所定の電圧を印加することにより、
イオン化プラズマ分解重合反応が発生し、磁性層を備え
た磁気ディスク1の表面に保護膜が形成される。
In the method of this embodiment, the magnetic disk 1 provided with a magnetic layer is set in the reaction vessel 4, and the inside of the reaction vessel 4 is evacuated through the exhaust pipe 7. Next, while continuing this exhaust, as a raw material gas into the reaction vessel 4 via the supply port 6, C 2 H 2 , C 2 H 4 , C 2 H 6 , CH 4 , C 4 H 10 or the like is saturated or Unsaturated hydrocarbons, those obtained by gasifying liquid hydrocarbons such as C 6 H 6 and C 6 H 12 at normal temperature and pressure, or these gaseous hydrocarbons and Ar, He, Ne, H 2 etc. A mixed gas with a gas other than hydrocarbons is supplied. In this way, by placing the inside of the reaction vessel 4 in a source gas atmosphere having a predetermined pressure and applying a predetermined voltage between the electrodes 2 and 3,
An ionized plasma decomposition polymerization reaction occurs, and a protective film is formed on the surface of the magnetic disk 1 having the magnetic layer.

【0015】なお、本発明において、保護膜は磁性層の
上に直接形成しても良いが、Au、Pt,Ni−P,C
r,Ni,SiO2,Si,Ti,Ti−C又はSi3
4等からなる非磁性下地層を介して形成することもでき
る。
In the present invention, the protective film may be formed directly on the magnetic layer, but Au, Pt, Ni-P, C may be used.
r, Ni, SiO 2, Si , Ti, Ti-C or Si 3 N
It can also be formed via a non-magnetic underlayer composed of 4 or the like.

【0016】イオン化プラズマ分解重合装置の操作条件
としては、反応容器内の圧力を0.001〜10Torrとし、電
極間に200〜2000Vの直流又は交流の電圧を印加する
か、又は電圧が200〜2000V、周波数が100KHz〜20MHzの
高周波電圧を印加することが好ましい。
The operating conditions of the ionization plasma decomposition polymerization apparatus are as follows: the pressure in the reaction vessel is 0.001 to 10 Torr, a DC or AC voltage of 200 to 2000 V is applied between the electrodes, or a voltage of 200 to 2000 V and a frequency. It is preferable to apply a high frequency voltage of 100 KHz to 20 MHz.

【0017】このようにして製造した磁気記憶媒体にお
いては、その表面に炭素/水素の割合が原子比で50/
50〜98/2である炭化水素質保護膜が形成されてい
るので、この磁気記憶媒体を高湿度条件下に暴露しても
耐摩耗性が劣化しないという優れた効果を有する。
In the magnetic storage medium thus manufactured, the ratio of carbon / hydrogen is 50 / atomic ratio on the surface.
Since the hydrocarbon protective film having a thickness of 50 to 98/2 is formed, it has an excellent effect that the wear resistance does not deteriorate even if this magnetic storage medium is exposed to high humidity conditions.

【0018】以下、本発明により製造した実施例をその
比較例と比較して説明する。実施例1 メッキディスクの製造 直径9cm、厚さ2mmの鏡面研摩したアルミ板上に非磁性N
i−P合金下地層を50μm厚に無電解メッキした後、30
μmまで鏡面研摩し、更にその上に下記表1に示すメッ
キ液及びメッキ条件でCo−Ni−P合金(Co:80
%、Ni;15%、P:5%)の磁性膜を0.1μm厚となる
ように無電解メッキした。無電解メッキの前処理として
は日本カニゼン(株)の「シューマセンシタイザー」及
び「シューマアクチベーター」を使用した。
The examples manufactured according to the present invention will be described below in comparison with the comparative examples. Example 1 Production of plated disk Non-magnetic N on a mirror-polished aluminum plate with a diameter of 9 cm and a thickness of 2 mm
After electroless plating the iP alloy underlayer to a thickness of 50 μm, 30
It was mirror-polished to a thickness of μm, and a Co-Ni-P alloy (Co: 80
%, Ni; 15%, P: 5%) was electroless plated to a thickness of 0.1 μm. As a pretreatment for electroless plating, "Schuma Sensitizer" and "Schuma Activator" from Nippon Kanigen Co., Ltd. were used.

【0019】[0019]

【表1】 [Table 1]

【0020】この、メッキディスクをメッキディスクA
として試料に供した。磁気記憶媒体の製造 図1に示す構造のイオン化プラズマ分解重合装置を用い
て、各種炭化水素ガスを原料とし、下記表2に示す条件
でメッキディスクA上に800Å厚の炭化水素膜を形成し
た。但し、表2において、DCは直流、ACは交流電圧
を示す。
This plated disk is called plated disk A
Was used as a sample. Manufacture of Magnetic Storage Medium Using the ionized plasma decomposition polymerization apparatus having the structure shown in FIG. 1, various hydrocarbon gases were used as raw materials and a hydrocarbon film having a thickness of 800 Å was formed on the plated disk A under the conditions shown in Table 2 below. However, in Table 2, DC indicates a direct current and AC indicates an alternating voltage.

【0021】比較のために、融点50〜70℃のパラフィン
をシクロヘキサンを溶媒としてスピンコート法によりメ
ッキディスクA上に800Å厚で施したものを作成した。
これを比較例15とする。
For comparison, a paraffin having a melting point of 50 to 70 ° C. was applied on the plating disk A to a thickness of 800 Å by spin coating using cyclohexane as a solvent.
This is Comparative Example 15.

【0022】[0022]

【表2】 [Table 2]

【0023】これらの試験材に対し、常態及び耐湿後に
行った摺動試験の結果を下記表3に示す。また、実施例
No.1〜No.11及び比較例12〜15と原料ガス、ガスの圧
力、印加電圧を同条件にし、反応時間だけを長くして厚
膜を作成し、そのC,H元素分析をした結果を下記表4
に示す。
Table 3 below shows the results of sliding tests conducted on these test materials under normal conditions and after moisture resistance. Example
No. 1 to No. 11 and Comparative Examples 12 to 15 were the same as the raw material gas, the pressure of the gas, and the applied voltage, the reaction time was lengthened to form a thick film, and the results of C and H elemental analysis The following Table 4
Shown in

【0024】[0024]

【表3】 [Table 3]

【0025】[0025]

【表4】 [Table 4]

【0026】但し、表3に示す物性等の測定は、次のよ
うにして行った。 1)動摩擦係数測定 装置は図2に示す構造の摺動物性測定装置を用い、ヘッ
ドは直径が2mmのサフアイア球を使用し、ヘッド荷重を5
gとし、相対速度が5m/secの条件下で動摩擦係数を測定
した。 2)摺動回数測定 図2に示す摺動物性測定装置を用い、ヘッドは直径が2m
mのサファイア球を使用し、ヘッド荷重を10gとし、相対
速度が10m/secの条件下で保護膜が破壊するまでの回数
を摺動回数とした。 3)CSS(コンタクト、スタート、ストップ)テスト ヘッドはIBM−3350タイプを使用し、ヘッド荷重を9.
8gとし、回転速度3600r.p.m、ON-OFF 30秒サイクルの条
件下でヘッドクラッシュが発生するまでのサイクル数を
CSSテスト回数とした。
However, the physical properties shown in Table 3 were measured as follows. 1) Dynamic friction coefficient measuring device The sliding physical property measuring device of the structure shown in Fig. 2 is used, the head is a sapphire ball with a diameter of 2 mm, and the head load is 5
g, and the dynamic friction coefficient was measured under the condition that the relative speed was 5 m / sec. 2) Measurement of number of sliding times Using the sliding property measuring device shown in Fig. 2, the head has a diameter of 2 m.
Using a sapphire ball of m, a head load of 10 g, and a relative speed of 10 m / sec, the number of times until the protective film broke was defined as the number of times of sliding. 3) CSS (contact, start, stop) test The head uses IBM-3350 type and the head load is 9.
The CSS test count was the number of cycles until a head crash occurred under the conditions of a rotation speed of 3600 rpm and an ON-OFF 30 second cycle at 8 g.

【0027】その結果、実施例1乃至12においては、
常態及び耐湿後のいずれの場合も、比較例に比して摺動
回数及びCSSテスト回数が大きく、極めて優れた耐摩
耗性を有する。
As a result, in Examples 1 to 12,
In both the normal state and after the moisture resistance, the number of sliding times and the number of CSS tests are large as compared with the comparative example, and the abrasion resistance is extremely excellent.

【0028】[0028]

【発明の効果】本発明によれば、高湿度条件下に暴露し
た場合でも、耐摩耗性が劣化しない磁気記録媒体の製造
方法を提供することができる。
According to the present invention, it is possible to provide a method of manufacturing a magnetic recording medium whose wear resistance does not deteriorate even when exposed to high humidity conditions.

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

【図1】イオン化プラズマ分解重合装置の説明図であ
る。
FIG. 1 is an explanatory diagram of an ionized plasma decomposition polymerization apparatus.

【図2】摺動物性測定装置の説明図である。FIG. 2 is an explanatory diagram of a sliding property measuring device.

【符号の説明】[Explanation of symbols]

1,17;磁気ディスク 2,3;電極 4;反応容器 5;反応容器台 6;ガス供給口 7;排気管 18;ホルダー 19;サファイア球 20;板バネ 21;歪ゲージ 22;XYステージ 23;ディスク回転用モーター 24;架台 1, 17; magnetic disk 2, 3; electrode 4; reaction container 5; reaction container stand 6; gas supply port 7; exhaust pipe 18; holder 19; sapphire sphere 20; leaf spring 21; strain gauge 22; XY stage 23; Disk rotation motor 24; stand

───────────────────────────────────────────────────── フロントページの続き (72)発明者 竹野 博 東京都町田市旭町3−5−1 電気化学 工業株式会社加工技術研究所内 (56)参考文献 特開 昭57−135443(JP,A) ─────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Hiroshi Takeno 3-5-1 Asahimachi, Machida, Tokyo Electrochemical Industry Co., Ltd. Processing Technology Laboratory (56) Reference JP-A-57-135443 (JP, A)

Claims (1)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 基体の上に設けた強磁性金属薄膜の表面
上に、炭化水素を含むガスのイオン化プラズマ分解重合
反応により、形成すべき炭化水素質保護膜の炭素/水素
の割合を原子比で50/50から98/2の範囲にする
ことを特徴とする磁気記憶媒体の製造方法。
1. A carbon / hydrogen ratio of a hydrocarbonaceous protective film to be formed on a surface of a ferromagnetic metal thin film provided on a substrate by an ionization plasma decomposition polymerization reaction of a gas containing a hydrocarbon in an atomic ratio. The manufacturing method of the magnetic storage medium is characterized in that the range is 50/50 to 98/2.
JP4232064A 1992-08-31 1992-08-31 Manufacturing method of magnetic storage medium Expired - Lifetime JP2552799B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP4232064A JP2552799B2 (en) 1992-08-31 1992-08-31 Manufacturing method of magnetic storage medium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4232064A JP2552799B2 (en) 1992-08-31 1992-08-31 Manufacturing method of magnetic storage medium

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
JP59012562A Division JP2549361B2 (en) 1984-01-26 1984-01-26 Magnetic storage media

Publications (2)

Publication Number Publication Date
JPH05217160A JPH05217160A (en) 1993-08-27
JP2552799B2 true JP2552799B2 (en) 1996-11-13

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JP4232064A Expired - Lifetime JP2552799B2 (en) 1992-08-31 1992-08-31 Manufacturing method of magnetic storage medium

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Publication number Priority date Publication date Assignee Title
GB1582231A (en) * 1976-08-13 1981-01-07 Nat Res Dev Application of a layer of carbonaceous material to a surface
JPS5778632A (en) * 1980-10-30 1982-05-17 Sekisui Chem Co Ltd Manufacture of magnetic recording medium
JPS57135443A (en) * 1981-02-16 1982-08-21 Fuji Photo Film Co Ltd Manufacture of magnetic recording medium

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