JP2001236638A - Method for forming lubricative film, recording medium and magnetic recorder - Google Patents

Method for forming lubricative film, recording medium and magnetic recorder

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Publication number
JP2001236638A
JP2001236638A JP2000040921A JP2000040921A JP2001236638A JP 2001236638 A JP2001236638 A JP 2001236638A JP 2000040921 A JP2000040921 A JP 2000040921A JP 2000040921 A JP2000040921 A JP 2000040921A JP 2001236638 A JP2001236638 A JP 2001236638A
Authority
JP
Japan
Prior art keywords
layer
lubricant
lubricant layer
group
lubricating 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.)
Granted
Application number
JP2000040921A
Other languages
Japanese (ja)
Other versions
JP4545867B2 (en
Inventor
Keiji Watabe
慶二 渡部
Hiroshi Chiba
洋 千葉
Eishin Yamakawa
栄進 山川
Yuichiro Itai
雄一郎 板井
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.)
Fujitsu Ltd
Original Assignee
Fujitsu Ltd
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Filing date
Publication date
Application filed by Fujitsu Ltd filed Critical Fujitsu Ltd
Priority to JP2000040921A priority Critical patent/JP4545867B2/en
Publication of JP2001236638A publication Critical patent/JP2001236638A/en
Application granted granted Critical
Publication of JP4545867B2 publication Critical patent/JP4545867B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Chemical Vapour Deposition (AREA)
  • Magnetic Record Carriers (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Lubricants (AREA)
  • Paints Or Removers (AREA)

Abstract

PROBLEM TO BE SOLVED: To improve adhesion to a recording medium side, to reduce friction on a slider and to sufficiently reduce adhesion properties to the slider regarding a method for forming a lubricative film, a recording medium and a magnetic disk device. SOLUTION: The lubricative film includes a lower lubricant layer 13 comprising a 1st polymer having a polar group or a group with >=7 introduced πelectrons as a terminal group and an upper lubricant layer 14 comprising a 2nd polymer applied on the lower lubricant layer 13 and having a terminal group different from that of the 1st polymer.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、潤滑膜形成方法、
記録媒体及び磁気ディスク装置に関し、より詳しくは、
記録媒体表面とヘッドの磨耗を抑制し、両者の接触によ
る記録データの破壊を防止するための潤滑膜形成方法、
記録媒体及び磁気記録装置に関する。
TECHNICAL FIELD The present invention relates to a method for forming a lubricating film,
Regarding recording media and magnetic disk devices,
A method of forming a lubricating film for suppressing wear of a recording medium surface and a head and preventing destruction of recording data due to contact between the two;
The present invention relates to a recording medium and a magnetic recording device.

【0002】[0002]

【従来の技術】近年、磁気ディスク装置においては、ド
ライブ装置の起動・停止方式として、ドライブ装置の停
止、起動の際に磁気ヘッドが磁気記録媒体に接触して触
れ合うコンタクト・スタート・ストップ(CSS)方式
が主流となっている。しかし、そのような磁気ディスク
装置においては、磁気ディスクと磁気ヘッドスライダー
が長時間接触した状態からディスクが再起動する際に高
いスティクション(吸着)が発生してディスクが起動で
きなくなったり、また、ディスクとヘッドが接触して磁
気記録データが破壊されるヘッドクラッシュが起きた
り、ヘッドやジンバルが損傷される恐れがある。
2. Description of the Related Art In recent years, in a magnetic disk drive, a contact start / stop (CSS) method in which a magnetic head comes into contact with and touches a magnetic recording medium when the drive is stopped or started, as a method of starting / stopping the drive. The method is the mainstream. However, in such a magnetic disk device, when the disk is restarted from a state where the magnetic disk and the magnetic head slider have been in contact for a long time, high stiction (adsorption) occurs, and the disk cannot be started. There is a risk that a head and a gimbal may be damaged due to a head crash where magnetic recording data is destroyed due to contact between the disk and the head.

【0003】スティクションの発生には、磁気ディスク
の磁性層又はその上の保護層の表面粗さや材料の性質が
大きく影響するので、スティクションを抑制するため
に、保護層の上に特定のフッ素含有樹脂からなる潤滑剤
層を形成することが提案されている。そのような磁気デ
ィスク(磁気記録媒体)は、図1に示すように、非磁性
基板1の上に磁性層2、保護層3及び潤滑剤層4を順に
形成した構造を有している。潤滑剤層4については、米
国特許3778308、米国特許4267238、米国
特許4268556に報告がある。
[0003] Since the surface roughness and material properties of the magnetic layer of the magnetic disk or the protective layer thereon greatly affect the generation of stiction, specific fluorine is deposited on the protective layer to suppress stiction. It has been proposed to form a lubricant layer made of a contained resin. Such a magnetic disk (magnetic recording medium) has a structure in which a magnetic layer 2, a protective layer 3, and a lubricant layer 4 are sequentially formed on a non-magnetic substrate 1, as shown in FIG. The lubricant layer 4 is reported in US Pat. No. 3,778,308, US Pat. No. 4,267,238, and US Pat. No. 4,268,556.

【0004】なお、保護層3の材料として、ダイヤモン
ドライクカ一ボン(DLC)や二酸化珪素が用いられて
いる。また、近年パーソナルコンピュータの爆発的な普
及と高性能化に伴い、磁気ディスク装置の高記録密化や
高速処理化が加速してきており、これに対応してヘッド
と記録媒体の距離(浮上量)を短く(低く)したり、デ
ィスクの回転速度を早くする必要がある。また,特に最
近販売台数が急増しているノートパソコン等では使用環
境が高温高湿から低温低湿まで様々であるため、これら
の環境においてもスティクションを抑える必要があり,
磁気ディスク装置の高性能化に向けて、潤滑剤の高性能
化が従来以上に重要度を増している。
[0004] As a material of the protective layer 3, diamond-like carbon (DLC) or silicon dioxide is used. In recent years, with the explosive popularization and high performance of personal computers, high recording density and high speed processing of magnetic disk devices have been accelerated, and the distance between the head and the recording medium (flying height) has been correspondingly increased. It is necessary to shorten (lower) and increase the rotation speed of the disk. In addition, especially in notebook PCs, whose sales volume has been increasing rapidly recently, the usage environment varies from high temperature and high humidity to low temperature and low humidity, so it is necessary to suppress stiction even in these environments.
To improve the performance of magnetic disk drives, the performance of lubricants has become more important than ever.

【0005】[0005]

【発明が解決しようとする課題】磁気ディスク用の潤滑
剤として用いられているパーフロロ樹脂化合物は、一般
的に基板との密着性を上げるために、樹脂構造の末端に
極性の高い成分を有し、この極性基が基板表面に吸着す
ることにより潤滑剤と基板の密着性が保たれる。図1で
は、樹脂構造を符号5、極性基を符号6で示している。
また、潤滑剤層は1回の塗布により形成される。
The perfluororesin compound used as a lubricant for magnetic disks generally has a highly polar component at the end of the resin structure in order to increase the adhesion to the substrate. The adhesion between the lubricant and the substrate is maintained by the adsorption of the polar group on the substrate surface. In FIG. 1, the resin structure is denoted by reference numeral 5 and the polar group is denoted by reference numeral 6.
The lubricant layer is formed by one application.

【0006】そのような潤滑剤層4では、保護層3に付
着しているボンド(bond)成分Aと、保護層3と結合せず
自由に動き回るモビリティ(mobile)成分Bとが存在す
る。モビリティ成分Bは、ディスクの高速回転の際に遠
心力でディスク周辺部に押し出されて潤滑剤層4の膜厚
変動を起こすとともに、スライダに付着して堆積し易
く、特にスライダのディスクからの浮上量が低い場合に
はヘッドクラッシュを引き起こし易い。
In such a lubricant layer 4, there are a bond component A attached to the protective layer 3 and a mobility component B that moves freely without being bonded to the protective layer 3. The mobility component B is pushed to the periphery of the disk by centrifugal force during high-speed rotation of the disk to cause a change in the thickness of the lubricant layer 4 and also easily adheres to and accumulates on the slider. In particular, the floating of the slider from the disk When the amount is low, a head crash is easily caused.

【0007】また、モビリティ成分Bでの極性基は、コ
ンタミを引きつけたり、ヘッドスライダとの摩擦を高め
る原因となる。今後の磁気ディスク装置の高性能化のた
めには、ボンド成分を増やし、モビリティ成分を減らす
ための潤滑剤層の形成方法の開発が検討されている。例
えば、潤滑剤を保護膜上に塗布する前に保護膜表面をプ
ラズマ処理することが特開昭62一150526、特開
昭63−2117に記載され、保護膜にオゾンUVを照
射する手法が特開平4−6624、特開平6−3019
70において提案されている。しかし、それらの方法に
よっては、ボンド層を効果的に増やすことは難しく、ま
た、表面処埋から潤滑剤塗布までの時間の相違により処
理効果がばらつくため、実用的でなかった。
[0007] The polar group in the mobility component B attracts contaminants and increases friction with a head slider. In order to improve the performance of magnetic disk devices in the future, development of a method for forming a lubricant layer to increase the bond component and reduce the mobility component is being studied. For example, JP-A-62-115026 and JP-A-63-2117 disclose plasma treatment of the surface of a protective film before applying a lubricant on the protective film. Kaihei 4-6624, JP-A-6-3019
70. However, these methods are not practical because it is difficult to effectively increase the number of bond layers, and the processing effect varies due to the difference in time from surface treatment to application of a lubricant.

【0008】また、特開平7−262555、特開平8
−124142において、潤滑剤塗布後に光を照射する
手法も提案されている。しかし、光照射により潤滑層表
面が酸化して十分な低摩擦特性が得られないという問題
と、光照射の際に空気中のコンタミの付着性が増すため
に高温高湿下で結露し、乾燥したあとには多量の結露痕
(コンタミ凝集物)が媒体表面に発生し、ヘッドを汚染
して浮上性の不良、トルクの増大、ヘッドの腐食を起こ
すといった間題があった。
Further, Japanese Patent Application Laid-Open Nos. Hei 7-262555 and Hei 8
In -124142, a method of irradiating light after applying a lubricant has also been proposed. However, the surface of the lubricating layer is oxidized by light irradiation, and sufficient low friction characteristics cannot be obtained.In addition, due to the increased adhesion of contaminants in the air during light irradiation, dew condensation occurs at high temperature and high humidity, and drying occurs. After that, a large amount of dew marks (contaminant aggregates) are generated on the medium surface, and there is a problem that the head is contaminated to cause poor flying performance, increase in torque, and cause corrosion of the head.

【0009】本発明の目的は、記録媒体側との密着性が
従来よりも高く、スライダとの摩擦が低く、スライダへ
の付着性を十分に低減することができる潤滑膜形成方法
と、その潤滑膜を有する記録媒体と、この記録媒体を有
する磁気記録装置を提供することにある。
SUMMARY OF THE INVENTION An object of the present invention is to provide a method of forming a lubricating film in which the adhesion to the recording medium is higher than before, the friction with the slider is low, and the adhesion to the slider can be sufficiently reduced. An object of the present invention is to provide a recording medium having a film and a magnetic recording device having the recording medium.

【0010】[0010]

【課題を解決するための手段】上記した課題は、被塗布
体の上に下側の潤滑剤層を塗布する工程と、塗布溶剤を
含む上側の潤滑剤層を前記下側の潤滑剤層の上に塗布す
る工程とを有し、さらに前記下側の層潤滑剤の90%以
上を前記塗布溶剤に不溶化する状態にさせることを特徴
とする潤滑膜形成方法によって解決される。
The above object is achieved by a step of applying a lower lubricant layer on an object to be coated, and a step of applying an upper lubricant layer containing a coating solvent to the lower lubricant layer. And a method of forming a lubricating film, wherein 90% or more of the lower layer lubricant is made insoluble in the coating solvent.

【0011】その潤滑膜形成方法において、前記下側の
潤滑剤層を前記被塗布体に塗布した後に、光照射、加熱
のうち少なくとも一方の処理により前記下側の潤滑剤層
を架橋させ、架橋後の前記下側の潤滑剤層の90%以上
をゲル化させてもよい。上記した潤滑膜形成方法におい
て、前記下側の潤滑剤層を前記被塗布体に塗布した後、
前記下側の潤滑剤層の一部の分子を溶剤の蒸気により洗
浄し、この洗浄後の前記下側の潤滑剤層の90%以上を
前記上側の潤滑剤層の前記塗布溶剤に不溶可させてもよ
い。
In the method of forming a lubricating film, after applying the lower lubricant layer to the object to be coated, the lower lubricant layer is cross-linked by at least one of light irradiation and heating. 90% or more of the subsequent lower lubricant layer may be gelled. In the above-described lubricating film forming method, after applying the lower lubricant layer to the object to be coated,
A part of the molecules of the lower lubricant layer are washed with a solvent vapor, and 90% or more of the lower lubricant layer after the washing is insoluble in the coating solvent of the upper lubricant layer. You may.

【0012】上記した潤滑膜形成方法において、前記上
側の潤滑剤層を、末端基に極性基を持たない弗素系ポリ
マーから構成してもよい。例えば、前記上側の潤滑剤層
は、末端基にCF3 基を有するパーフロロポリエーテルで
ある。上記した潤滑膜形成方法において、前記下側の潤
滑剤層を、未端基に極性基、7つ以上のπ電子が導入さ
れた基のいずれかの基を持つ弗素系ポリマーから構成し
てもよい。
In the above-described method for forming a lubricating film, the upper lubricant layer may be made of a fluorine-based polymer having no polar group at a terminal group. For example, the upper lubricant layer is a perfluoropolyether having a CF 3 terminal group. In the above-described method of forming a lubricating film, the lower lubricant layer may be formed of a fluorine-based polymer having a polar group at an end group or a group into which seven or more π electrons are introduced. Good.

【0013】上記した潤滑膜形成方法において、前記下
側の潤滑剤層と前記上側の潤滑剤層を形成した後に、前
記下側の潤滑剤層と前記上側の潤滑剤層に放射線を照射
することを特徴とする。上記した潤滑膜形成方法におい
て、前記被塗布体の最表層は、CVD法で成膜したカー
ボン薄膜であることを特徴とする。
In the above-described method of forming a lubricating film, the lower lubricant layer and the upper lubricant layer are irradiated with radiation after the lower lubricant layer and the upper lubricant layer are formed. It is characterized by. In the above-described lubricating film forming method, the outermost layer of the object to be coated is a carbon thin film formed by a CVD method.

【0014】また、上記した課題は、記録層と、前記記
録層の上に塗布され、且つ、未端基に極性基または7つ
以上のπ電子が導入された基を有する第1のポリマーか
らなる下側の潤滑剤層と、前記下側の潤滑剤層の上に塗
布され、且つ、末端に第1のポリマーと異なる末端基を
有する第2のポリマーからなる上側の潤滑剤層とを有す
ることを特徴とする記録媒体によって解決される。
[0014] The above-mentioned problem is also caused by the problem that the recording layer and the first polymer which is coated on the recording layer and has a polar group or a group in which seven or more π electrons are introduced into an unterminated group. A lower lubricant layer, and an upper lubricant layer that is applied on the lower lubricant layer and is made of a second polymer having a terminal group different from the first polymer at the terminal. It is solved by a recording medium characterized by the above.

【0015】また、上記した課題は、上記した記録媒体
を有し、前記記録層は磁性層であることを特徴とする磁
気ディスク装置によって解決される。次に、本発明の作
用について説明する。本発明によれば、記録媒体上に形
成される潤滑剤膜を二層構造とし、上側の潤滑剤の塗布
溶剤に対して下側の潤滑剤の分子の90%以上を不溶化
させるようにしている。
Further, the above-mentioned object is achieved by a magnetic disk drive having the above-mentioned recording medium, wherein the recording layer is a magnetic layer. Next, the operation of the present invention will be described. According to the present invention, the lubricant film formed on the recording medium has a two-layer structure, and 90% or more of the molecules of the lower lubricant are made insoluble in the solvent of the upper lubricant. .

【0016】これにより、下側の潤滑剤層をボンド層と
し、上側の潤滑剤層をモバイル層となるように、下側と
上側の潤滑剤層を2つの性質に分けることができる。こ
の場合、下側の潤滑剤層を構成する材料として極性基ま
たは7つ以上のπ電子が導入された基を未端基に有する
ポリマーを用いることにより、下側の潤滑剤層によって
潤滑膜の被塗布体上での移動が防止される。また、上側
の潤滑剤層を構成する材料として非極性基を有するポリ
マーを用いることにより、上側の潤滑剤層によって潤滑
膜のヘッドへの付着が防止され、しかも、コンタミの潤
滑膜への付着が防止されて結露痕が発生しにくくなる。
なお、その非極性基は、7つ以上のπ電子を有しない。
Thus, the lower and upper lubricant layers can be divided into two properties so that the lower lubricant layer is a bond layer and the upper lubricant layer is a mobile layer. In this case, by using a polymer having a non-terminal group having a polar group or a group into which seven or more π electrons are introduced as a material constituting the lower lubricant layer, the lower lubricant layer forms a lubricant film. Movement on the object is prevented. In addition, by using a polymer having a non-polar group as a material constituting the upper lubricant layer, the upper lubricant layer prevents the lubricant film from adhering to the head, and furthermore, prevents the contamination from adhering to the lubricant film. It is prevented and dew marks are hardly generated.
Note that the non-polar group does not have seven or more π electrons.

【0017】[0017]

【発明の実施の形態】以下に本発明の実施形態を図面に
基づいて説明する。発明者らは、上記した課題を解決す
るために鋭意検討を重ねた結果、図2に示すように、潤
滑剤を2層構造で塗布し、かつ、上層の潤滑剤14の塗
布の段階で下層の潤滑剤13の90%以上が上層の潤滑
剤14の塗布溶剤に不溶化していることを特徴とする潤
滑膜の形成方法を見出した。
Embodiments of the present invention will be described below with reference to the drawings. As a result of diligent studies to solve the above-mentioned problems, the inventors applied a lubricant in a two-layer structure as shown in FIG. A method for forming a lubricating film, characterized in that 90% or more of the lubricant 13 is insoluble in the coating solvent of the upper lubricant 14.

【0018】図2は、本発明の実施形態に係る記録ディ
スクの断面図であって、非磁性基板10の上には記録磁
性層11、保護層12が順に形成され、保護層12の上
には下層の潤滑剤13と上層の潤滑剤14が順に塗布さ
れていて、その二層構造潤滑剤が全体として潤滑層15
として機能する。ここで特に、下層の潤滑剤13が、末
端基に極性基または7つ以上のπ電子が導入された基を
有する弗素系ポリマーであること、及び上層の潤滑剤1
2が末端基に極性基を持たない弗素系ポリマーであるこ
とが本発明のポイントとなる。
FIG. 2 is a sectional view of a recording disk according to an embodiment of the present invention. A recording magnetic layer 11 and a protective layer 12 are sequentially formed on a non-magnetic substrate 10. The lower layer lubricant 13 and the upper layer lubricant 14 are sequentially applied.
Function as In particular, the lower lubricant 13 is a fluorine-based polymer having a polar group or a group into which seven or more π electrons are introduced as a terminal group, and the upper lubricant 1
The point of the present invention is that 2 is a fluorine-based polymer having no polar group in the terminal group.

【0019】すなわち、基板側の材料と結合しやすい吸
着基を末端に有するポリマーからなる下層の潤滑剤13
をボンド層として用いる一方で、上層の潤滑剤14はヘ
ッドスライダヘの吸着を抑える必要があるため、吸着し
やすい極性基を末端基に持たない材料から上層の潤滑剤
14を構成してモバイル層として用いる。ここで、上層
の潤滑剤14を下層の潤滑剤13上に塗布する際に、下
層の潤滑剤13が上層の潤滑剤14の塗布溶媒に多量に
溶解すると、上層の潤滑剤14に下層の潤滑剤13がミ
キシングして2層構造が形成できなくなるため、上層の
潤滑剤14の塗布前の段階で下層の潤滑剤13の90%
以上、好ましくは95%以上、更に好ましくは100%
が上層の潤滑剤12の塗布溶剤に不溶化していることが
必要である。
That is, the lower lubricant 13 made of a polymer having an adsorbing group at the terminal which is easily bonded to the material on the substrate side.
Is used as the bond layer, while the upper lubricant 14 needs to suppress adsorption to the head slider. Therefore, the upper lubricant 14 is composed of a material that does not have a polar group which is easily adsorbed at the terminal group, and the mobile lubricant is formed. Used as Here, when the upper lubricant layer 14 is applied on the lower lubricant layer 13, if the lower lubricant layer 13 is dissolved in a large amount in the solvent for the application of the upper lubricant layer 14, the lower lubricant layer 13 is applied to the upper lubricant layer 14. Since the mixing of the lubricant 13 makes it impossible to form a two-layer structure, 90% of the lubricant 13 in the lower layer is used before the application of the lubricant 14 in the upper layer.
Or more, preferably 95% or more, more preferably 100%
Must be insoluble in the coating solvent of the upper lubricant 12.

【0020】このため、例えば図3(a) に示すように、
下層の潤滑剤13を被塗布体(例えば、保護層12)上
に塗布した後に、光照射と加熱の少なくとも一方の処理
によって潤滑剤13を架橋させ、架橋後の潤滑剤13の
90%以上をゲル化する方法を用いる。その後、図3
(b) に示すように、下層の潤滑剤13の上に上層の潤滑
剤14を塗布する。
For this reason, for example, as shown in FIG.
After applying the lower lubricant 13 on the object to be coated (for example, the protective layer 12), the lubricant 13 is cross-linked by at least one of light irradiation and heating, and 90% or more of the cross-linked lubricant 13 is removed. A gelling method is used. Then, FIG.
As shown in (b), the upper lubricant 14 is applied on the lower lubricant 13.

【0021】また、例えば図4(a),(b) に示すように、
下層の潤滑剤13を被塗布体に塗布した後に、潤滑剤分
子を溶解できる溶剤により潤滑層13を洗浄することに
よって、洗浄後の潤滑剤13の90%以上をその上に塗
布される潤滑剤用の溶剤に対して不溶可にすることもで
きる。その洗浄は常に清浄な液体で洗浄することが好ま
しいことから、上記した溶剤の蒸気を用いて洗浄するこ
とが好ましい。
For example, as shown in FIGS. 4 (a) and 4 (b),
After applying the lower lubricant 13 to the object to be coated, the lubricant 13 is washed with a solvent capable of dissolving the lubricant molecules, so that 90% or more of the washed lubricant 13 is applied thereon. Insoluble in a solvent for use. Since it is preferable that the cleaning is always performed with a clean liquid, it is preferable to perform the cleaning using the vapor of the solvent described above.

【0022】この場合、潤滑剤13を構成するポリマー
分子の末端の極性基が被塗布体の材料と結合し、ポリマ
ー分子同士が結合したり絡み合っているので、洗浄処理
によって被塗布体上の潤滑層11が無くなることはな
く、その多くは被塗布体上に残っている。ところで、前
述のような上層の潤滑剤14は、ヘッドスライダとの吸
着をなくすために、末端基に極性基と7つ以上のπ電子
を持つ基とを有しない弗素系ポリマーであることが好ま
しい。この上層の潤滑剤12は、末端基に水酸基、カル
ボキシル基、カルボニル基、エステル基、工ーテル基、
アミノ基、イミド基、アジド基等の極牲基を持たないも
のであれば特に限定されないが、末端基にCF3 基を有す
るパーフロロポリエーテルを特に好ましく用いることか
できる。
In this case, since the polar group at the end of the polymer molecule constituting the lubricant 13 is bonded to the material of the object to be coated, and the polymer molecules are bonded or entangled, the lubrication on the object to be coated is performed by the cleaning treatment. The layer 11 is not lost, and much of it remains on the object to be coated. Incidentally, the upper lubricant 14 as described above is preferably a fluorine-based polymer having no polar group and no group having seven or more π electrons in the terminal group in order to eliminate adsorption to the head slider. . The upper lubricant 12 has a hydroxyl group, a carboxyl group, a carbonyl group, an ester group, a polyester group,
There is no particular limitation as long as it does not have polar groups such as an amino group, an imide group, and an azide group. Perfluoropolyether having a CF 3 terminal group can be particularly preferably used.

【0023】末端基に極性基を持たない弗素系ポリマー
としては、次の化学式(1)で示される構造物がある。
なお、式(1)でR’で示した基は、非極性基であって
7つ以上のπ電子を持たない。
As a fluorine-based polymer having no polar group in the terminal group, there is a structure represented by the following chemical formula (1).
The group represented by R ′ in the formula (1) is a non-polar group and does not have seven or more π electrons.

【0024】[0024]

【化1】 Embedded image

【0025】このような材料からなる上層の潤滑剤14
は、その末端基によって、コンタミを引きつけにくく、
ヘッドスライダに付着し難い。また、下層の潤滑剤13
は、逆に被塗布体(保護層12)への吸着が高い方が好
ましく、吸着力が高い末端基を有するか、または、前述
の光照射、加熱の少なくとも一方の処理により架橋する
官能基を有する潤滑剤であれば特に限定されない。この
場合、末端基に極性による吸着能カの高い極性基、また
はπ電子による吸着能カの高い7つ以上のπ電子か導入
された基を有する弗素系ポリマーを好ましく用いること
ができる。特に、末端基にビペロニル基、または7つ以
上のπ電子を持つトリオルガノシリル基を有するパーフ
ロロポリエーテルが好ましい。
The upper lubricant 14 made of such a material
Is difficult to attract contamination due to its terminal group,
Hard to adhere to the head slider. The lower lubricant 13
On the contrary, it is preferable that the adsorption to the object to be coated (the protective layer 12) is high, and the terminal group has a terminal group having a high adsorption force or a functional group which is crosslinked by at least one of the above-described light irradiation and heating. It is not particularly limited as long as it has a lubricant. In this case, it is preferable to use a fluorine-based polymer having, as a terminal group, a polar group having a high adsorptivity due to polarity or a group into which seven or more π electrons having a high adsorptivity due to π electrons have been introduced. In particular, a perfluoropolyether having a biperonyl group or a triorganosilyl group having 7 or more π electrons in a terminal group is preferable.

【0026】末端基に極性基または7つ以上のπ電子が
導入された基を有する弗素系ポリマーとしては、次の化
学式(2)で示される構造物がある。極性基として、例
えばハロゲン、ニトロ基、メトキシル基がある。なお、
式(2)においてRは、極性基、又は7つ以上のπ電子
を持つ基を示している。
As a fluorine-based polymer having a polar group or a group having seven or more π electrons introduced into its terminal group, there is a structure represented by the following chemical formula (2). Examples of the polar group include a halogen, a nitro group, and a methoxyl group. In addition,
In the formula (2), R represents a polar group or a group having seven or more π electrons.

【0027】[0027]

【化2】 Embedded image

【0028】このような材料からなる下層の潤滑剤13
は、被塗布体との吸着が強く、移動し難い上に、酸素の
部分で上層の潤滑剤14の分子とも比較的ボンドし易
い。また、このようなポリマーは、分子同士で結合もす
る。以上のような2層構造の潤滑層は、極性基を有さな
い高撥水性の上層のみがモバイル(フリー)層として働
くが、図5に示すように、2層構造の潤滑膜15を形成
した後、その2層の潤滑剤13,14に放射線照射を行
い、光架橋により上層の潤滑剤14の一部をボンド層と
して用いてもよい。ここで、放射線は、上層の潤滑剤1
4を構成するポリマーの末端基(例えば、CF3 基)を架
橋させることのできる遠紫外線、電子線、またはX線で
あることか好ましく、特に効率良く架橋させるために、
遠紫外線から真空紫外線領域の波長で半値幅15nm以下
の単色光を用いることが好ましい。さらに効率よく架橋
を行うためには、例えばKrF ,ArF ,XeCl,KrCl,X
e2 ,F2,Kr, Ar等のエキシマ光を用いることが好まし
い。
The lower lubricant 13 made of such a material
Is strongly adsorbed on the object to be coated, is hard to move, and is relatively easily bonded to molecules of the upper lubricant 14 in the oxygen portion. Such polymers also bond between molecules. In the lubricating layer having the two-layer structure as described above, only the high water-repellent upper layer having no polar group functions as a mobile (free) layer. However, as shown in FIG. After that, the two layers of lubricants 13 and 14 may be irradiated with radiation, and a part of the upper layer lubricant 14 may be used as a bond layer by photocrosslinking. Here, the radiation is applied to the upper lubricant 1
It is preferably a deep ultraviolet ray, an electron beam, or an X-ray capable of cross-linking the terminal group (for example, CF 3 group) of the polymer constituting 4, and in order to cross-link particularly efficiently,
It is preferable to use monochromatic light having a half-value width of 15 nm or less in a wavelength range from far ultraviolet rays to vacuum ultraviolet rays. For more efficient cross-linking, for example, KrF, ArF, XeCl, KrCl, X
It is preferable to use excimer light such as e 2 , F 2 , Kr, and Ar.

【0029】ここで放射線照射雰囲気は、空気中照射で
発生するオゾンによる酸化で潤滑剤の摩擦力が高まるの
を抑制するために、不活性ガスまたは真空雰囲気である
ことか好ましい。不活性ガスは、例えば窒素、アルゴ
ン、ヘリウムの少なくとも1つで置換された雰囲気を好
ましく用いることができる。また、光照射により潤滑剤
を架橋させる際には、図6に示すように、加熱処理しな
がら照射を行うと架橋の効率を上げることができ、プロ
セス時間の短縮に好ましく用いることができる。加熱処
理温度は、被加熱基体の熱安定性により選んで用いる。
磁気媒体の場合は、30℃〜300℃が好ましく、80
〜150℃を特に好ましく用いる。これより温度が低い
と架橋の効果が不十分であり、それより高いと磁性体や
保護膜の各特性が劣化する。
Here, the radiation irradiation atmosphere is preferably an inert gas or a vacuum atmosphere in order to suppress an increase in the frictional force of the lubricant due to oxidation by ozone generated by irradiation in the air. As the inert gas, for example, an atmosphere substituted with at least one of nitrogen, argon, and helium can be preferably used. In addition, when the lubricant is crosslinked by light irradiation, as shown in FIG. 6, if irradiation is performed while heating, the efficiency of crosslinking can be increased, which can be preferably used for shortening the process time. The heat treatment temperature is selected and used depending on the thermal stability of the substrate to be heated.
In the case of a magnetic medium, the temperature is preferably from 30 ° C to 300 ° C,
~ 150 ° C is particularly preferably used. If the temperature is lower than this, the effect of crosslinking is insufficient, and if it is higher than this, the properties of the magnetic substance and the protective film deteriorate.

【0030】本発明で、2層構造の潤滑膜を形成する方
法は特に限定されないが、ディップコート法、スピンコ
ート法を好ましく用いることができる。また、2層構造
の潤滑層の膜厚はトータルで1〜100Åが好ましく、
更に好ましくは5〜20Åである。これより薄いと磨耗
耐性は劣化し、厚いと摩擦特性が劣化する。潤滑層の上
層/下層の膜厚比は50/ 50〜1/ 99を好ましく用
いることかできる。これより上層が厚い場合にはディス
ク回転時のスピンオフの影響が大きくなり、また上層が
薄い場合には2層構造とした効果が不十分となる。
In the present invention, the method of forming a two-layer lubricating film is not particularly limited, but a dip coating method and a spin coating method can be preferably used. The total thickness of the two-layer lubricating layer is preferably 1 to 100 °,
More preferably, it is 5 to 20 °. If the thickness is smaller than this, the abrasion resistance deteriorates, and if it is thicker, the friction characteristics deteriorate. The thickness ratio of the upper layer / lower layer of the lubricating layer is preferably 50/50 to 1/99. If the upper layer is thicker than this, the effect of spin-off during disk rotation becomes greater, and if the upper layer is thinner, the effect of the two-layer structure becomes insufficient.

【0031】潤滑膜を塗布する際の被塗布体(保護層)
は、高記録密度磁気媒体の場合CVD法で成膜した膜厚
8nm以下のDLC(ダイアモンドライクカーボン)膜
を好ましく用いることができる。CVD成膜は、スパッ
タ成膜より薄いDLC膜を被塗布体上に供給できるた
め、磁気スペーシングの短縮が可能であるが、薄いため
に金属マイグレーションの頻度が高くなる。この際、本
発明の架橋度と撥水性の高い2層構造潤滑膜によるコン
タミ除去効果により、従来の潤滑膜形成方法よりも高温
高湿下で優れた腐食耐性能力を有効に発揮でき、信頼性
の高い高記録密度磁気媒体を供給できる。
Coating body (protective layer) when applying lubricating film
For a high recording density magnetic medium, a DLC (diamond-like carbon) film having a thickness of 8 nm or less formed by a CVD method can be preferably used. In the CVD film formation, a DLC film thinner than the sputtering film formation can be supplied onto the object to be coated, so that the magnetic spacing can be shortened. However, since the film is thin, the frequency of metal migration increases. At this time, due to the contamination removal effect of the two-layered lubricating film having high degree of crosslinking and high water repellency of the present invention, it is possible to effectively exhibit excellent corrosion resistance ability under high temperature and high humidity as compared with the conventional method of forming a lubricating film. A high recording density magnetic medium having a high density can be supplied.

【0032】このように本実施形態による潤滑膜形成方
法及び形成装置は、特に磁気ディスク媒体または磁気デ
ィスク装置の製造に好ましく用いることができるが、磁
気ディスク関連以外の用途にも適用することができる。
以下、本発明の実施例を示すが、本発明の内容は実施例
の内容に限定されるものではない。
As described above, the method and apparatus for forming a lubricating film according to the present embodiment can be preferably used particularly for manufacturing a magnetic disk medium or a magnetic disk device, but can also be applied to uses other than those related to magnetic disks. .
Hereinafter, although an example of the present invention is shown, the contents of the present invention are not limited to the contents of an example.

【0033】第1例 まず、図7(a) に示すように、アルミニウム基板20上
に磁性層21、保護膜22を有する構造を磁気ディスク
として用意した。この磁気ディスクは、NiP メッキされ
たアルミニウム基板20を研磨し、テクスチャー処理し
て中心線粗さ(Ra)を6.5nmとした後に、そのアル
ミニウム基板20上に、DCマグネトロンスパソタリン
グによりArガス雰囲気中でCr,CoCrTa系磁性層21を2
0nmの厚さに形成し、さらに、その磁性層21の上に
CVD法で膜厚8nmのDLC保護膜22を形成する工
程を経て形成される。
First Example First, as shown in FIG. 7A, a structure having a magnetic layer 21 and a protective film 22 on an aluminum substrate 20 was prepared as a magnetic disk. This magnetic disk is obtained by polishing and texturing a NiP-plated aluminum substrate 20 to have a center line roughness (Ra) of 6.5 nm, and then applying an Ar gas atmosphere on the aluminum substrate 20 by DC magnetron sputtering. Cr and CoCrTa based magnetic layers 21
It is formed to a thickness of 0 nm, and further through a step of forming a DLC protective film 22 having a thickness of 8 nm on the magnetic layer 21 by the CVD method.

【0034】そして、図7(b) に示すように、末端ビペ
ロニル基を有するパーフロロポリエーテルよりなる下層
潤滑膜23を保護膜22上にディップコート法で成膜
し、酸素濃度10ppm 以下の窒素雰囲気中で波長172
nmのXeエキシマランプからの光を100秒間で800mJ
/cm2の量で下層潤滑膜23に照射し、下層潤滑膜23内
で潤滑剤同士を架橋させた。媒体上のその下層潤滑膜2
3の膜厚を測定したところ10Åであった。
Then, as shown in FIG. 7 (b), a lower lubricating film 23 made of perfluoropolyether having a terminal biperonyl group is formed on the protective film 22 by a dip coating method. Wavelength 172 in atmosphere
800mJ in 100 seconds from Xe excimer lamp
The lower lubricating film 23 was irradiated at an amount of / cm 2 to crosslink the lubricants in the lower lubricating film 23. The lower lubricating film 2 on the medium
The film thickness of No. 3 was measured to be 10 °.

【0035】さらに、図7(c) に示すように、末端CF3
基を有するパーフロロポリエーテルよりなる上層潤滑膜
24を下層潤滑膜23上にディップコート法で5Åの厚
さで塗布した。これにより2層構造の潤滑膜25が保護
膜22上に形成される。次に、上記した下層潤滑膜23
のボンド率を調べるため、上層潤滑膜24を形成せず
に、下層潤滑膜23のみを上記と同様の条件で10Åの
膜厚で成膜した媒体を上層活性層24の塗布溶媒(3M
社製FC‐77)に浸漬してモバイル成分を溶解除去し、膜
厚を再測定した。
Furthermore, as shown in FIG. 7 (c), the terminal CF 3
An upper lubricating film 24 made of perfluoropolyether having a group was applied on the lower lubricating film 23 by a dip coating method to a thickness of 5 °. As a result, a two-layer lubricating film 25 is formed on the protective film 22. Next, the lower lubricating film 23
In order to examine the bond ratio of the upper active layer 24, a medium in which only the lower lubricating film 23 was formed to a thickness of 10 ° under the same conditions as above without forming the upper lubricating film 24 was used.
The mobile component was dissolved and removed by immersion in FC-77 (manufactured by Sharp), and the film thickness was measured again.

【0036】潤滑膜のボンド率は、上層潤滑膜24の塗
布用の溶媒に対して下層潤滑膜23がどの程度ボンドし
ているかを示すものであって、溶媒によって下層潤滑膜
23を溶解した後の溶解後膜厚を溶解前の初期膜厚で割
って求めた値の百分率で表される。その測定の結果、溶
解後膜厚は9.8Åとなり、下層潤滑膜23のボンド率
は98%であることから、上層潤滑膜24の塗布時に上
層潤滑膜24と下層潤滑膜23の間ではミキシング層が
殆ど形成されていないことを確認した。
The bond ratio of the lubricating film indicates the degree to which the lower lubricating film 23 is bonded to the solvent for coating the upper lubricating film 24. Is expressed as a percentage of the value obtained by dividing the film thickness after dissolution by the initial film thickness before dissolution. As a result of the measurement, the film thickness after dissolution was 9.8 °, and the bond ratio of the lower lubricating film 23 was 98%. Therefore, the mixing between the upper lubricating film 24 and the lower lubricating film 23 during the application of the upper lubricating film 24 was performed. It was confirmed that almost no layer was formed.

【0037】以上のような2層潤滑膜が塗布された磁気
記録媒体と、下層のみを15Å塗布した従来の磁気記録
媒体を準備し、それぞれ温度80℃、湿度90%の高温
高湿槽に入れて媒体を結露させた後に、CSSテスター
にて10Hz、3分間ヘッドシークを行い、シーク後の磁
気ヘッドを顕微鏡観察したところ、下層潤滑膜のみが存
在する磁気記録媒体によれば結露痕と潤滑剤吸着成分に
よりヘッドが汚染されていたのに対し、本第1例の2層
潤滑剤膜を有する磁気記録媒体によれば大幅にヘッド汚
染量が低減されていることがわかった。
A magnetic recording medium coated with the two-layer lubricating film as described above and a conventional magnetic recording medium coated with only the lower layer at 15 ° are prepared and placed in a high-temperature and high-humidity tank at 80 ° C. and 90% humidity, respectively. After the medium was condensed, the head was sought with a CSS tester at 10 Hz for 3 minutes, and the magnetic head after the seek was observed under a microscope. According to the magnetic recording medium having only the lower lubricating film, the dew condensation marks and the lubricant were observed. While the head was contaminated by the adsorbed component, it was found that the magnetic recording medium having the two-layer lubricant film of the first example greatly reduced the amount of head contamination.

【0038】第2例 まず、図8(a) に示すように、アルミニウム基板30上
に磁性層31、保護膜32を有する構造を磁気ディスク
として用意した。この磁気ディスクは、NiP メッキされ
たアルミニウム基板30を研磨し、テクスチャー処理し
て中心線粗さ(Ra)を6.5nmとした後に、そのアル
ミニウム基板30上に、DCマグネトロンスパソタリン
グによりArガス雰囲気中でCr,CoCrTa系磁性層31を2
0nmの厚さに形成し、さらに、その磁性層31の上に
CVD法で膜厚8nmのDLC保護膜32を形成する工
程を経て形成される。
Second Example First, as shown in FIG. 8A, a structure having a magnetic layer 31 and a protective film 32 on an aluminum substrate 30 was prepared as a magnetic disk. This magnetic disk is prepared by polishing and texture-treating a NiP-plated aluminum substrate 30 to have a center line roughness (Ra) of 6.5 nm, and then applying an Ar gas atmosphere on the aluminum substrate 30 by DC magnetron sputtering. Cr and CoCrTa based magnetic layers 31
It is formed to a thickness of 0 nm, and further through a step of forming a DLC protective film 32 having a thickness of 8 nm on the magnetic layer 31 by the CVD method.

【0039】次に、図8(b) に示すように、末端トリフ
ェニルシリル基を有するパーフロロポリエーテルからな
る下層潤滑膜33をディップコート法で保護膜32上に
成膜する。さらに、3M社製FC‐77溶媒の蒸気に下
層潤滑膜33を晒して蒸気洗浄を行った。蒸気洗浄後の
下層潤滑膜33の膜厚を測定したところ10Åであっ
た。
Next, as shown in FIG. 8B, a lower lubricating film 33 made of perfluoropolyether having a terminal triphenylsilyl group is formed on the protective film 32 by dip coating. Further, the lower lubricating film 33 was exposed to the vapor of 3M FC-77 solvent to perform vapor cleaning. When the film thickness of the lower lubricating film 33 after the steam cleaning was measured, it was 10 °.

【0040】次に、図8(c) に示すように、末端CF3
を有するパーフロロポリエーテルよりなる上層潤滑膜3
4をディップコート法で下層潤滑層33上に5Åの厚さ
で塗布した。これにより2層潤滑膜35が保護膜32上
に形成された。そして、下層潤滑膜33のボンド率を調
べるため、下層潤滑膜33のみを上記と同様に10Å成
膜した磁気記録媒体を上層潤滑膜34用の塗布溶媒(3
M社製FC‐77)に浸漬して下層潤滑膜33の表面のモバ
イル成分を溶解除去し、下層潤滑膜33の膜厚を再測定
した。
Next, as shown in FIG. 8C, an upper lubricating film 3 made of perfluoropolyether having a terminal CF 3 group is formed.
4 was applied on the lower lubricating layer 33 by a dip coating method in a thickness of 5 °. As a result, a two-layer lubricating film 35 was formed on the protective film 32. Then, in order to examine the bond ratio of the lower lubricating film 33, a magnetic recording medium in which only the lower lubricating film 33 was formed at a thickness of 10 ° in the same manner as described above was coated with a coating solvent (3
The mobile component on the surface of the lower lubricating film 33 was dissolved and removed by immersion in FC-77 manufactured by M Company, and the thickness of the lower lubricating film 33 was measured again.

【0041】その結果、溶解後のその膜厚は約10Åで
あり、下層潤滑膜33のボンド率(溶解後膜厚/初期膜
厚)は100%となることから、上層潤滑膜33の塗布
時に下層潤滑膜33と上層潤滑膜34の間にミキシング
層は殆ど形成されていないことが確認された。上記した
2層潤滑剤膜35が塗布された磁気記録媒体と、下層潤
滑膜のみが15Å塗布された磁気記録媒体を準備し、そ
れぞれ温度80℃、湿度90%の高温音湿槽に入れて媒
体を結露させた後に、CSSテスターにて10Hz、3分
間ヘッドシークを行い、シーク後のヘッドを顕微鏡観察
したところ、下層潤滑膜のみを有する磁気記録媒体では
結露痕と潤滑剤吸着成分によりヘッドが汚染されていた
のに対し、本第2例の2層潤滑剤は大幅にヘッド汚染量
が低減されていることがわかった。
As a result, the film thickness after dissolution is about 10 °, and the bond ratio (film thickness after dissolution / initial film thickness) of the lower lubricating film 33 is 100%. It was confirmed that almost no mixing layer was formed between the lower lubricating film 33 and the upper lubricating film 34. A magnetic recording medium coated with the above-described two-layer lubricant film 35 and a magnetic recording medium coated with only the lower-layer lubricating film at 15 ° are prepared and placed in a high-temperature sound and humidity chamber at a temperature of 80 ° C. and a humidity of 90%, respectively. After condensing, the head was sought with a CSS tester at 10 Hz for 3 minutes, and the head after the seek was observed under a microscope. In the case of a magnetic recording medium having only a lower lubricating film, the head was contaminated by dew condensation traces and lubricant adsorption components. On the other hand, it was found that the two-layer lubricant of the second example significantly reduced the amount of head contamination.

【0042】第3例 第1例、第2例と同様に磁気ディスク上に2層構造の潤
滑膜25(35)を形成した後、図9に示すように、窒
素(N2)雰囲気(酸素濃度10ppm 以下)中で波長17
2nm のXeエキシマランプにより光を100秒(80
0mJ/cm2)照射して上層潤滑膜23(33)と下層潤滑
膜24(34)の潤滑剤同士を架橋させた。
Third Example After forming a two-layer lubricating film 25 (35) on a magnetic disk in the same manner as in the first and second examples, as shown in FIG. 9, a nitrogen (N 2 ) atmosphere (oxygen Concentration of 10 ppm or less)
Light is emitted for 100 seconds (80 seconds) by a 2 nm Xe excimer lamp.
0 mJ / cm 2 ) was applied to crosslink the lubricants of the upper lubricating film 23 (33) and the lower lubricating film 24 (34).

【0043】この2層構造の潤滑膜25を有する媒体
と、下層潤滑膜のみを15Å塗布した媒休を準備し、そ
れぞれ温度80℃、湿度90%の高温高湿槽に入れてそ
れらの潤滑膜の表面で結露させた後、CSSテスターに
て10H z、3分間ヘッドシークを行い、シーク後のヘ
ッドを顕微鏡観察した。この結果、下層潤滑膜のみの媒
体では結露痕と潤滑剤吸着成分により磁気ヘッドが汚染
されていたのに対し、2層構造の潤滑膜ではヘッド汚染
が殆ど観察されなかった。
A medium having the two-layered lubricating film 25 and a medium having only the lower lubricating film coated by 15 ° are prepared, and put into a high-temperature and high-humidity bath at a temperature of 80 ° C. and a humidity of 90%, respectively. After dew condensation on the surface of the head, head seek was performed at 10 Hz for 3 minutes with a CSS tester, and the head after seek was observed under a microscope. As a result, the magnetic head was contaminated by the dew mark and the lubricant adsorbed component in the medium having only the lower lubricating film, whereas the head contamination was hardly observed in the lubricating film having the two-layer structure.

【0044】なお、窒素の代わりにアルゴン等の不活性
ガスを用いてもよいが、いずれも酸素濃度が10ppm 以
下であることが好ましい。第4例 実施例2、3と同様な工程で磁気記録媒体を形成した。
そして、図10に示すように、その磁気記録媒体41
と、アルミナとTiC との焼結体からなるスライダ42上
に形成された薄膜磁気ヘッド(不図示)と、スライダ4
2を支持するアームが取り付けられた磁気ディスク装置
40において、ヘッド荷重1.5gfにて静止状態から回
転速度1rpm への立ち上がり時における静摩擦係数μs
をディスク摩擦試験機で調ぺた。その結果を、表1に示
す。
Note that an inert gas such as argon may be used instead of nitrogen, but the oxygen concentration is preferably 10 ppm or less in any case. Fourth Example A magnetic recording medium was formed in the same steps as in Examples 2 and 3.
Then, as shown in FIG.
A thin-film magnetic head (not shown) formed on a slider 42 made of a sintered body of alumina and TiC;
The coefficient of static friction μ s at the time of rising from a stationary state to a rotation speed of 1 rpm with a head load of 1.5 gf in the magnetic disk device 40 to which the arm supporting
Was tested using a disk friction tester. Table 1 shows the results.

【0045】[0045]

【表1】 [Table 1]

【0046】表1の結果によれば、上記した第2例、第
3例で示した2層構造の潤滑層を持つ磁気ディスクで
は、第2例で述べた単層の下層潤滑層のみを有する磁気
ディスクに比べて、水接触角が高くて撥水性が良好であ
り、しかも摩擦係数が小さくなってスライダの摩耗を低
減することがわかった。なお、上記した2層構造の潤滑
層は、記録層の上に直に形成してもよい。 (付記)上記した潤滑膜形成方法は、被塗布体の上に下
側の潤滑剤層を塗布する工程と、塗布溶剤を含む上側の
潤滑剤層を前記下側の潤滑剤層の上に塗布する工程を有
し、前記下側の層潤滑剤の90%以上を前記塗布溶剤に
不溶化する状態にさせることを特徴とする。 (1)上記した潤滑膜形成方法において、前記下側の層
潤滑剤の90%以上を前記塗布溶剤に不溶化する状態に
させるのは、前記上側の潤滑剤層を塗布する前に行って
もよい。 (2)上記した潤滑膜形成方法において、前記下側の潤
滑剤層は、末端基にピペロニル基、7つ以上のπ電子を
有するトリオルガノシリル基のいずれかの基を有するパ
ーフロロポリエーテルであってもよい。 (3)前記放射線が遠紫外線、電子線、X線のいずれか
であってもよい。 (4)前記前記下側の層潤滑剤の90%以上を前記塗布
溶剤に不溶化する状態にさせるのは前記上側の潤滑剤層
を塗布した後に、放射線を照射することによって行わ
れ、その放射線は遠紫外線から真空紫外線領域の波長で
半値幅15nm以下の単色光であり、かつその照射雰囲
気が不活性ガス又は真空であるようにしてもよい。 (5)前記被塗布体は、磁性層を有していてもよい。
According to the results shown in Table 1, the magnetic disk having the two-layer lubricating layer shown in the second and third examples has only the single lower lubricating layer described in the second example. It was found that the water contact angle was higher and the water repellency was better than that of a magnetic disk, and the coefficient of friction was reduced to reduce wear of the slider. The lubricating layer having the two-layer structure described above may be formed directly on the recording layer. (Supplementary Note) In the above-described method for forming a lubricating film, a step of applying a lower lubricant layer on an object to be coated and a step of applying an upper lubricant layer containing a coating solvent on the lower lubricant layer And a step of making at least 90% of the lower layer lubricant insoluble in the coating solvent. (1) In the lubricating film forming method described above, the step of making at least 90% of the lower layer lubricant insoluble in the coating solvent may be performed before applying the upper lubricant layer. . (2) In the lubricating film forming method described above, the lower lubricant layer is a perfluoropolyether having any one of a piperonyl group and a triorganosilyl group having seven or more π electrons in a terminal group. There may be. (3) The radiation may be any one of a deep ultraviolet ray, an electron beam, and an X-ray. (4) Making at least 90% of the lower layer lubricant insoluble in the coating solvent is performed by applying radiation after applying the upper lubricant layer, and the radiation is applied. The light may be monochromatic light having a half-value width of 15 nm or less in a wavelength range from far ultraviolet to vacuum ultraviolet, and the irradiation atmosphere may be an inert gas or vacuum. (5) The object may have a magnetic layer.

【0047】[0047]

【発明の効果】以上述べたように本発明により.潤滑剤
と基板のボンド率が高く、摩擦、磨耗が低く、かつ撥水
性が高い潤滑膜を供給することができ、これによりヘッ
ド部分への潤滑剤や結露痕成分の堆積に起因するヘッド
クラッシュを防止でき、特に高温高湿環境での使用にお
いても信頼性の著しく高い磁気ディスク装置を供給する
ことができる。
As described above, according to the present invention. A high bond rate between the lubricant and the substrate, a low friction and wear, and a highly water-repellent lubricating film can be supplied, which prevents head crashes due to the accumulation of lubricant and condensation traces on the head. Thus, it is possible to provide a magnetic disk device having extremely high reliability even when used in a high-temperature and high-humidity environment.

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

【図1】図1は、従来の磁気ディスクの構成断面図であ
る。
FIG. 1 is a configuration sectional view of a conventional magnetic disk.

【図2】図2は、本発明の実施形態に係る磁気ディスク
の断面図である。
FIG. 2 is a sectional view of a magnetic disk according to the embodiment of the present invention.

【図3】図3(a),(b) は、本発明の実施形態に係る2層
構造潤滑膜の第1の形成工程を示す断面図である。
FIGS. 3A and 3B are cross-sectional views showing a first forming step of a two-layer structure lubricating film according to an embodiment of the present invention.

【図4】図4(a),(b) は、本発明の実施形態に係る2層
構造潤滑膜の第2の形成工程を示す断面図である。
FIGS. 4A and 4B are cross-sectional views showing a second forming step of a two-layer lubricating film according to the embodiment of the present invention.

【図5】図5は、本発明の実施形態に係る2層構造潤滑
膜の第3の形成工程を示す断面図である。
FIG. 5 is a cross-sectional view showing a third forming step of the two-layer lubricating film according to the embodiment of the present invention.

【図6】図6は、本発明の実施形態に係る2層構造潤滑
膜の第4の形成工程を示す断面図である。
FIG. 6 is a sectional view showing a fourth forming step of the two-layer structure lubricating film according to the embodiment of the present invention.

【図7】図7(a) 〜(c) は、本発明の実施形態の2層構
造潤滑膜の形成工程の第1例を示す断面図である。
FIGS. 7A to 7C are cross-sectional views showing a first example of a step of forming a two-layer lubricating film according to the embodiment of the present invention.

【図8】図8(a) 〜(c) は、本発明の実施形態の2層構
造潤滑膜の形成工程の第2例を示す断面図である。
FIGS. 8A to 8C are cross-sectional views showing a second example of the process of forming a two-layer lubricating film according to the embodiment of the present invention.

【図9】図9は、本発明の実施形態の2層構造潤滑膜の
形成工程の第2例を示す断面図である。
FIG. 9 is a cross-sectional view showing a second example of the process of forming a two-layer lubricating film according to the embodiment of the present invention.

【図10】図10は、本発明の実施形態の磁気ディスク
ドライブを示す平面図である。
FIG. 10 is a plan view showing a magnetic disk drive according to the embodiment of the present invention.

【符号の説明】[Explanation of symbols]

10…基板、11…磁性層、12…保護膜、13…下層
の潤滑剤、14…上層の潤滑剤、15…潤滑膜、20…
基板、21…磁性層、22…保護膜、23…下層の潤滑
剤、24…上層の潤滑剤、25…潤滑膜、30…基板、
31…磁性層、32…保護膜、33…下層の潤滑剤、3
4…上層の潤滑剤、35…潤滑膜、40…磁気ディスク
装置、41…磁気記録ディスク、42…スライダー、4
3…アーム。
Reference Signs List 10: substrate, 11: magnetic layer, 12: protective film, 13: lower lubricant, 14: upper lubricant, 15: lubricating film, 20 ...
Substrate, 21: magnetic layer, 22: protective film, 23: lower lubricant, 24: upper lubricant, 25: lubricating film, 30: substrate,
31: magnetic layer, 32: protective film, 33: lower lubricant, 3
4: Upper layer lubricant, 35: Lubricating film, 40: Magnetic disk device, 41: Magnetic recording disk, 42: Slider, 4
3 ... arm.

フロントページの続き (51)Int.Cl.7 識別記号 FI テーマコート゛(参考) // C23C 16/27 C23C 16/27 5D112 C10N 40:18 C10N 40:18 (72)発明者 山川 栄進 山形県東根市大字根元東根字大森5400番2 (番地なし) 株式会社山形富士通内 (72)発明者 板井 雄一郎 神奈川県川崎市中原区上小田中4丁目1番 1号 富士通株式会社内 Fターム(参考) 4D075 AE03 BB26Z BB42Z BB85Y DC28 EA37 4H104 CD04A LA03 LA20 PA16 4J038 DF011 NA22 PA07 PA17 PA19 PB11 4K030 BA28 CA02 DA08 HA04 LA20 5D006 AA01 AA02 AA06 DA03 FA05 5D112 AA07 AA11 BC02 BC05 CC01 CC12 CC13 FA09 Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat II (reference) // C23C 16/27 C23C 16/27 5D112 C10N 40:18 C10N 40:18 (72) Inventor Eishin Yamakawa Higashine-shi, Yamagata 5400-2 Omori, Higashi Nemoto, No. 5400-2 (No address) Inside Yamagata Fujitsu Co., Ltd. (72) Inventor Yuichiro Itai 4-1-1 Kamikodanaka, Nakahara-ku, Kawasaki City, Kanagawa Prefecture F-term within Fujitsu Co., Ltd. 4D075 AE03 BB26Z BB42Z BB85Y DC28 EA37 4H104 CD04A LA03 LA20 PA16 4J038 DF011 NA22 PA07 PA17 PA19 PB11 4K030 BA28 CA02 DA08 HA04 LA20 5D006 AA01 AA02 AA06 DA03 FA05 5D112 AA07 AA11 BC02 BC05 CC01 CC12 CC13 FA09

Claims (10)

【特許請求の範囲】[Claims] 【請求項1】被塗布体の上に下側の潤滑剤層を塗布する
工程と、 塗布溶剤を含む上側の潤滑剤層を前記下側の潤滑剤層の
上に塗布する工程を有し、 前記下側の層潤滑剤の90%以上を前記塗布溶剤に不溶
化する状態にさせることを特徴とする潤滑膜形成方法。
1. A step of applying a lower lubricant layer on an object to be coated, and a step of applying an upper lubricant layer containing a coating solvent on the lower lubricant layer, A lubricating film forming method, wherein 90% or more of the lower layer lubricant is made insoluble in the coating solvent.
【請求項2】前記下側の潤滑剤層を前記被塗布体に塗布
した後に、光照射、加熱のうち少なくとも一方の処理に
より前記下側の潤滑剤層を架橋させ、架橋後の前記下側
の潤滑剤層の90%以上がゲル化していることを特徴と
する請求項1記載の潤滑膜形成方法。
2. The method according to claim 1, wherein the lower lubricant layer is cross-linked by applying at least one of light irradiation and heating after the lower lubricant layer is applied to the object. 2. The method according to claim 1, wherein 90% or more of the lubricant layer is gelled.
【請求項3】前記下側の潤滑剤層を前記被塗布体に塗布
した後、前記下側の潤滑剤層の一部の分子を溶剤の蒸気
により洗浄し、この洗浄後の前記下側の潤滑剤層の90
%以上が前記上側の潤滑剤層の前記塗布溶剤に不溶可し
ていることを特徴とする請求項1記載の潤滑膜形成方
法。
3. After the lower lubricant layer is applied to the object to be coated, some molecules of the lower lubricant layer are washed with a solvent vapor, and the lower lubricant layer after the washing is removed. 90 of lubricant layer
2. The method of claim 1, wherein at least about% is insoluble in the coating solvent of the upper lubricant layer. 3.
【請求項4】前記上側の潤滑剤層は、末端基に極性基を
持たない弗素系ポリマーからなることを特徴とする請求
項1〜請求項3のいずれかに記載の潤滑膜形成方法。
4. The method according to claim 1, wherein the upper lubricant layer is made of a fluorine-based polymer having no polar group in a terminal group.
【請求項5】前記上側の潤滑剤層は、末端基にCF3 基を
有するパーフロロポリエーテルからなることを特徴とす
る請求項4に記載の潤滑膜形成方法。
5. The method according to claim 4, wherein said upper lubricant layer is made of perfluoropolyether having a CF 3 group at a terminal group.
【請求項6】前記下側の潤滑剤層は、未端基に極性基、
7つ以上のπ電子が導入された基のいずれかの基を持つ
弗素系ポリマーからなることを特徴とする請求項1〜請
求項3のいずれかに記載の潤滑膜形成方法。
6. The lower lubricant layer has a polar group at an unterminated group,
The lubricating film forming method according to any one of claims 1 to 3, wherein the method comprises a fluorine-based polymer having any one of groups into which seven or more π electrons have been introduced.
【請求項7】前記下側の潤滑剤層と前記上側の潤滑剤層
を形成した後に、前記下側の潤滑剤層と前記上側の潤滑
剤層に放射線を照射することを特徴とする請求項1〜請
求項6のいずれかに記載の潤滑膜形成方法。
7. The method according to claim 1, wherein the lower lubricant layer and the upper lubricant layer are irradiated with radiation after forming the lower lubricant layer and the upper lubricant layer. The method for forming a lubricating film according to claim 1.
【請求項8】前記被塗布体の最表層は、CVD法で成膜
したカーボン薄膜であることを特徴とする請求項1〜請
求項7のいずれかに記載の潤滑膜形成方法。
8. The method according to claim 1, wherein the outermost layer of the object to be coated is a carbon thin film formed by a CVD method.
【請求項9】記録層と、 前記記録層の上に塗布され、且つ、未端基に極性基、7
つ以上のπ電子が導入された基のいずれかを有する第1
のポリマーからなる下側の潤滑剤層と、 前記下側の潤滑剤層の上に塗布され、且つ、末端に第1
のポリマーと異なる末端基を有する第2のポリマーから
なる上側の潤滑剤層とを有することを特徴とする記録媒
体。
9. A recording layer, a polar group coated on the recording layer and having an unterminated group,
A first group having at least one group into which one or more π electrons have been introduced;
A lower lubricant layer composed of a polymer of the formula:
And an upper lubricant layer comprising a second polymer having a different end group.
【請求項10】請求項9に記載の記録媒体を有し、前記
記録層は磁性層であることを特徴とする磁気ディスク装
置。
10. A magnetic disk drive having the recording medium according to claim 9, wherein said recording layer is a magnetic layer.
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US7252897B2 (en) 2002-09-03 2007-08-07 Hoya Corporation Magnetic recording disk and process for manufacture thereof
JP2010067299A (en) * 2008-09-09 2010-03-25 Toshiba Storage Device Corp Magnetic disk device
JP2010086598A (en) * 2008-09-30 2010-04-15 Hoya Corp Method for manufacturing magnetic disk
JP2010135037A (en) * 2008-12-08 2010-06-17 Showa Denko Kk Testing method for recoding medium and method for manufacturing recoding medium
JP2010152959A (en) * 2008-12-24 2010-07-08 Hoya Corp Magnetic disk and method of manufacturing the same

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JPS61211827A (en) * 1985-03-16 1986-09-19 Hitachi Maxell Ltd Magnetic recording medium
JP2000003512A (en) * 1998-06-15 2000-01-07 Hitachi Ltd Magnetic disk and magnetic disk device having the same
JP2001184622A (en) * 1999-12-28 2001-07-06 Fuji Electric Co Ltd Magnetic recording medium, its producing method and magnetic recording device

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JP2001184622A (en) * 1999-12-28 2001-07-06 Fuji Electric Co Ltd Magnetic recording medium, its producing method and magnetic recording device

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7252897B2 (en) 2002-09-03 2007-08-07 Hoya Corporation Magnetic recording disk and process for manufacture thereof
US7277254B2 (en) 2002-09-03 2007-10-02 Hoya Corporation Magnetic recording disk and process for manufacture thereof
JP2010067299A (en) * 2008-09-09 2010-03-25 Toshiba Storage Device Corp Magnetic disk device
JP2010086598A (en) * 2008-09-30 2010-04-15 Hoya Corp Method for manufacturing magnetic disk
JP2010135037A (en) * 2008-12-08 2010-06-17 Showa Denko Kk Testing method for recoding medium and method for manufacturing recoding medium
JP2010152959A (en) * 2008-12-24 2010-07-08 Hoya Corp Magnetic disk and method of manufacturing the same

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