JPS61182631A - Production of magnetic recording medium - Google Patents

Production of magnetic recording medium

Info

Publication number
JPS61182631A
JPS61182631A JP60022263A JP2226385A JPS61182631A JP S61182631 A JPS61182631 A JP S61182631A JP 60022263 A JP60022263 A JP 60022263A JP 2226385 A JP2226385 A JP 2226385A JP S61182631 A JPS61182631 A JP S61182631A
Authority
JP
Japan
Prior art keywords
magnetic
powder
paint
medium
ferromagnetic powder
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
JP60022263A
Other languages
Japanese (ja)
Inventor
Tomu Sato
佐藤 富
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.)
Panasonic Holdings Corp
Original Assignee
Matsushita Electric Industrial Co 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 Matsushita Electric Industrial Co Ltd filed Critical Matsushita Electric Industrial Co Ltd
Priority to JP60022263A priority Critical patent/JPS61182631A/en
Publication of JPS61182631A publication Critical patent/JPS61182631A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To improve the dispersibility of magnetic powder by freezing quickly a suspension consisting of three components; ferromagnetic powder, dispersant and liquid medium, evaporating away the medium component in the frozen state and using the ferromagnetic powder obtd. in such a manner as a magnetic coating paint. CONSTITUTION:The suspension consisting of the three components; the ferromagnetic powder, the dispersant which assists the dispersibility of the ferromagnetic powder by adsorbing chemically on the surface of said powder and the liquid medium, for example, water or the medium, for example, dioxane which can be easily frozen and has the high vapor pressure in the frozen state is prepd. After such suspension is quickly frozen, the medium component is removed by a freeze drying. The magnetic paint is prepd. by using the resulted magnetic powder. Such paint is coated on a non-magnetic base to form a magnetic layer. The dispersibility of the magnetic powder is thus improved and the improvement in the surface characteristic of the magnetic recording medium is made possible.

Description

【発明の詳細な説明】 産業上の利用分野 本発明は磁気記録媒体を製造する方法に関するもので、
特にいわゆる塗布型の高密度磁気記録媒体を得るべく強
磁性微粒子の分散性の高い磁性塗料を作る手段に特長を
有するものである。
DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method of manufacturing a magnetic recording medium.
In particular, the present invention is characterized by a means for producing a magnetic coating material with high dispersibility of ferromagnetic particles in order to obtain a so-called coated type high-density magnetic recording medium.

従来の技術 塗布型の磁気記録媒体は周知のように強磁性粉末、有機
質バインダ、必要な添加剤、溶剤とから成る磁性塗料を
調製し、この塗料を非磁性の基材の上に塗布して製造さ
れる。ここに必要な添加剤とは、塗料化に際して意味を
もつ界面活性剤や、記録媒体としてその特性を向上させ
るために加えられる材料、たとえば磁性層強化のための
アルミナ粉末、導電性を付与するためのカーボン粉末、
潤滑性を与えるだめの潤滑剤等の有機および無機の物質
を指す。この磁気記録媒体の製造方法は勿論多くの工程
よ構成るのであるが、それらの中でとりわけ重要なのは
高い分散性を有する磁性塗料を得る工程である。磁性塗
料は前述の塗料成分の単なる混合物ではなくて強磁性粉
子が凝集することなくのぞましくは粒子ひとつひとつが
ばらばらに分散された状態であることが必要である。こ
れは磁気記録媒体の振巾対周波数特性、変調ノイズ、不
連続ノイズ等の重要な特性が用いられた磁性金粉の分散
の度合いに強く依存していることが知られているからで
ある。こうした事から、これまで高い分散性の磁性塗料
を得るために多くの方法が提案され実行されて来た。塗
料構成成分のひとつとして分散剤と呼ばれる成分を加え
て分散操作を行なう方法が多く採用されている。分散剤
としてリン酸エステル系物質、高級脂肪酸とその誘導体
など強磁性粉末の表面に化学吸着してその表面の性質を
変えるものが用いられる。また予め磁性粉子に表面処理
を施したのち塗料化することも考えられ、たとえば磁性
粉表面にシリカコロイド粒子を付着させて磁性粒子の凝
集を防止すると云う特開昭56−130838号公報の
方法はその1例である。また、磁性粉を加熱乾燥後に粉
砕して吸油量を減少させる事によシ分散性を改善できる
とした磁性粉の処理方法が特開昭48−104505号
公報で開示されている。こうした磁性粉体の表面改質処
理と塗料化に際しての分散剤の添加との両手段が併用さ
れることも当然行なわれている。
Conventional technology As is well known, coating-type magnetic recording media involves preparing a magnetic coating consisting of ferromagnetic powder, an organic binder, necessary additives, and a solvent, and applying this coating onto a non-magnetic base material. Manufactured. The additives needed here include surfactants, which are important when making paints, and materials added to improve the properties of recording media, such as alumina powder to strengthen the magnetic layer, and materials to impart conductivity. carbon powder,
Refers to organic and inorganic substances such as lubricants that provide lubricity. The method for manufacturing this magnetic recording medium is of course comprised of many steps, but the most important of these is the step of obtaining a highly dispersible magnetic paint. The magnetic paint is not simply a mixture of the above-mentioned paint components, but it is necessary that the ferromagnetic particles are not agglomerated and preferably each particle is dispersed separately. This is because it is known that important characteristics of a magnetic recording medium, such as amplitude versus frequency characteristics, modulation noise, and discontinuous noise, strongly depend on the degree of dispersion of the magnetic gold powder used. For these reasons, many methods have been proposed and implemented to obtain highly dispersible magnetic paints. A commonly used method is to add a component called a dispersant as one of the constituent components of the paint to carry out the dispersion operation. Dispersants used include substances such as phosphoric acid ester substances, higher fatty acids and their derivatives, which chemically adsorb to the surface of the ferromagnetic powder and change the properties of the surface. It is also possible to surface-treat the magnetic powder in advance and then use it as a paint; for example, the method disclosed in Japanese Patent Application Laid-Open No. 130838/1983, in which colloidal silica particles are attached to the surface of the magnetic powder to prevent agglomeration of the magnetic particles. is one example. Further, JP-A-48-104505 discloses a method for processing magnetic powder that improves dispersibility by reducing oil absorption by crushing the magnetic powder after heating and drying it. Naturally, both the surface modification treatment of the magnetic powder and the addition of a dispersant when forming the powder into a paint are used in combination.

しかしながら近年、よシ一層の高密度磁気記録の要望に
こたえるために磁性粉末の粒子サイズのより一層の微細
化が進みつつあり、これは分散が困難な方向であるので
前述のような従来の諸方法では充分に分散しきれないと
云う問題があった。
However, in recent years, in order to meet the demand for even higher density magnetic recording, the particle size of magnetic powder has become increasingly finer, which makes dispersion difficult, so conventional methods such as those mentioned above have become more and more difficult. However, there was a problem in that the dispersion could not be sufficiently achieved using this method.

発明が解決しようとする問題点 このように1ミクロンの数分の1の粒子サイズの磁性微
粒体を用いる磁性塗料の調製は、分散剤の採用や凝集防
止策の採用しながら塗料に高いせん断応力を加えて混練
し微粒子集体体を崩して高分散状態とするのであるが、
なおまだ不充分である。過度の混線加工は磁性粒子の破
壊を招く。本発明はこの問題点を解決する方法を与える
ものである。
Problems to be Solved by the Invention As described above, the preparation of magnetic paint using magnetic fine particles with a particle size of a fraction of a micrometer requires high shear stress to be applied to the paint, while employing dispersants and measures to prevent agglomeration. is added and kneaded to break up the fine particle aggregates and create a highly dispersed state.
However, it is still insufficient. Excessive cross-wire processing leads to destruction of magnetic particles. The present invention provides a method to solve this problem.

問題点を解決するための手段 本発明は強磁性粉末の前処理として粉末表面処理の操作
の中に凍結乾燥法による処理を行ないしかるのちに通常
の分散手段により塗料化を行なうことによシ高分散塗料
が容易に得られると云う知見に基づくものである。即ち
この磁気記録媒体の製造方法では、まず強磁性粉末、こ
の粉末の表面に化学吸着してその分散性を助ける効果を
もつ分散剤、および適当な液体媒質たとえば水あるいは
ジオキサンのように容易に凍結でき且つ凍結状態での蒸
気圧が高いものの3成分よ9成る懸濁物を作る。次いで
この懸濁物を急速凍結する。しかるのち通常の凍結乾燥
法により媒質成分を除去する。
Means for Solving the Problems The present invention provides a highly efficient solution by pre-treating ferromagnetic powder by freeze-drying during the powder surface treatment, and then converting it into a paint using conventional dispersion means. This is based on the knowledge that dispersed paints can be easily obtained. That is, in this method of manufacturing a magnetic recording medium, first, a ferromagnetic powder, a dispersant that is chemically adsorbed onto the surface of the powder and has the effect of aiding its dispersibility, and a suitable liquid medium such as water or dioxane that freezes easily. A suspension consisting of 3 components is made, which has a high vapor pressure in the frozen state. This suspension is then flash frozen. Thereafter, the medium components are removed by a conventional freeze-drying method.

かくして得られた磁性粉末はきわめてかさだかいもので
ある。この粉末を用いて磁性塗料としこの塗料を非磁性
支持体上に塗布して磁性層を形成する。ここにおいて磁
性粉末とは磁気記録媒体に用いられる酸化物、金属、あ
るいは他の種類のものであってよく、その形状及び粒子
サイズも特に規定するものではない。また上述の磁性塗
料とは、表面処理され且つ凍結乾燥処理された強磁性粉
末と有機質バインダ、通常必要な無機質や有機質の添加
剤および溶剤とから成るもので本発明に固有に必要な添
加剤成分は何ら含まない。また分散剤とは、磁性粉体の
表面に吸着してその分散を助けるこの分野で知られてい
る化合物を指し、本発明に固有に必要な新規なものを指
すものではない。
The magnetic powder thus obtained is extremely bulky. This powder is used as a magnetic paint, and this paint is applied onto a non-magnetic support to form a magnetic layer. The magnetic powder herein may be an oxide, metal, or other type of powder used in magnetic recording media, and its shape and particle size are not particularly limited. Furthermore, the above-mentioned magnetic paint is composed of surface-treated and freeze-dried ferromagnetic powder, an organic binder, and usually necessary inorganic and organic additives and solvents, which are additive components unique to the present invention. does not contain anything. Further, the term "dispersant" refers to a compound known in this field that adsorbs to the surface of magnetic powder and aids in its dispersion, and does not refer to a new compound uniquely required for the present invention.

更に塗料化に際して用いられる分散機器としては通常用
いられるものでよいのであって、たとえばボールミル、
アトライタ、ロールミル、ペブルミル・サンドグライン
ダ、ストーンミル、ミキサー。
Furthermore, the dispersion equipment used for making the paint may be any commonly used dispersion equipment, such as a ball mill,
Attritor, roll mill, pebble mill/sand grinder, stone mill, mixer.

ニーグー、ディスパー、衝撃ミル、コロイドミル。Negoo, Disper, Impact Mill, Colloid Mill.

ホモジナイザ、超音波分散器等が適宜単独もしくは組み
合せて使用できる。
A homogenizer, an ultrasonic disperser, etc. can be used alone or in combination as appropriate.

作  用 作用の第1点は懸濁物が凍結する時にかなシの体積増加
がありこの時強磁性粉末の凝集体が崩壊する点にあると
みられる。更に作用の第2点は液相中で表面処理された
粉体が凍結状態から直接乾燥されるので粉体にとって再
凝集の機会が与えられない点にあるとみられる。
The first point of action appears to be that when the suspension freezes, the volume of the ferromagnetic powder increases, and at this time the ferromagnetic powder aggregates collapse. Furthermore, the second point of action appears to be that the powder surface-treated in the liquid phase is dried directly from the frozen state, so that the powder is not given a chance to reagglomerate.

実施例 次に実施例により本発明を説明する。Example Next, the present invention will be explained with reference to examples.

実施例1 BICT表面積40(vのCo被着型γ−Fe2o3粉
末5oot tステアリン酸ナトリウム16f。
Example 1 BICT surface area 40(v) Co-coated γ-Fe2O3 powder 5oot tSodium stearate 16f.

純水1ぶとをボールミルで混和して懸濁液を作る。Mix 1 cup of pure water in a ball mill to make a suspension.

この懸濁液を圧縮空気を用いてノズルよシ液体窒素中に
噴射して凍結する。凍結物を凍結乾燥器で処理して氷結
している水分を蒸発せしめて乾燥した磁性粉を得る。こ
の磁性粉を用いて次の組成の磁性塗料を作る。
This suspension is injected into liquid nitrogen through a nozzle using compressed air and frozen. The frozen product is treated with a freeze dryer to evaporate the frozen water and obtain dry magnetic powder. A magnetic paint with the following composition is made using this magnetic powder.

磁性粉           100重量部ポリウレタ
ン          1j  1ニトロセルロース 
      11 1カーボンブラツク       
 4Iアルミナ微粉          5Iステアリ
ン酸          2Iオレイルオレート   
     2 〃溶剤            320
 N上記配合割合の組成物をコロイドミルとサンドミル
とを順次用いて分散し、更に硬化剤としてポリイソシア
ネートを6部添加して混合し磁性塗料とした。この塗料
を公称値1ミクロンのフィルタによシ加圧濾過し、直ち
にポリエチレンテレフタレートフィルム上に塗布する。
Magnetic powder 100 parts by weight Polyurethane 1j 1 Nitrocellulose
11 1 carbon black
4I alumina fine powder 5I stearic acid 2I oleyl oleate
2 Solvent 320
N A composition having the above-mentioned mixing ratio was dispersed using a colloid mill and a sand mill sequentially, and 6 parts of polyisocyanate as a curing agent was added and mixed to obtain a magnetic paint. The paint is pressure filtered through a nominal 1 micron filter and immediately applied onto polyethylene terephthalate film.

これを乾燥硬化して磁気記録媒体試料とする。上記配合
割合の磁性塗料はこの分野においてはあシふれた組成の
ひとつである。
This is dried and hardened to obtain a magnetic recording medium sample. A magnetic paint having the above-mentioned compounding ratio is one of the popular compositions in this field.

実施例2 実施例1においてステアリン酸ナトリウムの代りに同量
のレシチン、純水の代りに同量のジオキサンを用いる以
外はすべて同様にして磁気記録媒体を作成した。
Example 2 A magnetic recording medium was prepared in the same manner as in Example 1 except that the same amount of lecithin was used instead of sodium stearate and the same amount of dioxane was used instead of pure water.

比較例1 実施例2において次の2点を変更する以外はすべて同様
にして比較用試料を作成した。
Comparative Example 1 A comparative sample was prepared in the same manner as in Example 2 except for the following two changes.

(イ)磁性粉、分散剤としてのレシチンおよび媒質より
成る懸濁物を作成せず、したがって凍結乾燥処理を施さ
ない。
(a) A suspension consisting of magnetic powder, lecithin as a dispersant and a medium is not created, and therefore no freeze-drying treatment is performed.

(ロ)塗料化に際して、レシチン3重量部を添加する。(b) When making a paint, 3 parts by weight of lecithin is added.

以上3つの試料に関して得られた計測値を次にのべる0 ■ 磁性塗料の濾過率:公称1ミクロンの濾過板を用い
ての2.5Kf/cIIでの加圧濾過率。
The measured values obtained for the above three samples are listed below. ■ Filtration rate of magnetic paint: Pressure filtration rate at 2.5 Kf/cII using a nominally 1 micron filter plate.

■ 磁性層の光沢度:カレンダ処理をする前の段階での
磁性層の45度光沢度0 ■ 磁性層表面粗さ:カレンダ処理後の磁性層表面のR
a  (中心線平均粗さ)表示による表面粗度。
■ Magnetic layer glossiness: 45 degree glossiness of the magnetic layer before calendering 0 ■ Magnetic layer surface roughness: R of the magnetic layer surface after calendering
Surface roughness expressed as a (center line average roughness).

■ ビデオ特性:VTRを用いた5MHz  における
再生出力値。比較例試料をo dB とする。
■ Video characteristics: Playback output value at 5MHz using a VTR. Let the comparative sample be odB.

発明の効果 以上の実施例と比較例かられかるように本発明による方
法で作成された磁気記録媒体はカレンダ前の磁性層の光
沢度およびカレンダ後の磁性層表面粗さの両面からみて
表面性が向上しておシこの効果がビデオ特性に明らかに
表われている。これは塗料濾過率の値と併せて考察する
に磁性粉末の分散性が改善されている事を意味している
としてよく、本方法はすぐれた特長をもつものである。
Effects of the Invention As can be seen from the above Examples and Comparative Examples, the magnetic recording medium produced by the method of the present invention has excellent surface properties in terms of both the glossiness of the magnetic layer before calendering and the surface roughness of the magnetic layer after calendering. The effect of this improvement is clearly visible in the video characteristics. When considered in conjunction with the value of paint filtration rate, this can be said to mean that the dispersibility of the magnetic powder is improved, and this method has an excellent feature.

Claims (1)

【特許請求の範囲】[Claims] 強磁性粉末、該強磁性粉末の表面に化学吸着してその分
散性を助ける分散剤および液体媒質の3成分よりなる懸
濁物を急速凍結し、凍結状態のまゝ該媒質成分を蒸発除
去して得られた強磁性粉末を用いて磁性塗料とし、該塗
料を非磁性の支持体上に塗布して磁性層を形成すること
を特徴とする磁気記録媒体の製造方法。
A suspension consisting of three components: a ferromagnetic powder, a dispersant that chemically adsorbs to the surface of the ferromagnetic powder to help its dispersibility, and a liquid medium is rapidly frozen, and the medium components are removed by evaporation while in the frozen state. 1. A method for manufacturing a magnetic recording medium, which comprises using the obtained ferromagnetic powder as a magnetic coating material, and coating the coating material on a non-magnetic support to form a magnetic layer.
JP60022263A 1985-02-07 1985-02-07 Production of magnetic recording medium Pending JPS61182631A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP60022263A JPS61182631A (en) 1985-02-07 1985-02-07 Production of magnetic recording medium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP60022263A JPS61182631A (en) 1985-02-07 1985-02-07 Production of magnetic recording medium

Publications (1)

Publication Number Publication Date
JPS61182631A true JPS61182631A (en) 1986-08-15

Family

ID=12077879

Family Applications (1)

Application Number Title Priority Date Filing Date
JP60022263A Pending JPS61182631A (en) 1985-02-07 1985-02-07 Production of magnetic recording medium

Country Status (1)

Country Link
JP (1) JPS61182631A (en)

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