JPS62159338A - magnetic disk - Google Patents
magnetic diskInfo
- Publication number
- JPS62159338A JPS62159338A JP61000852A JP85286A JPS62159338A JP S62159338 A JPS62159338 A JP S62159338A JP 61000852 A JP61000852 A JP 61000852A JP 85286 A JP85286 A JP 85286A JP S62159338 A JPS62159338 A JP S62159338A
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- JP
- Japan
- Prior art keywords
- layer
- magnetic
- powder
- substrate
- average particle
- 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.)
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Links
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- Paints Or Removers (AREA)
- Magnetic Record Carriers (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は磁性層の厚さが5μm以下の高密度記録に適
した磁気記録媒体に関し、さらに詳しくは耐久性に優れ
た前記の磁気記録媒体に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a magnetic recording medium suitable for high-density recording in which the thickness of the magnetic layer is 5 μm or less, and more specifically to the above-mentioned magnetic recording medium with excellent durability. Regarding.
磁気記録媒体の磁性層は、通常、磁性粉末、結合剤成分
、有機溶剤およびその他の必要成分からなる磁性塗料を
ポリエステルフィルムなどの基体上に塗布、乾燥してつ
くられ、このようにしてつくられる磁性層の基体に対す
る接着性を改善し、また表面電気抵抗を低減するため、
ポリエステル樹脂を主体とした下塗り層を磁性層と基体
との間に形成したり、またカーボンブランクなどの導電
性粉末を均一に分散させた下塗り層を設けることが行わ
れている。(特開昭55−84040号)〔発明が解決
しようとする問題点〕
ところが、磁気記録の高密度記録化に対応して、磁性層
の厚さを可及的に薄(すると、減磁損失が少なくなって
記録密度が高密度化される反面、磁性層中に含有される
充愼剤などがしだいに少なくなり、磁性層の機械的強度
が低下して充分な耐久性が得られなくなる。特に10℃
以下の低温の場合は、磁性層にかかる磁気ヘッドの摺動
応力の影響が大きく、磁性層が短時間で破壊されること
があり、耐久性が大きく低下する。The magnetic layer of a magnetic recording medium is usually made by applying a magnetic paint consisting of magnetic powder, a binder component, an organic solvent, and other necessary components onto a substrate such as a polyester film and drying it. In order to improve the adhesion of the magnetic layer to the substrate and reduce the surface electrical resistance,
An undercoat layer mainly made of polyester resin is formed between the magnetic layer and the substrate, or an undercoat layer is provided in which conductive powder such as carbon blank is uniformly dispersed. (Unexamined Japanese Patent Publication No. 55-84040) [Problems to be Solved by the Invention] However, in response to the increasing density of magnetic recording, the thickness of the magnetic layer is reduced as much as possible (which reduces demagnetization loss). On the other hand, the amount of filler contained in the magnetic layer gradually decreases, and the mechanical strength of the magnetic layer decreases, making it impossible to obtain sufficient durability. Especially 10℃
In the case of a low temperature below, the influence of the sliding stress of the magnetic head on the magnetic layer is large, and the magnetic layer may be destroyed in a short period of time, resulting in a significant decrease in durability.
この発明は、かかる現状に鑑み種々検討を行った結果な
されたもので、基体と、この基体上に形成する厚さが5
μm以下の磁性層との間に、平均粒子径が0.1〜3μ
mの非磁性粉末を含む下塗り層を設けることによって、
厚さが極めて薄い磁性層の耐久性を充分に向上させ、高
密度記録が良好に行えるようにしたものである。This invention was made as a result of various studies in view of the current situation, and includes a base body and a thickness of 5.5 mm formed on the base body.
The average particle diameter is 0.1 to 3 μm between the magnetic layer and the magnetic layer of μm or less.
By providing an undercoat layer containing m non-magnetic powder,
The durability of the magnetic layer, which is extremely thin, has been sufficiently improved to enable high-density recording to be performed satisfactorily.
この発明において、基体上に下塗り層を介して形成され
る磁性層は、高密度記録が良好に行えるようにするため
5μm以下にするのが好ましく、これより厚くすると減
磁損失が大きくなって高密度記録が良好に行えない。In this invention, the magnetic layer formed on the substrate via the undercoat layer is preferably 5 μm or less in order to enable good high-density recording; if it is thicker than this, demagnetization loss increases and Density recording cannot be performed well.
また、この発明において、基体と磁性層との間に設ける
下塗り層は、平均粒子径が0.1〜3μmの非磁性粉末
を含有させ、層厚をこれらの非磁性粉末を充分に含有で
きる0、1〜3μmの厚さにするのが好ましく、このよ
うに平均粒子径が0.1〜3μmの非磁性粉末を含有さ
せた層厚が001〜3μmの下塗り層を、磁性層と基体
との間に設けると、下塗り層に含有させた非磁性粉末に
よって磁気ヘッドの摺動により生じる内部応力を分散す
ることができて、磁性層の機械的強度を充分に補強する
ことができ、磁性層の厚みが可及的に薄い場合でも磁性
層を充分に補強して、耐久性を充分に向上することがで
きる。Further, in the present invention, the undercoat layer provided between the substrate and the magnetic layer contains non-magnetic powders having an average particle diameter of 0.1 to 3 μm, and the layer thickness is set to 0.00000000000000000000000000000, which is sufficient to contain these non-magnetic powders. The thickness of the undercoat layer is preferably 0.01 to 3 μm and contains nonmagnetic powder with an average particle size of 0.1 to 3 μm. When provided between the layers, the non-magnetic powder contained in the undercoat layer can disperse the internal stress caused by the sliding of the magnetic head, sufficiently reinforcing the mechanical strength of the magnetic layer, and increasing the strength of the magnetic layer. Even when the thickness is as thin as possible, the magnetic layer can be sufficiently reinforced and durability can be sufficiently improved.
このような下塗り層中に含有させる非磁性粉末としては
、平均粒子径が0.1〜3μmの酸化物粉末が好ましく
使用され、平均粒子径0.3〜1.0μmのものがより
好ましく使用される。このような非磁性粉末としては、
たとえば、A12o3粉末、αF e 203粉末、C
aCO3粉末、MgO粉末、Cr2O3粉末、BaSO
4粉末、BaCO3粉末、ZnO粉末、Cu2O粉末、
CuO粉末、Tio2粉末などが好適なものとして使用
される。使用量は、下塗り層の全固形成分に対して20
〜80重量%の範囲内で使用するのが好ましく、これよ
り少なずぎると所期の効果が得られず、多すぎると下塗
り層の表面粗さが大きくなり、磁性層のノイズ増加の原
因となる。As the non-magnetic powder contained in such an undercoat layer, an oxide powder with an average particle size of 0.1 to 3 μm is preferably used, and one with an average particle size of 0.3 to 1.0 μm is more preferably used. Ru. As such non-magnetic powder,
For example, A12o3 powder, αF e 203 powder, C
aCO3 powder, MgO powder, Cr2O3 powder, BaSO
4 powder, BaCO3 powder, ZnO powder, Cu2O powder,
CuO powder, Tio2 powder, etc. are preferably used. The amount used is 20% based on the total solid components of the undercoat layer.
It is preferable to use it within the range of ~80% by weight; if it is less than this, the desired effect will not be obtained, and if it is too much, the surface roughness of the undercoat layer will increase, causing increased noise in the magnetic layer. .
このような非磁性粉末を含む下塗り層は、通常、これら
の非磁性粉末を、結合剤樹脂および有機溶剤等とともに
混合分散して下塗り要用塗料を調製し、これをポリエス
テルフィルムなどの基体上に塗布し、乾燥して形成され
る。このようにして形成される下塗り層の層厚は、前記
の非磁性粉末を充分に含有することができるように、0
.1〜3μmの範囲内にするのが好ましい。An undercoat layer containing such non-magnetic powder is usually prepared by mixing and dispersing these non-magnetic powders with a binder resin, an organic solvent, etc. to prepare an undercoat paint, and applying this onto a substrate such as a polyester film. It is formed by applying and drying. The thickness of the undercoat layer formed in this way is set to 0.
.. Preferably, the thickness is within the range of 1 to 3 μm.
ここで、下塗り層に使用される結合剤樹脂としては、塩
化ビニル−酢酸ビニル系共重合体、ポリビニルブチラー
ル樹脂、繊維素系樹脂、ポリウレタン系樹脂、ポリエス
テル系樹脂、エポキシ系樹脂、ポリエーテル系樹脂、イ
ソシアネート化合物、放射線硬化型樹脂など従来から汎
用されている結合剤樹脂がいずれも好適に使用される。Here, the binder resin used for the undercoat layer includes vinyl chloride-vinyl acetate copolymer, polyvinyl butyral resin, cellulose resin, polyurethane resin, polyester resin, epoxy resin, and polyether resin. , isocyanate compounds, radiation-curable resins, and other binder resins that have been widely used in the past are all suitably used.
また、有機溶剤としては、アセトン、メチルイソブチル
ケトン、メチルエチルケトン、シクロヘキサノン、トル
エン、酢酸エチル、テトラヒドロフラン、ジメチルホル
ムアミドなど従来一般に使用される有機溶剤がいずれも
単独で、或いは二種以上混合して使用される。Further, as the organic solvent, conventionally commonly used organic solvents such as acetone, methyl isobutyl ketone, methyl ethyl ketone, cyclohexanone, toluene, ethyl acetate, tetrahydrofuran, and dimethyl formamide can be used alone or in a mixture of two or more kinds. .
下塗り層上の磁性層の形成は、γ−Fe203−粉末、
Fe3O4粉末、CO含有r−Fe203粉末、CO含
有Fe3O4粉末、Fe粉末、C。The magnetic layer on the undercoat layer is formed using γ-Fe203 powder,
Fe3O4 powder, CO-containing r-Fe203 powder, CO-containing Fe3O4 powder, Fe powder, C.
粉末、Fe−Ni粉末およびバリウムフェライト、スト
ロンチウムフェライトなどの従来公知の各種磁性粉末を
、結合剤樹脂および有機溶剤等とともに混合分散して磁
性塗料を調製し、この磁性塗料を、基体上に形成した下
塗り層上に塗布、乾燥するなどして形成される。A magnetic paint was prepared by mixing and dispersing various conventionally known magnetic powders such as powder, Fe-Ni powder, barium ferrite, and strontium ferrite together with a binder resin and an organic solvent, and this magnetic paint was formed on a substrate. It is formed by coating and drying on the undercoat layer.
この際、使用する結合剤樹脂および有機溶剤は、前記の
下塗り層を形成する場合に使用したものと同じものがい
ずれも好適に使用される。At this time, the binder resin and organic solvent used are preferably the same as those used in forming the undercoat layer.
なお、磁性塗料中には、通常使用されている各種添加剤
、たとえば、潤滑剤、分散剤、研暦剤、帯電防止剤など
を適宜に添加使用してもよい。In addition, various commonly used additives such as lubricants, dispersants, polishing agents, antistatic agents, etc. may be appropriately added to the magnetic paint.
次に、この発明の実施例について説明する。 Next, embodiments of the invention will be described.
実施例1
ポリエステル樹脂 100重量部Al2
O3粉末(粒子径0.7 100〃μm)
シクロへキサノン 400〃トルエン
400〃この組成物をボールミル
中で24時間混合分11にして下塗り要用塗料を調整し
、これらを厚さ75μmのポリエステルフィルムの両面
に、乾燥厚が3μmとなるように、塗布、乾燥し、カレ
ンダ処理して下塗り層を形成した。Example 1 Polyester resin 100 parts by weight Al2
O3 powder (particle size 0.7 to 100〃μm) Cyclohexanone 400〃Toluene
400〃This composition was mixed in a ball mill for 24 hours to prepare a paint required for undercoating, and this was applied to both sides of a 75 μm thick polyester film so that the dry thickness was 3 μm, and dried. An undercoat layer was formed by calendering.
次いで、このポリエステルフィルム両面の下塗り層上に
、下記組成の磁性塗料を乾燥厚が0.7μmとなるよう
に、塗布、乾燥し、50℃、10kg/ cnlでカレ
ンダ処理して磁性層を形成した。しかる後、円盤状に打
抜き加工処理して、第1図に示すように、ポリエステル
フィルム1の両面に、下塗り層2および磁性1ii3を
積層形成した磁気ディスクAをつくった。Next, on the undercoat layer on both sides of this polyester film, a magnetic paint having the following composition was applied to a dry thickness of 0.7 μm, dried, and calendered at 50° C. and 10 kg/cnl to form a magnetic layer. . Thereafter, it was punched into a disk shape to produce a magnetic disk A in which an undercoat layer 2 and a magnetic layer 1ii3 were laminated on both sides of a polyester film 1, as shown in FIG.
磁性塗料−
α−Fe磁性粉末 500重量部塩化ビニ
ル−酢酸ビニル−ビニ 50//ルアルコ一ル共重合
体)
ポリウレタン樹脂 30〃イソシアネ
一ト化合物 20〃オレイルオレート
15〃シクロへキサノン
650〃トルエン 650〃実施
例2
実施例1における下塗り雇用塗料の組成において、Al
2O3粉末に代えてCaCO3粉末(平均粒子径0.−
1μm)を同量使用した以外は、実施例1と同様にして
下塗り層を形成し、磁気ディスクAをつくった。Magnetic paint - α-Fe magnetic powder 500 parts by weight Vinyl chloride-vinyl acetate-vinyl 50//alcohol copolymer) Polyurethane resin 30 Isocyanate compound 20 Oley oleate
15〃Cyclohexanone
650〃Toluene 650〃Example 2 In the composition of the undercoat paint in Example 1, Al
CaCO3 powder (average particle size 0.-
A magnetic disk A was produced by forming an undercoat layer in the same manner as in Example 1, except that the same amount of 1 μm) was used.
実施例3
実施例1における下塗り雇用塗料の組成において、Al
2O,粉末に代えて(X−Fe203粉末(平均粒子径
0.3μm)を同量使用した以外は、実施例1と同様に
して下塗り層を形成し、磁気ディスクAをつくった。Example 3 In the composition of the undercoating paint in Example 1, Al
An undercoat layer was formed in the same manner as in Example 1, except that the same amount of (X-Fe203 powder (average particle size: 0.3 μm) was used instead of 2O2 powder, and magnetic disk A was prepared.
比較例1
実施例1における下塗り雇用塗料の組成において、平均
粒子径が0.7μmのAl2O3粉末に代えて平均粒子
径が0.07μmのAl2O3粉末を同量使用した以外
は〈実施例1と同様にして下塗り層を形成し、磁気ディ
スクをつくった。Comparative Example 1 Same as Example 1 except that in the composition of the undercoating paint in Example 1, the same amount of Al2O3 powder with an average particle size of 0.07 μm was used instead of the Al2O3 powder with an average particle size of 0.7 μm. Then, an undercoat layer was formed and a magnetic disk was manufactured.
比較例2
実施例1における下塗り雇用塗料の組成において、平均
粒子径が0.7μmのAl2O3粉末に代えて平均粒子
径が4.0μmのAl2O3粉末を同量使用した以外は
、実施例1と同様にして下塗り層を形成し、磁気ディス
クをつくった。Comparative Example 2 Same as Example 1 except that in the composition of the undercoating paint in Example 1, the same amount of Al2O3 powder with an average particle size of 4.0 μm was used instead of the Al2O3 powder with an average particle size of 0.7 μm. Then, an undercoat layer was formed and a magnetic disk was manufactured.
比較例3
実施例1における下塗り雇用塗料の組成において、Al
2O3粉末に代えて平均粒子径が0.2μmのカーボン
ブラックを同量使用した以外は、実施例1と同様にして
下塗り層を形成し、磁気ディスクをつくった。Comparative Example 3 In the composition of the undercoating paint in Example 1, Al
An undercoat layer was formed in the same manner as in Example 1, except that the same amount of carbon black having an average particle size of 0.2 μm was used in place of 2O3 powder, and a magnetic disk was produced.
比較例4
実施例1における下塗り雇用塗料の組成において、Al
2O3粉末を省いた以外は、実施例1と同様にして下塗
り層を形成し、磁気ディスクをつく った。Comparative Example 4 In the composition of the undercoating paint in Example 1, Al
An undercoat layer was formed in the same manner as in Example 1, except that the 2O3 powder was omitted, and a magnetic disk was produced.
各実施例および比較例で得られた磁気ディスクについて
、耐久性を調べた。耐久性は、磁気ディスクを磁気ディ
スク駆動装置に装着し、相対速度3m/sec、ヘッド
圧20gで、磁気ディスクに傷が発生するまでの時間を
測定して調べた。The durability of the magnetic disks obtained in each example and comparative example was examined. Durability was examined by mounting the magnetic disk in a magnetic disk drive and measuring the time until scratches appeared on the magnetic disk at a relative speed of 3 m/sec and a head pressure of 20 g.
下記第1表はその結果である。Table 1 below shows the results.
第1表−
〔発明の効果〕
上記第1表から明らかなように、この発明で得られた磁
気ディスク(実施例1ないし3)は、比較例1ないし4
で得られた磁気ディスクに比し、傷が発生するまでの時
間が長(、このことからこの発明によって得られる磁気
記録媒体は、耐久性が充分に向上されていることがわか
る。Table 1 - [Effects of the Invention] As is clear from the above Table 1, the magnetic disks (Examples 1 to 3) obtained by the present invention are the same as those of Comparative Examples 1 to 4.
Compared to the magnetic disk obtained by the present invention, it takes a longer time for scratches to occur (This shows that the magnetic recording medium obtained by the present invention has sufficiently improved durability.
第1図はこの発明で得られた磁気ディスクの部分拡大断
面図である。
1・・・ポリエステルフィルム(基体)、2・・・下塗
り層、3・・・磁性層、A・・・磁気ディスク(磁気記
録媒体)FIG. 1 is a partially enlarged sectional view of a magnetic disk obtained by the present invention. 1... Polyester film (substrate), 2... Undercoat layer, 3... Magnetic layer, A... Magnetic disk (magnetic recording medium)
Claims (1)
末を含む下塗り層を設け、この下塗り層上に厚さが5μ
m以下の磁性層を設けたことを特徴とする磁気記録媒体1. An undercoat layer containing non-magnetic powder with an average particle size of 0.1 to 3 μm is provided on the substrate, and a layer with a thickness of 5 μm is provided on this undercoat layer.
A magnetic recording medium characterized by having a magnetic layer having a thickness of m or less.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP61000852A JPH0816978B2 (en) | 1986-01-06 | 1986-01-06 | Magnetic disk |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP61000852A JPH0816978B2 (en) | 1986-01-06 | 1986-01-06 | Magnetic disk |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP7051697A Division JPH09231548A (en) | 1997-03-06 | 1997-03-06 | Magnetic disk |
JP7051797A Division JPH09231549A (en) | 1997-03-06 | 1997-03-06 | Magnetic disk |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS62159338A true JPS62159338A (en) | 1987-07-15 |
JPH0816978B2 JPH0816978B2 (en) | 1996-02-21 |
Family
ID=11485172
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP61000852A Expired - Lifetime JPH0816978B2 (en) | 1986-01-06 | 1986-01-06 | Magnetic disk |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0816978B2 (en) |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62222427A (en) * | 1986-03-25 | 1987-09-30 | Toshiba Corp | Magnetic recording medium |
JPH02260234A (en) * | 1989-03-31 | 1990-10-23 | Konica Corp | Magnetic recording medium |
JPH05182177A (en) * | 1992-01-08 | 1993-07-23 | Fuji Photo Film Co Ltd | Magnetic recording medium |
JPH05298653A (en) * | 1992-04-14 | 1993-11-12 | Fuji Photo Film Co Ltd | Magnetic recording medium |
JPH0850718A (en) * | 1995-07-27 | 1996-02-20 | Fuji Photo Film Co Ltd | Magnetic recording medium |
EP0769775A1 (en) | 1995-10-20 | 1997-04-23 | Toda Kogyo Corp. | Hematite particles for non-magnetic undercoat layer for magnetic recording medium, process for producing the same, non-magnetic undercoat layer and magnetic recording medium |
US5763046A (en) * | 1991-01-21 | 1998-06-09 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US5827600A (en) * | 1991-01-21 | 1998-10-27 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5613515A (en) * | 1979-07-16 | 1981-02-09 | Tdk Corp | Magnetic recording medium |
JPS5928226A (en) * | 1982-08-09 | 1984-02-14 | Victor Co Of Japan Ltd | Magnetic recording medium |
JPS59223935A (en) * | 1983-06-03 | 1984-12-15 | Tdk Corp | Magnetic recording medium |
-
1986
- 1986-01-06 JP JP61000852A patent/JPH0816978B2/en not_active Expired - Lifetime
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5613515A (en) * | 1979-07-16 | 1981-02-09 | Tdk Corp | Magnetic recording medium |
JPS5928226A (en) * | 1982-08-09 | 1984-02-14 | Victor Co Of Japan Ltd | Magnetic recording medium |
JPS59223935A (en) * | 1983-06-03 | 1984-12-15 | Tdk Corp | Magnetic recording medium |
Cited By (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62222427A (en) * | 1986-03-25 | 1987-09-30 | Toshiba Corp | Magnetic recording medium |
JPH02260234A (en) * | 1989-03-31 | 1990-10-23 | Konica Corp | Magnetic recording medium |
US5827600A (en) * | 1991-01-21 | 1998-10-27 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US6025082A (en) * | 1991-01-21 | 2000-02-15 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US6020022A (en) * | 1991-01-21 | 2000-02-01 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US6015602A (en) * | 1991-01-21 | 2000-01-18 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US5985408A (en) * | 1991-01-21 | 1999-11-16 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US5763046A (en) * | 1991-01-21 | 1998-06-09 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US5851622A (en) * | 1991-01-21 | 1998-12-22 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US5811172A (en) * | 1991-01-21 | 1998-09-22 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US5811166A (en) * | 1991-01-21 | 1998-09-22 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US5792543A (en) * | 1991-04-25 | 1998-08-11 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
US5780141A (en) * | 1991-04-25 | 1998-07-14 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
JPH05182177A (en) * | 1992-01-08 | 1993-07-23 | Fuji Photo Film Co Ltd | Magnetic recording medium |
JPH05298653A (en) * | 1992-04-14 | 1993-11-12 | Fuji Photo Film Co Ltd | Magnetic recording medium |
JPH0850718A (en) * | 1995-07-27 | 1996-02-20 | Fuji Photo Film Co Ltd | Magnetic recording medium |
EP0769775A1 (en) | 1995-10-20 | 1997-04-23 | Toda Kogyo Corp. | Hematite particles for non-magnetic undercoat layer for magnetic recording medium, process for producing the same, non-magnetic undercoat layer and magnetic recording medium |
Also Published As
Publication number | Publication date |
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JPH0816978B2 (en) | 1996-02-21 |
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EXPY | Cancellation because of completion of term |