JP2000260017A - Magnetic recording medium and production of magnetic recording medium - Google Patents
Magnetic recording medium and production of magnetic recording mediumInfo
- Publication number
- JP2000260017A JP2000260017A JP37160199A JP37160199A JP2000260017A JP 2000260017 A JP2000260017 A JP 2000260017A JP 37160199 A JP37160199 A JP 37160199A JP 37160199 A JP37160199 A JP 37160199A JP 2000260017 A JP2000260017 A JP 2000260017A
- Authority
- JP
- Japan
- Prior art keywords
- integer
- lubricant
- recording medium
- magnetic recording
- perfluoropolyether
- 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
Links
Landscapes
- Lubricants (AREA)
- Magnetic Record Carriers (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、コンピューターの
外部記録装置に搭載される磁気記録媒体および該磁気記
録媒体の製造方法に関する。特に本発明は、磁気記録媒
体の表面に液体潤滑剤を塗布して潤滑特性およびＣＳＳ
耐久性を改善する。The present invention relates to a magnetic recording medium mounted on an external recording device of a computer and a method for manufacturing the magnetic recording medium. In particular, the present invention is to apply a liquid lubricant to the surface of a magnetic recording medium to improve the lubrication characteristics and CSS.
Improve durability.
【０００２】[0002]
【従来の技術】固体磁気記録媒体を用いた記録装置等
は、一般に、磁気記録媒体の回転時には磁気ヘッドが浮
上し、回転駆動モータが停止した時には磁気ヘッドが磁
気記録媒体表面と接触するコンタクト・スタート・スト
ップ（ＣＳＳ）方式が採用されている。従来の磁気記録
媒体は、表面保護層としてダイヤモンド状カーボン（Ｄ
ＬＣ）に、さらに少量のＮやＳｉ等を添加したものが用
いられている。そして、一般に、このような表面保護層
の潤滑特性を改良するために、分子内に水酸基やピペロ
ニル基などの有極性末端基を有するパーフルオロポリエ
ーテル系潤滑剤を単独または環状トリホスファゼン系潤
滑剤と組み合わせて該表面保護層上を塗布する。このよ
うな潤滑剤で保護層表面を覆い尽くすことは、表面にガ
スや有機汚染物が吸着することを防ぎ、さらに潤滑特性
を向上させ、ＣＳＳ耐久性に優れかつ安定した磁気記録
媒体を得る一つの手段となる。2. Description of the Related Art Generally, in a recording apparatus using a solid magnetic recording medium, a magnetic head floats when the magnetic recording medium is rotating, and contacts when the rotary drive motor stops when the magnetic head comes into contact with the surface of the magnetic recording medium. A start / stop (CSS) method is employed. Conventional magnetic recording media use diamond-like carbon (D
LC) to which a small amount of N, Si, or the like is further added. Generally, in order to improve the lubricating properties of such a surface protective layer, a perfluoropolyether-based lubricant having a polar terminal group such as a hydroxyl group or a piperonyl group in a molecule is used alone or in a cyclic triphosphazene-based lubricant. And apply on the surface protective layer. Covering the surface of the protective layer with such a lubricant can prevent gas and organic contaminants from adsorbing to the surface, further improve the lubricating properties, and provide a stable magnetic recording medium having excellent CSS durability. Means.
【０００３】ＤＬＣ系カーボンの表面は、反応性のカル
ボニル基、カルボキシル基や水酸基等の官能基を有する
薄い酸化膜で覆われており、ここに、汚染物が積極的に
吸着、結合し存在する。このような汚染物の吸着は、極
性末端基を有するパーフルオロポリエーテルを使用する
ことで抑止することができるが、使用するパーフルオロ
ポリエーテルの分子量が低すぎると潤滑特性が低下し、
逆に分子量が高すぎるとヘッドと潤滑層との吸着傾向が
高くなる。そのため、重量平均分子量が１，５００〜
５，５００であるパーフルオロポリエーテルが一般に使
用されている。しかし、比較的分子量の大きいパーフル
オロポリエーテルを使用した場合、一般的に保護層上に
数１０Å塗布した程度では分子と分子との間に隙間が生
じ、保護層表面を完全に覆うことは困難である。このよ
うな比較的分子量の大きいパーフルオロポリエーテルを
使用して保護層表面を完全に覆うためには、潤滑層の膜
厚を５０Å以上に厚く塗布しなければならず、５０Å位
まで厚くすると磁気記録媒体と磁気ヘッドとの吸着を回
避することは困難である。[0003] The surface of DLC-based carbon is covered with a thin oxide film having a functional group such as a reactive carbonyl group, carboxyl group, or hydroxyl group, and contaminants are actively adsorbed and bonded to the thin oxide film. . The adsorption of such contaminants can be suppressed by using a perfluoropolyether having a polar end group, but if the molecular weight of the perfluoropolyether used is too low, the lubricating properties deteriorate,
Conversely, if the molecular weight is too high, the tendency of adsorption between the head and the lubricating layer increases. Therefore, the weight average molecular weight is 1,500 to
5,500 perfluoropolyethers are commonly used. However, when a perfluoropolyether having a relatively large molecular weight is used, a gap is generally formed between molecules when several tens of degrees are applied on the protective layer, and it is difficult to completely cover the surface of the protective layer. It is. In order to completely cover the surface of the protective layer using such a perfluoropolyether having a relatively high molecular weight, the lubricating layer must be applied to a thickness of 50 mm or more. It is difficult to avoid adsorption between the recording medium and the magnetic head.
【０００４】近年では高密度記録に伴い磁気ヘッドの低
浮上化が進み、磁気ヘッドの構造も従来のＴＲＣヘッド
からＴｒｉ−Ｐａｄヘッド、ＭＲヘッド等の低浮上型ヘ
ッドが採用されるようになってきた。それに伴い、ヘッ
ド材質が触媒作用を受けるか、または摩擦熱を発生する
ことにより、パーフルオロポリエーテル系潤滑剤の主鎖
部（エーテル部位）では分解が進むことになる。さら
に、この分解物やディスク表面に吸着したガス等の腐食
成分が磁気ヘッド表面に転写され、磁気ヘッドの浮上特
性を乱し、再生出力の低下を招くことになる。また、分
解したパーフルオロポリエーテル系潤滑剤は、潤滑特性
が低下するため保護層の摩耗が生じ、最悪の場合、ヘッ
ドクラッシュを引き起こすことになる。In recent years, the flying height of a magnetic head has been reduced due to high-density recording, and the structure of the magnetic head has been changed from a conventional TRC head to a low flying type head such as a Tri-Pad head or an MR head. Was. As a result, the head material is catalyzed or generates frictional heat, so that the decomposition proceeds in the main chain portion (ether portion) of the perfluoropolyether-based lubricant. Further, corrosive components such as these decomposed products and gas adsorbed on the disk surface are transferred to the surface of the magnetic head, disturbing the flying characteristics of the magnetic head, and lowering the reproduction output. In addition, the decomposed perfluoropolyether-based lubricant deteriorates the lubricating properties, causing wear of the protective layer, and in the worst case, causes a head crash.
【０００５】一方で、従来から環状トリホスファゼン系
潤滑剤は、潤滑特性の向上やパーフルオロポリエーテル
系潤滑剤の分解抑制に効果があることが知られている。
例えば、特開平９−３０５９６１号公報では、以下の構
造式で示されるような環状トリホスファゼン系潤滑剤を
パーフルオロポリエーテル系潤滑剤と組み合わせて使用
することにより磁気記録媒体における潤滑特性が改善さ
れることを開示している。On the other hand, it has been known that a cyclic triphosphazene-based lubricant is effective in improving lubricating characteristics and suppressing decomposition of a perfluoropolyether-based lubricant.
For example, in JP-A-9-305961, the lubricating properties of a magnetic recording medium are improved by using a cyclic triphosphazene-based lubricant represented by the following structural formula in combination with a perfluoropolyether-based lubricant. It is disclosed that.
【０００６】[0006]
【化７】 Embedded image
【０００７】[0007]
【発明が解決しようとする課題】しかし、パーフルオロ
ポリエーテル系潤滑剤と環状トリフォスファゼン系潤滑
剤とは非常に混ざりにくく、さらに潤滑層として塗布さ
れ、ある環境下に放置されると凝集してしまうという解
決すべき課題がある。その結果、従来の技術では固定磁
気記録媒体を用いた記録装置の特性が大幅に低下するこ
とがある。However, the perfluoropolyether-based lubricant and the cyclic triphosphazene-based lubricant are very difficult to mix with each other, and are further applied as a lubricating layer and aggregate when left in a certain environment. There is a problem to be solved. As a result, the characteristics of the recording apparatus using the fixed magnetic recording medium in the related art may be significantly reduced.
【０００８】上述した課題を解決するために、各種パー
フルオロポリエーテル系潤滑剤を用いる試みが種々なさ
れているが、要求される全ての性能を満足し得る技術は
未だ確立されていないのが現状である。Various attempts have been made to use various perfluoropolyether-based lubricants in order to solve the above-mentioned problems. However, a technique capable of satisfying all required performances has not yet been established. It is.
【０００９】従って、本発明の目的は、高密度記録に伴
う磁気ヘッドの低浮上化による潤滑剤の分解、保護膜の
摩耗を防止し、長期にわたる潤滑特性の安定化（ＣＳＳ
耐久性の向上）を実現する磁気記録媒体およびその製造
方法を提供することである。Accordingly, an object of the present invention is to prevent the decomposition of a lubricant and the abrasion of a protective film due to the low flying height of a magnetic head accompanying high-density recording, and to stabilize the lubrication characteristics for a long time (CSS
It is an object of the present invention to provide a magnetic recording medium that realizes (improvement in durability) and a method for manufacturing the same.
【００１０】[0010]
【課題を解決するための手段】本発明者らは、前記の目
的を達成するため、潤滑層に用いる潤滑剤について鋭意
検討した結果、潤滑特性の向上またはパーフルオロポリ
エーテル系潤滑剤の分解抑制に効果をもつ環状トリホス
ファゼン系潤滑剤と、パーフルオロポリエーテル系潤滑
剤とを同一分子構造内に有する化合物を使用し、前記の
目的を達成できることを見出し本願発明を完成するに至
った。Means for Solving the Problems In order to achieve the above object, the present inventors have intensively studied a lubricant used for a lubricating layer, and as a result, have improved lubricating properties or suppressed decomposition of a perfluoropolyether-based lubricant. It has been found that the above-mentioned object can be achieved by using a compound having a cyclic triphosphazene-based lubricant and a perfluoropolyether-based lubricant having the same effect in the same molecular structure, thereby completing the present invention.
【００１１】すなわち、本発明の磁気記録媒体は、非磁
性基体上に下地層、磁性層、保護層、および潤滑層を有
し、上記潤滑層が分子内に環状トリホスファゼン末端基
を有するパーフルオロポリエーテル系潤滑剤を含むこと
を特徴とする。That is, the magnetic recording medium of the present invention has a base layer, a magnetic layer, a protective layer, and a lubricating layer on a nonmagnetic substrate, and the lubricating layer has a cyclic triphosphazene terminal group in the molecule. It is characterized by containing a polyether-based lubricant.
【００１２】ここで、上述した分子内に環状トリホスフ
ァゼン末端基を有するパーフルオロポリエーテル系潤滑
剤は、以下の構造式：The above-mentioned perfluoropolyether-based lubricant having a cyclic triphosphazene terminal group in the molecule is represented by the following structural formula:
【００１３】[0013]
【化８】 Embedded image
【００１４】（式中、ｎは１から５の整数、ｐは０また
は１以上の整数、ｑは０または１以上の整数）、Wherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more.
【００１５】[0015]
【化９】 Embedded image
【００１６】（式中、ｎは１から５の整数、ｐは０また
は１以上の整数、ｑは０または１以上の整数）、およびWherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more.
【化１０】 （式中、ｎは１から５の整数、ｐは０または１以上の整
数、ｑは０または１以上の整数）からなる群から少なく
とも１つ選ぶことができる。Embedded image Wherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more.
【００１７】また、本発明の磁気記録媒体の製造方法
は、非磁性基体上に下地層を積層する工程と、該下地層
上に磁性層を積層する工程と、該磁性層上に保護層を積
層する工程と、該保護層上に潤滑層を積層する工程とを
具え、上記潤滑層は、以下の構造式：Further, the method for manufacturing a magnetic recording medium of the present invention comprises a step of laminating a base layer on a non-magnetic substrate, a step of laminating a magnetic layer on the base layer, and a step of forming a protective layer on the magnetic layer. And a step of laminating a lubricating layer on the protective layer, wherein the lubricating layer has the following structural formula:
【００１８】[0018]
【化１１】 Embedded image
【００１９】（式中、ｎは１から５の整数、ｐは０また
は１以上の整数、ｑは０または１以上の整数）、Wherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more.
【００２０】[0020]
【化１２】 Embedded image
【００２１】（式中、ｎは１から５の整数、ｐは０また
は１以上の整数、ｑは０または１以上の整数）およびWherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more.
【化１３】 （式中、ｎは１から５の整数、ｐは０または１以上の整
数、ｑは０または１以上の整数）からなる群から選ばれ
る分子内に環状トリホスファゼン末端基を有するパーフ
ルオロポリエーテル系潤滑剤を少なくとも１つ用いて形
成されることを特徴とする。Embedded image Wherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is an integer of 0 or 1 or more. A perfluoropolyether having a cyclic triphosphazene terminal group in a molecule selected from the group consisting of: It is characterized by being formed using at least one system lubricant.
【００２２】ここで、上述した分子内に環状トリホスフ
ァゼン末端基を有するパーフルオロポリエーテル系潤滑
剤を塗布する方法は、ディップコート法またはスピンコ
ート法であることが好ましい。Here, the method for applying the above-mentioned perfluoropolyether-based lubricant having a cyclic triphosphazene terminal group in the molecule is preferably a dip coating method or a spin coating method.
【００２３】[0023]
【発明の実施の形態】本発明にもとづく磁気記録媒体
は、該磁気記録媒体の表面の潤滑特性を改善するために
潤滑層に分子内に環状トリホスファゼン末端基を有する
パーフルオロポリエーテル系潤滑剤を使用する。該分子
内に環状トリホスファゼン末端基を有するパーフルオロ
ポリエーテル系潤滑剤は、以下の構造式：BEST MODE FOR CARRYING OUT THE INVENTION A magnetic recording medium according to the present invention is a perfluoropolyether-based lubricant having a cyclic triphosphazene terminal group in a molecule in a lubricating layer in order to improve the lubricating properties of the surface of the magnetic recording medium. Use The perfluoropolyether-based lubricant having a cyclic triphosphazene terminal group in the molecule has the following structural formula:
【００２４】[0024]
【化１４】 Embedded image
【００２５】（式中、ｎは１から５の整数、ｐは０また
は１以上の整数、ｑは０または１以上の整数）、Wherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more.
【化１５】 （式中、ｎは１から５の整数、ｐは０または１以上の整
数、ｑは０または１以上の整数）およびEmbedded image (Where n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is an integer of 0 or 1 or more) and
【００２６】[0026]
【化１６】 Embedded image
【００２７】（式中、ｎは１から５の整数、ｐは０また
は１以上の整数、ｑは０または１以上の整数）からなる
群から選ばれる少なくとも１つの潤滑剤である。ここ
で、前記構造式（Ｉ）で示される潤滑剤におけるｎ、ｐ
およびｑの値、前記構造式（II）で示される潤滑剤にお
けるｎ、ｐおよびｑの値、および前記構造式 (III)で示
される潤滑剤におけるｎ、ｐおよびｑの値は、それぞれ
決定的なものではない。(Wherein, n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more). Here, n, p in the lubricant represented by the structural formula (I)
And q, the values of n, p and q in the lubricant represented by the structural formula (II), and the values of n, p and q in the lubricant represented by the structural formula (III) are decisive, respectively. Not something.
【００２８】構造式（Ｉ）、（II）または（III）で示
される分子内に環状トリホスファゼン末端基を有するパ
ーフルオロポリエーテル系潤滑剤は、限定されるもので
はないが、例えば、鎖状分子の末端に水酸基を有するパ
ーフルオロポリエーテルのナトリウムアルコキシド、ｍ
−トリフルオロメチルフェノールのナトリウムフェノキ
シドとを慣用の方法にしたがってそれぞれ調製し、これ
らを環状トリホスファゼン化合物と混合することによっ
て得られる。The perfluoropolyether-based lubricant having a cyclic triphosphazene terminal group in the molecule represented by the structural formula (I), (II) or (III) is not limited. Sodium alkoxide of perfluoropolyether having a hydroxyl group at the terminal of the molecule, m
-Trifluoromethylphenol and sodium phenoxide are each prepared according to a conventional method, and are obtained by mixing these with a cyclic triphosphazene compound.
【００２９】上記構造式（Ｉ）、（II）および (III)で
示される分子内に環状トリホスファゼン末端基を有する
パーフルオロポリエーテル潤滑剤は、単独でまたはこれ
らを組み合わせて使用することができ、単層または多層
の潤滑層にしてもよい。また、必要に応じて任意の溶剤
で希釈してもよく、０．０５重量％の濃度が適当であ
る。前記潤滑剤の塗布は、当業者に既知の方法、好まし
くはディップコート法、スピンコート法を用いて行う。The perfluoropolyether lubricant having a cyclic triphosphazene terminal group in the molecule represented by the above structural formulas (I), (II) and (III) can be used alone or in combination. It may be a single-layer or multi-layer lubrication layer. Further, if necessary, it may be diluted with an arbitrary solvent, and a concentration of 0.05% by weight is appropriate. The application of the lubricant is performed by a method known to those skilled in the art, preferably, a dip coating method or a spin coating method.
【００３０】本発明に係る分子内に環状トリホスファゼ
ン末端基を有するパーフルオロポリエーテル系潤滑剤を
使用し、磁気記録媒体の表面を完全に覆うことにより、
汚染物の吸着抑止および潤滑特性の向上を実現すること
ができ、その結果、ＣＳＳ耐久性に優れた磁気記録媒体
を得ることが可能となる。By using the perfluoropolyether-based lubricant having a cyclic triphosphazene terminal group in the molecule according to the present invention to completely cover the surface of the magnetic recording medium,
Suppression of contaminant adsorption and improvement of lubrication characteristics can be realized, and as a result, a magnetic recording medium having excellent CSS durability can be obtained.
【００３１】本発明に係る磁気記録媒体の一実施態様例
を図１に示し、図１を参照しながら以下に説明するが、
これらに限定されるものではない。One embodiment of the magnetic recording medium according to the present invention is shown in FIG. 1 and will be described below with reference to FIG.
It is not limited to these.
【００３２】本発明に係る磁気記録媒体の一実施態様例
では、非磁性基体１１（例えばＡｌ−Ｍｇ）および非磁
性金属層１２（例えば、合金基板上に無電解メッキした
Ｎｉ−Ｐ）とからなる非磁性の基体１、該基体１の上に
積層した非磁性の金属下地層２、該金属下地層２の上に
薄膜状に積層した強磁性合金である磁性層３（例えば、
Ｃｏ−Ｃｒ−Ｔａ、Ｃｏ−Ｃｒ−Ｐｔ等）、さらに該磁
性層３の上に積層した保護層４（例えば、ＤＬＣ）とを
備える。そして、前記のように保護層４まで順次積層し
た上に、さらに潤滑層５を設ける。In one embodiment of the magnetic recording medium according to the present invention, a non-magnetic substrate 11 (eg, Al—Mg) and a non-magnetic metal layer 12 (eg, Ni—P electrolessly plated on an alloy substrate) are used. A non-magnetic substrate 1, a non-magnetic metal underlayer 2 laminated on the substrate 1, and a magnetic layer 3 (for example, a ferromagnetic alloy laminated in a thin film on the metal underlayer 2).
Co-Cr-Ta, Co-Cr-Pt, etc.) and a protective layer 4 (for example, DLC) laminated on the magnetic layer 3. Then, a lubricating layer 5 is further provided after sequentially laminating up to the protective layer 4 as described above.
【００３３】以下、本発明に係る磁気記録媒体の製造方
法について実施例により説明するが、本発明は以下に示
す実施例に限定されるものではなく、その要旨を逸脱し
ない範囲において種々変更可能であることは言うまでも
ない。Hereinafter, the method for manufacturing a magnetic recording medium according to the present invention will be described with reference to examples. However, the present invention is not limited to the examples described below, and various modifications can be made without departing from the spirit of the present invention. Needless to say, there is.
【００３４】１．磁気記録媒体の作製 （実施例１）最初に本発明に係る磁気記録媒体の潤滑層
に使用する構造式（Ｉ）で示される潤滑剤の調製につい
て例示する。 1. Preparation of Magnetic Recording Medium (Example 1) First, the preparation of the lubricant represented by the structural formula (I) used for the lubricating layer of the magnetic recording medium according to the present invention will be exemplified.
【００３５】（ａ）ナトリウムアルコキシド化 蒸留などでよく脱水させた３０ｍｌのＨＦＥ７２００
（商品名、３Ｍ社製）に金属ナトリウム１．０ｇを加え
たものを、１０ｇのパーフルオロポリエーテル系化合物
（ＨＯ−ＣＨ2ＣＦ2（ＯＣＦ2ＣＦ2）p−（ＯＣＦ2）q
−ＯＣＦ2ＣＨ2−ＯＨ（ｐは０または１以上の整数、ｑ
は０または１以上の整数）、例えばFomblin Z-DOLアウ
ジモンド（株）社製）と０．１ｇのピリジンとを８０ｍ
ｌのＨＦＥ７２００に溶解させた溶液に加えた後、０℃
に冷却した。この溶液の温度を０℃以下に保ちながら、
１０時間にわたって撹拌した。ＮＭＲ測定により反応の
終点を確認した後、反応溶液を濾過して固形物を取り除
き、純水で洗浄し、さらにＨＦＥ７２００を除去して目
的とするナトリウム パーフルオロアルコキシド８．０
ｇを得た。(A) Sodium alkoxide formation 30 ml of HFE7200 well dehydrated by distillation or the like
1.0 g of perfluoropolyether compound (HO-CH 2 CF 2 (OCF 2 CF 2 ) p- (OCF 2 ) q
—OCF 2 CH 2 —OH (p is 0 or an integer of 1 or more, q
Is 0 or an integer of 1 or more), for example, Fomblin Z-DOL manufactured by Audimond Co., Ltd.) and 0.1 g of pyridine for 80 m.
1 HFE7200, added at 0 ° C.
And cooled. While keeping the temperature of this solution below 0 ° C,
Stirred for 10 hours. After confirming the end point of the reaction by NMR measurement, the reaction solution was filtered to remove solids, washed with pure water, and HFE7200 was removed to obtain the target sodium perfluoroalkoxide 8.0.
g was obtained.
【００３６】（ｂ）ナトリウムフェノキシド化 蒸留などでよく脱水させた３０ｍｌのジエチルエーテル
に金属ナトリウム１．０ｇを加えたものを、１０ｇのｍ
−トリフルオロメチルフェノールと０．１ｇのピリジン
とを８０ｍｌのジエチルエーテルに溶解させた溶液に加
えた後、０℃に冷却した。この溶液を０℃以下に保ちな
がら、５時間にわたって撹拌した。ＮＭＲ測定により反
応の終点を確認した後、反応溶液を濾過して固形物を取
り除き、純水で洗浄し、さらにジエチルエーテルを除去
して目的とするナトリウム ｍ−トリフルオロメチルフ
ェノキシド８．５ｇを得た。(B) Sodium phenoxide formation A mixture of 30 ml of diethyl ether, well dehydrated by distillation or the like, and 1.0 g of metallic sodium added to 10 g of m
-Added to a solution of trifluoromethylphenol and 0.1 g of pyridine in 80 ml of diethyl ether and cooled to 0 ° C. The solution was stirred for 5 hours while maintaining the temperature at 0 ° C or lower. After confirming the end point of the reaction by NMR measurement, the reaction solution was filtered to remove solid matter, washed with pure water, and further removed with diethyl ether to obtain 8.5 g of target sodium m-trifluoromethylphenoxide. Was.
【００３７】（ｃ）パーフルオロポリエーテル系潤滑剤
の調製 オートクレーブに、上記（ａ）で得られたナトリウム
パーフルオロポリエーテルアルコキシドを２．０ｇ、上
記（ｂ）で得られたナトリウム ｍ−トリフルオロメチ
ルフェノキシドを６．０ｇ、ヘキサクロロホスファゼン
Ｎ3Ｐ3Ｃｌ6を３．０ｇ、さらにＨＦＥ７２００を５０
ｍｌ入れて、オートクレーブ内をＮ2で置換した後、９
０℃で２５０時間にわたって反応させた。ＮＭＲ測定に
より反応の終点を確認した後、水およびエタノールで洗
浄し、所望の環状トリホスファゼンを鎖状分子の末端に
有する１，２，３，４，５，６−フロロヘプタノールを
２．４ｇ得た。得られた潤滑剤は必要に応じて適当な溶
剤で希釈して使用する。(C) Preparation of Perfluoropolyether Lubricant The sodium obtained in the above (a) was placed in an autoclave.
2.0 g of perfluoropolyether alkoxide, 6.0 g of sodium m-trifluoromethylphenoxide obtained in (b) above, 3.0 g of hexachlorophosphazene N 3 P 3 Cl 6 , and 50 g of HFE7200
After the autoclave was replaced with N 2 ,
The reaction was carried out at 0 ° C. for 250 hours. After confirming the end point of the reaction by NMR measurement, the reaction was washed with water and ethanol, and 2.4 g of 1,2,3,4,5,6-fluoroheptanol having the desired cyclic triphosphazene at the terminal of the chain molecule. Obtained. The obtained lubricant is used by diluting it with an appropriate solvent if necessary.
【００３８】次に、上述のようにして得られたパーフル
オロポリエーテル系潤滑剤を用いた磁気記録媒体の製造
について例示する。Next, the manufacture of a magnetic recording medium using the perfluoropolyether-based lubricant obtained as described above will be described.
【００３９】Ａｌ−Ｍｇ合金基板上に無電解メッキによ
りＮｉ−Ｐメッキを施した非磁性金属層を１３μｍ形成
し、その表面をポリッシュにより表面粗さＲａが１０Å
になるように研磨した後、ダイヤモンドスラリーを使用
して、表面粗さＲａが４０Åとなるように、同心円上の
溝をテクスチャー加工により施した。得られた基体を洗
浄した後、ＤＣスパッタ法により膜厚５００ÅのＣｒか
らなる非磁性金属下地層、次いで膜厚３００ÅのＣｏ−
Ｃｒ−Ｔａからなる磁性層、さらに膜厚１５０ÅのＤＬ
Ｃからなる保護層を作製した。A nonmagnetic metal layer having a Ni-P plating of 13 μm was formed on an Al—Mg alloy substrate by electroless plating, and the surface thereof was polished to a surface roughness Ra of 10 °.
After polishing, concentric grooves were formed by texture processing using diamond slurry so that the surface roughness Ra was 40 °. After the obtained substrate was washed, a nonmagnetic metal underlayer made of Cr having a thickness of 500 、 was formed by DC sputtering, and then a Co-
Magnetic layer made of Cr-Ta, and DL having a thickness of 150 °
A protective layer made of C was produced.
【００４０】上述のように保護層まで順次積層した上
（以下、保護層の上という）に、分子内に環状トリホス
ファゼン末端基を有するパーフルオロポリエーテル
（Ｉ）の潤滑剤を３Ｍ社製のＨＦＥ−７１００（商品
名）といったフルオロカーボンを溶剤として用いて希釈
し、０．０５重量％の濃度に調製した。得られた潤滑剤
溶液をディップコート法により塗布し、２０Åの潤滑層
を有する磁気記録媒体を作製した。As described above, a layer of a perfluoropolyether (I) having a cyclic triphosphazene terminal group in the molecule is further laminated with a lubricant of 3M Co., Ltd. It was diluted with a fluorocarbon such as HFE-7100 (trade name) as a solvent to prepare a concentration of 0.05% by weight. The obtained lubricant solution was applied by a dip coating method to produce a magnetic recording medium having a lubricating layer of 20 °.
【００４１】（実施例２）構造式（Ｉ）で示される潤滑
剤の代りに、分子内に環状トリホスファゼン末端基を有
するパーフルオロポリエーテル（II）の潤滑剤を使用す
ることを除いて、実施例１と同様に実施することにより
相当する磁気記録媒体を作製した。Example 2 A lubricant of perfluoropolyether (II) having a cyclic triphosphazene end group in the molecule was used instead of the lubricant represented by the structural formula (I), except that A corresponding magnetic recording medium was produced by performing the same operation as in Example 1.
【００４２】なお、構造式（II）で示される潤滑剤の調
製は、末端に水酸基を有するパーフルオロポリエーテル
として、ＨＯ−ＣＨ2ＣＦ2−（ＯＣＦ2ＣＦ2）p−（Ｏ
ＣＦ2）q−ＯＣＦ3（ｐは０または１以上の整数、ｑは
０または１以上の整数）を用いて実施した。The lubricant represented by the structural formula (II) was prepared as a perfluoropolyether having a hydroxyl group at a terminal as HO—CH 2 CF 2 — (OCF 2 CF 2 ) p — (O
CF 2) q -OCF 3 (p is 0 or an integer of 1 or more, q was carried out using a 0 or an integer of 1 or more).
【００４３】（実施例３）構造式（Ｉ）で示される潤滑
剤の代りに、分子内に環状トリホスファゼン末端基を有
するパーフルオロポリエーテル(III)の潤滑剤を使用す
ることを除いて、実施例１と同様に実施することにより
相当する磁気記録媒体を作製した。Example 3 A lubricant of perfluoropolyether (III) having a cyclic triphosphazene end group in the molecule was used instead of the lubricant represented by the structural formula (I), A corresponding magnetic recording medium was produced by performing the same operation as in Example 1.
【００４４】なお、構造式(III)で示される潤滑剤の調
製には、末端に水酸基を有するパーフルオロポリエーテ
ルとして、ＨＯ−ＣＨ2（ＣＦ2ＣＦ2）3Ｆ（ｐは０また
は１以上の整数、ｑは０または１以上の整数）を用いて
実施した。In preparing the lubricant represented by the structural formula (III), HO-CH 2 (CF 2 CF 2 ) 3 F (p is 0 or 1 or more) is used as a perfluoropolyether having a hydroxyl group at a terminal. , And q is 0 or an integer of 1 or more).
【００４５】（比較例１）構造式（Ｉ）で示される潤滑
剤の代りに、アウジモント社製のFomblin Z-dol4000
（商品名）といった水酸基を末端基に有するパーフルオ
ロポリエーテルを使用したことを除いて、実施例１と同
様に実施することにより相当する磁気記録媒体を作製し
た。(Comparative Example 1) Instead of the lubricant represented by the structural formula (I), Fomblin Z-dol4000 manufactured by Ausimont was used.
A corresponding magnetic recording medium was produced in the same manner as in Example 1, except that a perfluoropolyether having a hydroxyl group as a terminal group such as (trade name) was used.
【００４６】２．磁気記録媒体の評価 上述実施例１〜３および比較例１で作製した各々の磁気
記録媒体表面の潤滑層に関して、以下評価１および２に
示すような分解に対する評価を行った。 2. Evaluation of Magnetic Recording Medium With respect to the lubricating layers on the surfaces of the magnetic recording media produced in Examples 1 to 3 and Comparative Example 1, evaluations on decomposition as shown in Evaluations 1 and 2 below were performed.
【００４７】評価１ 上述実施例１〜３および比較例１において作製した各々
の磁気記録媒体の表面上に、Ａｌ2 Ｏ3 −ＴｉＣ粉と超
純水との混合液１滴を滴下し、次いでデシケータ内に入
れ８０℃／８０％相対湿度条件下で２４時間放置した。
次いで、磁気記録媒体の表面にある潤滑剤の分解の有無
をフーリエ変換式赤外分光光度計（ＦＴ−ＩＲ）を用い
て確認した。これらの結果を表１に示す。 Evaluation 1 One drop of a mixed solution of Al 2 O 3 —TiC powder and ultrapure water was dropped on the surface of each of the magnetic recording media prepared in Examples 1 to 3 and Comparative Example 1, and then It was placed in a desiccator and left under a condition of 80 ° C./80% relative humidity for 24 hours.
Next, the presence or absence of decomposition of the lubricant on the surface of the magnetic recording medium was confirmed using a Fourier transform infrared spectrophotometer (FT-IR). Table 1 shows the results.
【００４８】評価２ 上述実施例１〜３および比較例１において作製した各々
の磁気記録媒体の表面上に超純水１滴を滴下した媒体
と、１０ｃｃの１％Ｈ2ＳＯ4とを入れたシャーレをデシ
ケータ内に入れ８０℃／８０％相対湿度の条件下で２４
時間放置した。次いで、磁気媒体の表面にある潤滑剤の
分解の有無をフーリエ変換式赤外分光光度計（ＦＴ−Ｉ
Ｒ）を用いて確認した。これらの結果を表１に示す。 Evaluation 2 A medium in which one drop of ultrapure water was dropped on the surface of each of the magnetic recording media prepared in Examples 1 to 3 and Comparative Example 1, and 10 cc of 1% H 2 SO 4 were placed. Place the petri dish in a desiccator and place it under 80 ° C / 80% relative humidity for 24 hours.
Left for hours. Next, the presence or absence of decomposition of the lubricant on the surface of the magnetic medium is determined by a Fourier transform infrared spectrophotometer (FT-I).
R). Table 1 shows the results.
【００４９】[0049]
【表１】 [Table 1]
【００５０】表１から明らかなように、評価１および評
価２のいずれにおいても、潤滑層に本発明に係る分子内
に環状トリホスファゼン末端基を有するパーフルオロポ
リエーテル系潤滑剤を使用した磁気記録媒体（実施例１
〜３）では潤滑剤の分解が確認されなかった。一方、比
較例１では潤滑剤の分解が確認された。As is clear from Table 1, in both Evaluation 1 and Evaluation 2, magnetic recording was performed using the perfluoropolyether-based lubricant having a cyclic triphosphazene end group in the molecule according to the present invention in the lubricating layer. Medium (Example 1
In Nos. 3), no decomposition of the lubricant was confirmed. On the other hand, in Comparative Example 1, decomposition of the lubricant was confirmed.
【００５１】次に、上述実施例１〜３および比較例１に
おいて作製した磁気記録媒体に関して、以下評価３およ
び４に示すような潤滑特性の評価を行った。Next, the lubricating properties of the magnetic recording media manufactured in Examples 1 to 3 and Comparative Example 1 were evaluated as shown in Evaluations 3 and 4 below.
【００５２】評価３ 上述実施例１〜３および比較例１において作製した各々
の磁気記録媒体の表面上に、ヘッド荷重が３．５ｇｆの
磁気ヘッドを、半径位置１８．５ｍｍ、回転数１ｒｐｍ
で摺動させ、その時の動摩擦係数μIを測定した。次い
で、回転数１００ｒｐｍで摺動させた時の動摩擦係数μ
Lを測定した。これらの結果を表２に示す。 Evaluation 3 A magnetic head having a head load of 3.5 gf was placed on the surface of each of the magnetic recording media prepared in Examples 1 to 3 and Comparative Example 1 at a radial position of 18.5 mm and a rotation speed of 1 rpm.
In slid was measured dynamic friction coefficient mu I at that time. Next, the coefficient of dynamic friction μ when slid at a rotation speed of 100 rpm
L was measured. Table 2 shows the results.
【００５３】評価４ 上述実施例１〜３および比較例１において作製した各々
の磁気記録媒体を、評価３と同様のヘッドを用い実際の
磁気ディスクドライブに組み込み、初期摩擦係数μIを
測定した。次いで、常温／常湿（２５℃／５０％）と６
０℃／８０％相対湿度の条件下で２０，０００回のＣＳ
Ｓを繰り返した後、摩擦係数μLを測定した。また、６
０℃／８０％相対湿度の条件下で２０，０００回のＣＳ
Ｓを繰り返したものについて、ヘッドの汚れの有無を光
学顕微鏡により観察した。これらの結果を表２に示す。[0053] The magnetic recording medium of each prepared in the evaluation 4 above Examples 1-3 and Comparative Example 1, incorporated into actual magnetic disk drive using the same head and evaluation 3 was measured the initial friction coefficient mu I. Then, normal temperature / normal humidity (25 ° C / 50%) and 6
20,000 cycles of CS under the condition of 0 ° C / 80% relative humidity
After repeating the S, to measure the friction coefficient μ L. Also, 6
20,000 cycles of CS under the condition of 0 ° C / 80% relative humidity
With respect to the sample obtained by repeating S, the presence or absence of dirt on the head was observed with an optical microscope. Table 2 shows the results.
【００５４】[0054]
【表２】 [Table 2]
【００５５】表２から明らかなように、評価３および４
について、保護層を本発明に係る分子内に環状トリホス
ファゼン末端基を有するパーフルオロポリエーテル系潤
滑剤で塗布した磁気記録媒体は、いずれの環境において
も初期摩擦係数μI が小さく、２０，０００回のＣＳＳ
における摩擦係数の上昇も少ない。一方、比較例１では
摩擦係数が上昇し、さらに保護層の摩耗が生じた。この
ことから、本発明に係る潤滑剤を使用することで、磁気
記録媒体の摺動特性およびＣＳＳ耐久性を改善できるこ
とが分かった。As is clear from Table 2, evaluations 3 and 4
For magnetic recording medium coated with a perfluoropolyether lubricant having a cyclic Torihosufazen terminal group a protective layer in the molecule according to the present invention has a small initial friction coefficient mu I In either environment, 20,000 Times CSS
The rise of the coefficient of friction at the time is also small. On the other hand, in Comparative Example 1, the coefficient of friction increased, and the protective layer was further worn. From this, it was found that the use of the lubricant according to the present invention can improve the sliding characteristics and CSS durability of the magnetic recording medium.
【００５６】また、本発明に係る潤滑剤を保護層上に塗
布した磁気記録媒体において、ヘッドの汚れは確認でき
なかった。In the magnetic recording medium in which the lubricant according to the present invention was coated on the protective layer, no contamination of the head was confirmed.
【００５７】[0057]
【発明の効果】以上の説明から明らかなように、本発明
に係る分子内に環状トリホスファゼン末端基を有するパ
ーフルオロポリエーテル系潤滑剤を使用することによ
り、磁気ディスク表面からの潤滑剤や潤滑剤の分解物が
磁気ヘッドに転写されることなく、かつ高速回転時の保
護層の摩耗を防止することができる。その結果、従来の
ものに比べて長期使用時における潤滑層の特性安定に優
れた磁気記録媒体を提供することが可能である。As is apparent from the above description, by using the perfluoropolyether-based lubricant having a cyclic triphosphazene end group in the molecule according to the present invention, the lubricant and lubrication from the surface of the magnetic disk can be improved. The decomposition product of the agent is not transferred to the magnetic head, and the abrasion of the protective layer during high-speed rotation can be prevented. As a result, it is possible to provide a magnetic recording medium that is more excellent in stability of the characteristics of the lubricating layer during long-term use than the conventional one.
【図１】図１は、本発明にもとづく磁気記録媒体の一例
を示す断面斜視図である。FIG. 1 is a sectional perspective view showing an example of a magnetic recording medium according to the present invention.
１ 基体 ２ 非磁性下地層 ３ 磁性層 ４ 保護層 ５ 液体潤滑層 １１ 非磁性基板 １２ 非磁性金属層（メッキ層） DESCRIPTION OF SYMBOLS 1 Base | substrate 2 Nonmagnetic underlayer 3 Magnetic layer 4 Protective layer 5 Liquid lubrication layer 11 Nonmagnetic substrate 12 Nonmagnetic metal layer (plating layer)
Claims (4)
層、および潤滑層を有する磁気記録媒体において、前記
潤滑層は分子内に環状トリホスファゼン末端基を有する
パーフルオロポリエーテル系潤滑剤を含むことを特徴と
する磁気記録媒体。1. A magnetic recording medium having an underlayer, a magnetic layer, a protective layer, and a lubricating layer on a nonmagnetic substrate, wherein the lubricating layer is a perfluoropolyether-based lubricant having a cyclic triphosphazene terminal group in a molecule. A magnetic recording medium comprising:
基を有するパーフルオロポリエーテル系潤滑剤は、以下
の構造式： 【化１】 （式中、ｎは１から５の整数、ｐは０または１以上の整
数、ｑは０または１以上の整数）、 【化２】 （式中、ｎは１から５の整数、ｐは０または１以上の整
数、ｑは０または１以上の整数）、および 【化３】 （式中、ｎは１から５の整数、ｐは０または１以上の整
数、ｑは０または１以上の整数）からなる群から少なく
とも１つ選ばれることを特徴とする請求項１に記載の磁
気記録媒体。2. The perfluoropolyether-based lubricant having a cyclic triphosphazene terminal group in the molecule has the following structural formula: (Wherein, n is an integer of 1 to 5, p is an integer of 0 or 1 or more, and q is an integer of 0 or 1 or more). Wherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more. The method according to claim 1, wherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more. Magnetic recording medium.
と、該下地層上に磁性層を積層する工程と、該磁性層上
に保護層を積層する工程と、該保護層上に潤滑層を積層
する工程とを具えた磁気記録媒体の製造方法において、 前記潤滑層は、以下の構造式： 【化４】 （式中、ｎは１から５の整数、ｐは０または１以上の整
数、ｑは０または１以上の整数）、 【化５】 （式中、ｎは１から５の整数、ｐは０または１以上の整
数、ｑは０または１以上の整数）および 【化６】 （式中、ｎは１から５の整数、ｐは０または１以上の整
数、ｑは０または１以上の整数）からなる群から選ばれ
る分子内に環状トリホスファゼン末端基を有するパーフ
ルオロポリエーテル系潤滑剤の少なくとも１つを用いて
形成されることを特徴とする磁気記録媒体の製造方法。3. A step of laminating an underlayer on a nonmagnetic substrate, a step of laminating a magnetic layer on the underlayer, a step of laminating a protective layer on the magnetic layer, and a step of lubricating on the protective layer. A lubricating layer, wherein the lubricating layer has the following structural formula: (Wherein, n is an integer of 1 to 5, p is an integer of 0 or 1 or more, and q is an integer of 0 or 1 or more). Wherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is 0 or an integer of 1 or more. Wherein n is an integer of 1 to 5, p is 0 or an integer of 1 or more, and q is an integer of 0 or 1 or more. A perfluoropolyether having a cyclic triphosphazene terminal group in a molecule selected from the group consisting of: A method for manufacturing a magnetic recording medium, wherein the method is formed using at least one of a system lubricant.
基を有するパーフルオロポリエーテル系潤滑剤を塗布す
る方法が、ディップコート法またはスピンコート法であ
ることを特徴とする請求項３に記載の磁気記録媒体の製
造方法。4. The method according to claim 3, wherein the method of applying the perfluoropolyether-based lubricant having a cyclic triphosphazene terminal group in the molecule is a dip coating method or a spin coating method. Manufacturing method of recording medium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP37160199A JP4326097B2 (en) | 1999-01-07 | 1999-12-27 | Magnetic recording medium and method of manufacturing the magnetic recording medium |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP218599 | 1999-01-07 | ||
| JP11-2185 | 1999-01-07 | ||
| JP37160199A JP4326097B2 (en) | 1999-01-07 | 1999-12-27 | Magnetic recording medium and method of manufacturing the magnetic recording medium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000260017A true JP2000260017A (en) | 2000-09-22 |
| JP4326097B2 JP4326097B2 (en) | 2009-09-02 |
Family
ID=26335524
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP37160199A Expired - Lifetime JP4326097B2 (en) | 1999-01-07 | 1999-12-27 | Magnetic recording medium and method of manufacturing the magnetic recording medium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4326097B2 (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006009057A1 (en) * | 2004-07-23 | 2006-01-26 | Matsumura Oil Research Corp. | Lubricant for recording medium and magnetic disk |
| SG130014A1 (en) * | 2002-09-03 | 2007-03-20 | Hoya Corp | Magnetic recording disk and process for manufacturing thereof |
| WO2007083792A1 (en) * | 2006-01-23 | 2007-07-26 | Hoya Corporation | Magnetic disk |
| WO2007105437A1 (en) * | 2006-02-28 | 2007-09-20 | Matsumura Oil Research Corp. | Lubricating agent for recording medium and magnetic disk |
| JP2008008681A (en) * | 2006-06-27 | 2008-01-17 | Fuji Electric Device Technology Co Ltd | Film thickness measuring method for lubrication layer of magnetic recording medium and magnetic recording medium |
| WO2008140121A1 (en) * | 2007-05-15 | 2008-11-20 | Matsumura Oil Research Corp. | Perfluoropolyether compound, and lubricant and magnetic disk each using the same |
| JP2010006810A (en) * | 2008-06-23 | 2010-01-14 | Seagate Technology Llc | Lubricant compound and magnetic data storage device |
| US20110143165A1 (en) * | 2008-09-05 | 2011-06-16 | Moresco Corporation | Lubricant and magnetic disk |
| WO2011136379A1 (en) * | 2010-04-26 | 2011-11-03 | 株式会社Moresco | Cyclophosphazene compound, lubricant comprising same, and magnetic disk |
| JP5034027B2 (en) * | 2005-10-03 | 2012-09-26 | 株式会社Ｍｏｒｅｓｃｏ | Perfluoropolyether compound, lubricant using the same, and magnetic disk |
| US9384771B2 (en) | 2013-12-20 | 2016-07-05 | HGST Netherlands B.V. | Lubricants providing magnetic head wear reduction and magnetic spacing improvement |
-
1999
- 1999-12-27 JP JP37160199A patent/JP4326097B2/en not_active Expired - Lifetime
Cited By (24)
| 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 |
| SG130014A1 (en) * | 2002-09-03 | 2007-03-20 | Hoya Corp | Magnetic recording disk and process for manufacturing thereof |
| US7277254B2 (en) | 2002-09-03 | 2007-10-02 | Hoya Corporation | Magnetic recording disk and process for manufacture thereof |
| JP4570622B2 (en) * | 2004-07-23 | 2010-10-27 | 株式会社Ｍｏｒｅｓｃｏ | Lubricant for recording medium and magnetic disk |
| JPWO2006009057A1 (en) * | 2004-07-23 | 2008-05-01 | 株式会社松村石油研究所 | Lubricant for recording medium and magnetic disk |
| US7670695B2 (en) | 2004-07-23 | 2010-03-02 | Moresco Corporation | Lubricant for recording medium and magnetic disk |
| WO2006009057A1 (en) * | 2004-07-23 | 2006-01-26 | Matsumura Oil Research Corp. | Lubricant for recording medium and magnetic disk |
| JP5034027B2 (en) * | 2005-10-03 | 2012-09-26 | 株式会社Ｍｏｒｅｓｃｏ | Perfluoropolyether compound, lubricant using the same, and magnetic disk |
| JP4654339B2 (en) * | 2006-01-23 | 2011-03-16 | ダブリュディ・メディア・シンガポール・プライベートリミテッド | Magnetic disk |
| WO2007083792A1 (en) * | 2006-01-23 | 2007-07-26 | Hoya Corporation | Magnetic disk |
| JP2007193924A (en) * | 2006-01-23 | 2007-08-02 | Hoya Corp | Magnetic disk |
| US7833641B2 (en) | 2006-01-23 | 2010-11-16 | Wd Media (Singapore) Pte. Ltd. | Magnetic disk |
| WO2007105437A1 (en) * | 2006-02-28 | 2007-09-20 | Matsumura Oil Research Corp. | Lubricating agent for recording medium and magnetic disk |
| JP2008008681A (en) * | 2006-06-27 | 2008-01-17 | Fuji Electric Device Technology Co Ltd | Film thickness measuring method for lubrication layer of magnetic recording medium and magnetic recording medium |
| WO2008140121A1 (en) * | 2007-05-15 | 2008-11-20 | Matsumura Oil Research Corp. | Perfluoropolyether compound, and lubricant and magnetic disk each using the same |
| JP5358837B2 (en) * | 2007-05-15 | 2013-12-04 | 株式会社Ｍｏｒｅｓｃｏ | Perfluoropolyether compound, lubricant using the same, and magnetic disk |
| JP2010006810A (en) * | 2008-06-23 | 2010-01-14 | Seagate Technology Llc | Lubricant compound and magnetic data storage device |
| US8586703B2 (en) | 2008-06-23 | 2013-11-19 | Seagate Technology Llc | Low profile lubricant with cyclophosphazene ring attached |
| US20110143165A1 (en) * | 2008-09-05 | 2011-06-16 | Moresco Corporation | Lubricant and magnetic disk |
| US8679656B2 (en) * | 2008-09-05 | 2014-03-25 | Moresco Corporation | Lubricant and magnetic disk |
| JP5544520B2 (en) * | 2008-09-05 | 2014-07-09 | 株式会社Ｍｏｒｅｓｃｏ | Lubricant and magnetic disk |
| WO2011136379A1 (en) * | 2010-04-26 | 2011-11-03 | 株式会社Moresco | Cyclophosphazene compound, lubricant comprising same, and magnetic disk |
| US8936859B2 (en) | 2010-04-26 | 2015-01-20 | Moresco Corporation | Cyclophosphazene compound, lubricant comprising same, and magnetic disk |
| US9384771B2 (en) | 2013-12-20 | 2016-07-05 | HGST Netherlands B.V. | Lubricants providing magnetic head wear reduction and magnetic spacing improvement |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4326097B2 (en) | 2009-09-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5743438B2 (en) | Lubricant for magnetic disk, magnetic disk and manufacturing method thereof | |
| JP5134413B2 (en) | Magnetic disk and manufacturing method thereof | |
| WO2010038773A1 (en) | Magnetic disk and method for manufacturing the magnetic disk | |
| WO2009123043A1 (en) | Magnetic disk and process for producing the magnetic disk | |
| US20100239887A1 (en) | Lubricant and magnetic disk | |
| JPH0883423A (en) | Magnetic disk | |
| US6730403B1 (en) | Magnetic recording medium and method for manufacturing the same | |
| JP4099860B2 (en) | Liquid lubricant, magnetic recording medium using the same, and manufacturing method thereof | |
| US7510999B2 (en) | Lubricant composition for magnetic recording media | |
| JP2000260017A (en) | Magnetic recording medium and production of magnetic recording medium | |
| JPH09282642A (en) | Magnetic recording medium | |
| JP4297461B2 (en) | Magnetic recording medium and method for manufacturing the same | |
| JP3223238B2 (en) | Magnetic recording media | |
| WO2009123037A1 (en) | Magnetic disc and method for manufacturing the same | |
| JP4042086B2 (en) | Magnetic recording medium and method of manufacturing the magnetic recording medium | |
| JP2956674B2 (en) | Lubricant for magnetic recording medium, magnetic recording medium and magnetic recording device | |
| JPH09305961A (en) | Magnetic recording medium and its manufacture | |
| JP2560183B2 (en) | Lubricant and magnetic recording medium using the same | |
| JP2893240B2 (en) | Magnetic recording media | |
| JP2897156B2 (en) | Magnetic recording media | |
| JP3888625B2 (en) | Magnetic disk and manufacturing method thereof | |
| JP2967746B2 (en) | Lubricant for magnetic recording medium and magnetic recording medium using the same | |
| JP2004352999A (en) | Lubricant containing phosphazene compound | |
| JP5484764B2 (en) | Lubricant compound for magnetic disk and magnetic disk | |
| JP2001184622A (en) | Magnetic recording medium, its producing method and magnetic recording device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A625 | Written request for application examination (by other person) |
Free format text: JAPANESE INTERMEDIATE CODE: A625 Effective date: 20031209 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20031225 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A821 Effective date: 20040210 |
|
| RD02 | Notification of acceptance of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7422 Effective date: 20040210 |
|
| RD04 | Notification of resignation of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7424 Effective date: 20040213 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20050428 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20050520 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20050719 |
|
| A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 20060929 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20061127 |
|
| A911 | Transfer to examiner for re-examination before appeal (zenchi) |
Free format text: JAPANESE INTERMEDIATE CODE: A911 Effective date: 20061212 |
|
| A912 | Re-examination (zenchi) completed and case transferred to appeal board |
Free format text: JAPANESE INTERMEDIATE CODE: A912 Effective date: 20070112 |
|
| RD02 | Notification of acceptance of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7422 Effective date: 20081216 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20090609 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120619 Year of fee payment: 3 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 4326097 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120619 Year of fee payment: 3 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120619 Year of fee payment: 3 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130619 Year of fee payment: 4 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| EXPY | Cancellation because of completion of term |