JPH02284966A - Production of magnetic coating - Google Patents

Production of magnetic coating

Info

Publication number
JPH02284966A
JPH02284966A JP10592089A JP10592089A JPH02284966A JP H02284966 A JPH02284966 A JP H02284966A JP 10592089 A JP10592089 A JP 10592089A JP 10592089 A JP10592089 A JP 10592089A JP H02284966 A JPH02284966 A JP H02284966A
Authority
JP
Japan
Prior art keywords
magnetic
resin
magnetic powder
kneading
surface area
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP10592089A
Other languages
Japanese (ja)
Inventor
Hidekazu Takasago
高砂 英一
Yoshiki Kato
加藤 義喜
Masaaki Imamura
今村 昌明
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.)
Hitachi Ltd
Original Assignee
Hitachi Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hitachi Ltd filed Critical Hitachi Ltd
Priority to JP10592089A priority Critical patent/JPH02284966A/en
Publication of JPH02284966A publication Critical patent/JPH02284966A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To obtain a magnetic coating capable of providing an uniform coating film having excellent characteristics to a magnetic recording medium by dispersing pulverized magnetic powder having large specific surface area into a resin at a specific ratio. CONSTITUTION:For example, (B) an epoxy resin is blended with (A) magnetic powder having >=38m<2>/g BET value (specific surface area) at a resin amount of >=0.004g based on 1m<2> total surface area of the component A and the blend is subjected to first kneading using a kneader, etc., in 10-400kg/cm<2> shearing stress. Then (C) as necessary a resin and (D) solvent are added thereto and the blend is subjected to second kneading in shearing stress smaller than the above-mentioned shearing stress to provide the aimed magnetic coating.

Description

【発明の詳細な説明】[Detailed description of the invention]

【産業上の利用分野1 本発明は、記憶装置等に用いる磁気記録媒体の塗膜を形
成するための磁性塗料を製造する方法に関する。 【従来の技術】 従来、磁気記録媒体の塗膜を形成するための磁性塗料は
、特開昭56−44712号公報及び特公昭57−44
712号公報に記載のように、磁性粉と高分子結合剤で
ある樹脂とを混合し、大きなすり応力で混練りし、さら
にこの混合物に高分子結合剤である樹脂と溶媒とを加え
て混練りを続けて製造していた。上記の第1の混練りは
、大きなすり応力を与えるため、例えばニーダ−等を用
いて行なう、この工程で磁性粉は十分に分散される。さ
らに、塗膜としたときに優れた特性を示す組成とするた
め、混合物に高分子結合剤と溶媒とを加えて混練りする
。この第2の混練りは、第1の混練りの場合のように大
きなずり応力を与える必要、がないので、例えばボール
ミルにより行なう。
INDUSTRIAL APPLICATION FIELD 1 The present invention relates to a method for producing a magnetic coating material for forming a coating film on a magnetic recording medium used in a storage device or the like. [Prior Art] Conventionally, magnetic paints for forming coating films on magnetic recording media have been disclosed in Japanese Patent Application Laid-Open No. 56-44712 and Japanese Patent Publication No. 57-44.
As described in Japanese Patent Application No. 712, magnetic powder and a resin as a polymeric binder are mixed and kneaded with a large abrasion stress, and then a resin as a polymeric binder and a solvent are added to this mixture and mixed. They continued to knead and manufacture it. The above-mentioned first kneading is performed using, for example, a kneader in order to apply a large abrasion stress, and the magnetic powder is sufficiently dispersed in this step. Furthermore, in order to obtain a composition that exhibits excellent properties when formed into a coating film, a polymeric binder and a solvent are added to the mixture and kneaded. This second kneading is carried out using, for example, a ball mill, since there is no need to apply a large shear stress as in the case of the first kneading.

【発明が解決しようとする課題】[Problem to be solved by the invention]

上記従来技術は、微細化された。比表面積(BET値)
が大きな磁性粉を用いた磁性塗料とすることについては
十分考慮されておらず、このような磁性粉を用いたとき
、1先られた磁気記録媒体の塗膜の特性が十分でないと
いう問題があった。 本発明の目的は、微細化された、比表面積が大きな磁性
粉を用いて磁性塗料を製造する方法を提供することにあ
る。
The above conventional technology has been miniaturized. Specific surface area (BET value)
Not enough consideration has been given to the use of magnetic paints that use magnetic powders with large magnetic particles, and when such magnetic powders are used, there is a problem in that the coating film properties of magnetic recording media are not sufficient. Ta. An object of the present invention is to provide a method for producing a magnetic paint using finely divided magnetic powder having a large specific surface area.

【課題を解決するための手段l 上記目的は、少なくとも磁性粉と樹脂とを大きなずり応
力で第1の混練りを行ない混練り物とし、さらに該混練
り物に上記樹脂と同じ又は異なる樹脂の少なくとも一種
と溶剤とを加えて上記すり応力より小さいずり応力で第
2の混練りを行ない磁性塗料とする磁性塗料の製造方法
において、上記磁性粉は、BET値が38m2/g以上
の比表面積を有する磁性粉であり、上記磁性粉のBET
値で表した表面積の合計の1m”当りに対する上記樹脂
の重量をQ、004g以上として上記第1の混練りを行
なうことを特徴とする磁性塗料の製造方法により達成さ
れる。 本発明において磁性塗料は種種の組成のものを用いるこ
とができるが、好ましい組成の一例を次ぎに示す。 磁性粉            100重量部PVB等
のビニル樹脂  1.5〜30重量部エポキシ樹脂  
     10〜70重量部フェノール樹脂     
 10〜70重量部溶媒         300〜8
00重量部必要ならばこの組成物にさらにアルミナ等の
充填剤の0.1〜15重量部やポリウレタン等の他の樹
脂の2〜30重量部を加えた組成物も適用できる。 上記第1の混練りにおいては、大きなずり応力で混練り
を行なうために、例えばニーダ−等で混練りすることが
好ましい。大きなすり応力とは10〜400kg/cm
”の範囲が好ましく。 20〜300kg/am”の範囲がより好ましい。 すり応力が300kg/cm”を越えた状態で長時間混
練りすると樹脂が機械的作用によって劣化する傾向がや
やあり、400kg/cm2を越えるとその傾向がやや
大きくなるためである。 上記の組成の磁性塗料を製造fるときは、第1の混練り
において磁性粉とエポキシ樹脂と冷媒とを混練りするこ
とが好ましい。この場合、磁性粉100重量部にエポキ
シ樹脂10〜40重量部を加えることが好ましい、さら
に、エンキシ樹脂を20.5重量部以上とすることが特
に好ましい。 最終の磁性塗料の組成として、より多くのエポキシ樹脂
を必要とするときは、第2の混練りにおいて不足の分の
エポキシ樹脂を加えればよい。溶媒の量は上記の範囲の
すり応力にするために適宜定めればよいが例えば10〜
60重量部程重量すればよい、すり応力は混合物の粘度
の外に、ニーダ−のブレードの回転数やブレードと容器
の間隔等の種種の要因で決まるので、上記の範囲のすり
応力にするための好ましい溶媒の量は、上記範囲から大
きく変わる一場合もある。 充填剤を必要とするときは、第1の混練りにおいて充填
剤を加えて混練りしてもよく、別に分散処理をして第2
の混練りにおいて加えてもよく、どのような方法でもよ
い。 本発明において、大きな比表面積を有する磁性粉として
BET値が約38m2/g以上の比表面積を有する磁性
粉を用いることが好ましい。また、第1の混練りを行な
うときの樹脂の量は、磁性粉の73ET値で表した表面
積の合計の1m2当りに対する上記樹脂の重量を0.0
04g以上が好ましい、磁性粉のBET値で表した表面
積の合計とは、BET値と磁性粉の量(g数)を掛けた
値である。 上記の磁性塗料を用いて磁気記録媒体を製造する方法は
、磁性塗料を基板に塗布し、磁場配向し、加熱硬化して
行なう。塗膜は磁場配向することが好ましいが、磁場配
向しなくてもよい。 【作用】 磁性粉は、高分子結合剤である樹脂を吸着し、磁性塗料
として分散状態を保っている。磁性粉と樹脂の量の比が
一定であるならば、比表面積が大きい磁性粉を用いたと
きは、磁性粉に吸着される樹脂の量が単位表面積当りで
は減少することになる。すると磁性粉の磁気的引力を妨
げていた吸着樹脂による反発力が減少し、磁性粉の凝集
が生じ、このような状態の塗料を用いて形成した塗膜の
特性は低下する。 ところが、磁性粉の分散の最初の工祝で用いる樹脂の量
を磁性粉の比表面積が増すと共に増加し、磁性粉表面で
の吸着樹脂の量を単位面積当りほぼ一定に保つことによ
り、磁性粉の凝集を防止し、磁性粉が均一に分散した塗
料を得ることができる。 このような塗料を用いて製造した塗膜は特性が優れる。 [実施例) 以下に実施例を示す。 実施例1 エポキシ樹脂0.66kg、磁性粉(BET値38m”
/g)3.0kg、単結晶アルミナ0.27kgをニー
ダ−混線機に投入し、約15分間部合を行なう。次ぎに
シクロヘキサノンを2.2kg徐々に添加し、ニーダ−
混練りを約50kg/cm2のずり応力を加えて4時間
行なう。この間ニーダー混練りの状件は同じでも、混合
物の粘度が変化してすり応力は100kg/am2以上
になるが最後には約100 k g / c mとなる
。この混線物の約90%を秤量してボールミルポットに
とり、シクロヘキサノンを添加し、7日間ボールミル混
練りを行なう。次ぎに、全組成物が表1の重量比になる
ように、混合物にエポキシ樹脂の残りの量とフェノール
樹脂とポリビニルブチラール(表においてPVBと略す
)とさらにシクロヘキサノン、イソホロンの混合溶剤を
加えボールミル混練りを行ない、磁性塗料を得た。 表1 磁性粉       55   重量部単結晶アルミナ
    5   重量部エポキシ樹脂    17.6
 重量部フェノール樹脂   17.6 重量部PVB
         4.8  重量部次ぎにこの塗料を
、予め表面を清浄にしたアルミニウム円板に回転塗布し
1周知の方法で磁場配向し、220℃で硬化して磁気デ
ィスクを得た。 この磁気ディスクの塗膜の膜厚は0.9μIn、面粗さ
はRa=0.04であった。 この磁気ディスクをさらに研磨し、潤滑剤であるパーフ
ロロアルキルポリエーテルを塗布した。 この磁気ディスクの電気特性は、従来のものと比較しノ
イズが減少しS / N比が向上した。 実施例2,3 BET値の異なる磁性粉を用いて磁気ディスクを製造し
た。この場合、ニーダ−混練りのときのエポキシ樹脂の
量を表2に示すように変え、エポキシ樹脂の量を増した
ときは、後のボールミル混練りにおけるエポキシ樹脂の
量を減らして最後の組成が表1の組成になるように調整
し、他は実施例1と同様にした。表2には、実施例1の
組成も共に示す。また1表3に比較例として製造した磁
性塗料のニーダ−混練りのときの組成を示す。比較例の
場合も最後の組成比は実施例1と同じになるように調整
し、他は同様の方法出製造した。製造した磁気ディスク
の塗膜の面粗さを、実施例1、表2 実施例      N。 磁性粉BET値 (+n2/g) 磁性粉     (kg) エポキシ樹脂  (kg) 比 (樹脂/磁性粉) 単位表面積当り樹脂量(g) 3.0 0.66 0.22 o、oosg 3、O o、72 0.24 0.0055 3.0 0.76 0.25 0.0053 表3 比較例  No        I   H■磁性粉B
ET値 (m”/g)   28  38  48磁性
粉     (kg)   3.0 3.0 3.0エ
ポキシ樹脂  (kg)   0,36 0.36 0
.36比 (樹脂/磁性粉)    0.12.0.1
2 0.12表及び図に見られるように、比表面積の小
さい磁性粉を用いたときは、比較例で製造した磁気ディ
スクの塗膜の面粗さも良好であるが、比表面積の大きい
磁性粉を用いたときは、その面粗さは劣化する。一方、
本実施例の場合、比表面積の太きい磁性粉を用いても得
られた塗膜の面粗さは良好である。 さらに本発明においては面粗さの良好な薄い塗膜、例え
ば膜厚089μm以下の塗膜を形成することもできる。 比較例の場合、約1μm以上の膜厚でないと均一な塗膜
は得られなかった。 【発明の効果1 本発明によれば、比表面積の大きい磁性粉を用い、磁性
粉を分散する工程における樹脂の量を調節して磁性塗料
を製造することにより、この磁性塗料から均一な特性の
優れた塗膜を有する磁気記録媒体を得ることができた。
[Means for Solving the Problems] The above object is to first knead at least a magnetic powder and a resin with a large shear stress to form a kneaded product, and further add at least one kind of resin that is the same as or different from the above resin to the kneaded product. In the method for producing a magnetic paint, the magnetic paint is prepared by adding a solvent and a second kneading at a shear stress smaller than the above-mentioned shear stress, wherein the above-mentioned magnetic powder is a magnetic powder having a specific surface area with a BET value of 38 m2/g or more. BET of the above magnetic powder
This is achieved by a method for producing a magnetic paint, characterized in that the first kneading is carried out with the weight of the resin per 1 m'' of the total surface area expressed as Q, 004 g or more. Although various compositions can be used, examples of preferable compositions are shown below: Magnetic powder 100 parts by weight Vinyl resin such as PVB 1.5 to 30 parts by weight Epoxy resin
10-70 parts by weight phenolic resin
10-70 parts by weight Solvent 300-8
If necessary, a composition in which 0.1 to 15 parts by weight of a filler such as alumina or 2 to 30 parts by weight of another resin such as polyurethane is added to this composition can also be applied. In the first kneading, kneading is preferably carried out using, for example, a kneader in order to perform kneading with a large shear stress. Large abrasion stress is 10 to 400 kg/cm
A range of "20 to 300 kg/am" is more preferable. This is because there is a slight tendency for the resin to deteriorate due to mechanical action if kneaded for a long time with the abrasion stress exceeding 300 kg/cm2, and this tendency increases somewhat when the abrasion stress exceeds 400 kg/cm2. When manufacturing magnetic paint, it is preferable to knead magnetic powder, epoxy resin, and refrigerant in the first kneading step.In this case, 10 to 40 parts by weight of epoxy resin should be added to 100 parts by weight of magnetic powder. It is preferable that the amount of epoxy resin is 20.5 parts by weight or more, and it is particularly preferable that the amount of epoxy resin is 20.5 parts by weight or more.If more epoxy resin is required in the composition of the final magnetic coating, the insufficient amount is added in the second kneading process. of epoxy resin may be added.The amount of solvent may be determined as appropriate to achieve the abrasion stress within the above range.
It is sufficient to add about 60 parts by weight. Since the abrasive stress is determined by various factors such as the rotation speed of the kneader blade and the distance between the blade and the container in addition to the viscosity of the mixture, in order to achieve the abrasive stress within the above range, The preferred amount of solvent may vary widely from the above ranges. If a filler is required, the filler may be added and kneaded during the first kneading process, or a separate dispersion treatment may be performed to perform the second kneading process.
It may be added during kneading, and any method may be used. In the present invention, it is preferable to use a magnetic powder having a specific surface area with a BET value of about 38 m2/g or more as the magnetic powder having a large specific surface area. In addition, the amount of resin when performing the first kneading is such that the weight of the resin is 0.0 per m2 of the total surface area expressed by the 73ET value of the magnetic powder.
The total surface area expressed by the BET value of the magnetic powder, which is preferably 0.4 g or more, is the value obtained by multiplying the BET value by the amount (g number) of the magnetic powder. A method for manufacturing a magnetic recording medium using the above-described magnetic paint is to apply the magnetic paint to a substrate, orient it in a magnetic field, and harden it by heating. Although the coating film is preferably oriented in a magnetic field, it does not have to be oriented in a magnetic field. [Operation] Magnetic powder adsorbs resin, which is a polymeric binder, and maintains a dispersed state as a magnetic paint. If the ratio of the amounts of magnetic powder and resin is constant, when magnetic powder with a large specific surface area is used, the amount of resin adsorbed to the magnetic powder will decrease per unit surface area. As a result, the repulsive force caused by the adsorbing resin that had been blocking the magnetic attraction of the magnetic powder decreases, causing agglomeration of the magnetic powder, and the properties of the coating film formed using the paint in such a state deteriorate. However, by increasing the amount of resin used in the initial process of dispersing magnetic powder as the specific surface area of the magnetic powder increases, and by keeping the amount of adsorbed resin on the surface of the magnetic powder almost constant per unit area, It is possible to prevent the agglomeration of particles and obtain a paint in which magnetic powder is uniformly dispersed. Coating films produced using such paints have excellent properties. [Example] Examples are shown below. Example 1 Epoxy resin 0.66 kg, magnetic powder (BET value 38 m"
/g) and 0.27 kg of single-crystal alumina were put into a kneader mixer, and the mixing was carried out for about 15 minutes. Next, 2.2 kg of cyclohexanone was gradually added to the kneader.
Kneading is carried out for 4 hours while applying a shear stress of about 50 kg/cm2. During this time, even if the kneading conditions remain the same, the viscosity of the mixture changes and the abrasion stress increases to 100 kg/am2 or more, but eventually reaches about 100 kg/cm2. Approximately 90% of this mixed material was weighed and placed in a ball mill pot, cyclohexanone was added, and ball mill kneading was carried out for 7 days. Next, the remaining amount of epoxy resin, phenol resin, polyvinyl butyral (abbreviated as PVB in the table), and a mixed solvent of cyclohexanone and isophorone were added to the mixture and mixed in a ball mill so that the weight ratio of the entire composition was as shown in Table 1. A magnetic paint was obtained by kneading. Table 1 Magnetic powder 55 parts by weight Single crystal alumina 5 parts by weight Epoxy resin 17.6
Part by weight Phenol resin 17.6 Part by weight PVB
4.8 parts by weight Next, this paint was spin-coated onto an aluminum disk whose surface had been cleaned in advance, oriented in a magnetic field by a well-known method, and cured at 220° C. to obtain a magnetic disk. The film thickness of the coating film of this magnetic disk was 0.9 μIn, and the surface roughness was Ra=0.04. This magnetic disk was further polished and coated with perfluoroalkyl polyether as a lubricant. The electrical characteristics of this magnetic disk include reduced noise and improved S/N ratio compared to conventional magnetic disks. Examples 2 and 3 Magnetic disks were manufactured using magnetic powders having different BET values. In this case, change the amount of epoxy resin during kneader kneading as shown in Table 2. If the amount of epoxy resin is increased, the amount of epoxy resin in the subsequent ball mill kneading is reduced to maintain the final composition. The composition was adjusted to have the composition shown in Table 1, and the rest was the same as in Example 1. Table 2 also shows the composition of Example 1. Further, Table 1 shows the composition of the magnetic paint produced as a comparative example when kneaded in a kneader. In the case of the comparative example as well, the final composition ratio was adjusted to be the same as in Example 1, and the other components were manufactured using the same method. The surface roughness of the coating film of the manufactured magnetic disk is shown in Example 1 and Table 2. Magnetic powder BET value (+n2/g) Magnetic powder (kg) Epoxy resin (kg) Ratio (resin/magnetic powder) Amount of resin per unit surface area (g) 3.0 0.66 0.22 o, oosg 3, O o , 72 0.24 0.0055 3.0 0.76 0.25 0.0053 Table 3 Comparative example No I H■Magnetic powder B
ET value (m”/g) 28 38 48 Magnetic powder (kg) 3.0 3.0 3.0 Epoxy resin (kg) 0,36 0.36 0
.. 36 ratio (resin/magnetic powder) 0.12.0.1
2 As seen in Table 0.12 and the figure, when magnetic powder with a small specific surface area was used, the surface roughness of the coating film of the magnetic disk manufactured in the comparative example was also good, but when magnetic powder with a large specific surface area was used, the surface roughness of the coating film was good. When using , the surface roughness deteriorates. on the other hand,
In the case of this example, the surface roughness of the coating film obtained was good even when magnetic powder with a large specific surface area was used. Furthermore, in the present invention, it is also possible to form a thin coating film with good surface roughness, for example, a coating film with a thickness of 089 μm or less. In the case of the comparative example, a uniform coating film could not be obtained unless the film thickness was approximately 1 μm or more. Effect of the invention 1 According to the present invention, by manufacturing a magnetic paint by using magnetic powder with a large specific surface area and adjusting the amount of resin in the process of dispersing the magnetic powder, uniform characteristics can be obtained from this magnetic paint. A magnetic recording medium with an excellent coating film could be obtained.

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

第1図は、本発明を説明するための磁気ディスクの塗膜
の面粗さを示す図である。
FIG. 1 is a diagram showing the surface roughness of a coating film of a magnetic disk for explaining the present invention.

Claims (1)

【特許請求の範囲】[Claims] 1、少なくとも磁性粉と樹脂とを大きなずり応力で第1
の混練りを行ない混練り物とし、さらに該混練り物に上
記樹脂と同じ又は異なる樹脂の少なくとも一種と溶剤と
を加えて上記ずり応力より小さいずり応力で第2の混練
りを行ない磁性塗料とする磁性塗料の製造方法において
、上記磁性粉は、BET値が38m^2/g以上の比表
面積を有する磁性粉であり、上記磁性粉のBET値で表
した表面積の合計の1m^2当りに対する上記樹脂の重
量を0.004g以上として上記第1の混練りを行なう
ことを特徴とする磁性塗料の製造方法。
1. At least the magnetic powder and resin are first
A magnetic paint is obtained by kneading the mixture to obtain a kneaded product, and then adding at least one type of resin that is the same as or different from the above resin and a solvent to the kneaded product and performing a second kneading at a shear stress smaller than the above-mentioned shear stress to obtain a magnetic paint. In the method for producing a coating material, the magnetic powder is a magnetic powder having a specific surface area with a BET value of 38 m^2/g or more, and the above resin per 1 m^2 of the total surface area expressed by the BET value of the magnetic powder. A method for producing a magnetic paint, characterized in that the first kneading is performed with a weight of 0.004 g or more.
JP10592089A 1989-04-27 1989-04-27 Production of magnetic coating Pending JPH02284966A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10592089A JPH02284966A (en) 1989-04-27 1989-04-27 Production of magnetic coating

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10592089A JPH02284966A (en) 1989-04-27 1989-04-27 Production of magnetic coating

Publications (1)

Publication Number Publication Date
JPH02284966A true JPH02284966A (en) 1990-11-22

Family

ID=14420302

Family Applications (1)

Application Number Title Priority Date Filing Date
JP10592089A Pending JPH02284966A (en) 1989-04-27 1989-04-27 Production of magnetic coating

Country Status (1)

Country Link
JP (1) JPH02284966A (en)

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