JPS63168818A - Magnetic recording medium - Google Patents

Magnetic recording medium

Info

Publication number
JPS63168818A
JPS63168818A JP54787A JP54787A JPS63168818A JP S63168818 A JPS63168818 A JP S63168818A JP 54787 A JP54787 A JP 54787A JP 54787 A JP54787 A JP 54787A JP S63168818 A JPS63168818 A JP S63168818A
Authority
JP
Japan
Prior art keywords
film
spherical silica
silica particles
magnetic recording
recording medium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP54787A
Other languages
Japanese (ja)
Other versions
JPH0628099B2 (en
Inventor
Hisashi Hamano
浜野 久
Kinji Hasegawa
欣治 長谷川
Norihiro Nomi
能美 慶弘
Hideo Kato
秀雄 加藤
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.)
Teijin Ltd
Original Assignee
Teijin 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 Teijin Ltd filed Critical Teijin Ltd
Priority to JP62000547A priority Critical patent/JPH0628099B2/en
Publication of JPS63168818A publication Critical patent/JPS63168818A/en
Publication of JPH0628099B2 publication Critical patent/JPH0628099B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Magnetic Record Carriers (AREA)
  • Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

PURPOSE:To obtain a magnetic recording medium which permits high-density recording and withstands repetitive use by using a biaxially oriented polyester film into which spherical silica particle having a specified average grain size and grain size ratio are dispersed and incorporated. CONSTITUTION:The biaxially oriented polyester film into which the spherical silica particles having 0.3-4mum average grain size and 1.0-1.2 grain size ratio (major axis/minor axis) are dispersed and incorporated at 0.01-1wt.% is used. The polyester into which the spherical silica particles are dispersed and incorporated is produced by adding the spherical silica particles (preferably in the form of slurry in glycol) to the polyester at the time of reaction for forming ordinary polyester, for example, at an arbitrary timing during ester exchange reaction or polycondensation reaction in the case by an ester exchange method or at an arbitrary timing in the case by a direct polymn. method. The magnetic recording medium formed by using such biaxially oriented polyester film has an excellent electromagnetic conversion characteristic, slipperiness, running durability, etc.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 不発明は磁気記録媒体に関し、更に旺しくはxi変換特
性にすぐれ、特定の球状シリカ微粒子を含有し、耐剛れ
性に貢れ、更には滑り性の改IIされた二軸配向ポリニ
スナルフィルムを基体とすることを特徴とする磁気記録
媒体に関する。
[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a magnetic recording medium, and more preferably has excellent xi conversion characteristics, contains specific spherical silica fine particles, contributes to stiffness resistance, and furthermore The present invention relates to a magnetic recording medium characterized by having a substrate made of a biaxially oriented polynisnar film with improved sliding properties.

〔従来技術〕[Prior art]

ポリエステルフィルムをベースとした磁気記録媒体とし
て、例えばビデオテープ、オーデオデープ、フンビュー
クテープ、フミンビーディスク等が仰られ、広く用いら
れている。
Examples of magnetic recording media based on polyester films include video tapes, audio tapes, Humbuk tapes, and Huminbee disks, which are widely used.

これらの用途分野は近年、藺密良紀録化、−品質化の景
求がますます高まり、これに伴ってベースとなるポリエ
ステルフィルムには赤面が平坦でしかも滑り性に丁ぐれ
、かつ耐久走行性。
In recent years, demand for improved quality has increased in these fields of application, and as a result, the base polyester film has to have a flat surface, excellent slipperiness, and durable running properties. .

耐F511れ性に丁ぐれていることの*Xがますます強
(なっている。
The *X of being excellent in F511 resistance to scratches is becoming more and more strong.

従来、易滑性を同上させる方法としてポリエステルに戻
ぽカルシウム寺の無機質粒子を添加yる方法、又はポリ
エステルの会成時Kl[合系内でカルシウム、リチウム
あるいはリンを含む微粒子を析出せしめる方法が提案さ
れている。
Conventionally, methods for improving slipperiness include adding calcium-containing inorganic particles to polyester, or precipitating fine particles containing calcium, lithium, or phosphorus in the composite system during the formation of polyester. Proposed.

いずれの方法もポリエステルを成形、−伸製膜する際に
微粒子に由来してフィルム表面に突起を形成し、フィル
ムの易滑性上hミ之辻ゐもの2あう。
In both methods, projections are formed on the surface of the film due to fine particles when polyester is formed and stretched into a film, which is problematic in terms of the slipperiness of the film.

しかしながら、王妃の如き微粒子による突起によってフ
ィルムの滑り性をrR1!する方法では、通常、フィル
ム表面を粗面化する程滑り性は向上するが、一方では該
粗面化に起因して磁気塗料をm布後の表面が粗れ電磁変
換特性が悪化する傾向がある。
However, the projections caused by the queen-like particles reduce the film's slipperiness to rR1! In this method, the slipperiness usually improves as the film surface becomes rougher, but on the other hand, due to the roughening, the surface after applying the magnetic paint tends to become rough and the electromagnetic conversion characteristics tend to deteriorate. be.

これらの相反する平坦性と易滑性とを解決する方策の一
つとして、大粒径の粒子と小粒径の粒子とを併存させろ
複合系無機粒子を利用する手段も数多く提*され【いる
。しかしながら、これらの手段にも問題があり、そのま
までは磁気記録媒体の高級グレード化例えば高VB度化
As one of the measures to solve these contradictory problems of flatness and slipperiness, many methods have been proposed, including the use of composite inorganic particles in which large-sized particles and small-sized particles coexist. . However, these methods also have problems, and if they are not used as they are, it will be difficult to upgrade the magnetic recording medium to a higher grade, for example, to increase the VB degree.

嶋品實化等の*累に応じることが幽しい。この理由は、
複合系無機粒子に用いられる大粒径程子のサイズが高級
グレード化の景求品質に対して粗大であること、大粒子
になればなる4!4フィルム六面の突起は痛くなると共
に粒子の囲りのボイドも大きくなり、不a布でのクリー
ニング工程あるいはカレンダー加エエ根においC1%い
突起部が刈り落され、ドロップアウト(記録再生時に発
生する情報の欠落部)の原因をひきおこし、11LK加
エエ根でのカレンダー汚れや、ベースフィルム表面清掃
用のダストファブリック汚れをひきおこし、磁気記録媒
体としての特性を大きく損うことになる。
It is difficult to respond to the demands of Shima Shinako and others. The reason for this is
The size of the large particle diameter scaler used for composite inorganic particles is too large compared to the desired quality of high-grade grades. The voids in the area also become larger, and during the cleaning process with non-a cloth or calendering, the C1% protrusion is cut off at the root, causing dropouts (missing information that occurs during recording and playback), and 11LK addition. This causes calendar stains from the air roots and stains from the dust fabric used for cleaning the base film surface, which greatly impairs its properties as a magnetic recording medium.

〔発明の目的〕[Purpose of the invention]

本発明者は、上述の問題点を解決し、高級品質の磁気記
録用途分野に適用可能な平坦性と易滑性と耐削れ性とを
兼備したフィルムの開発に成功し、該フィルムなi体と
する磁気記録媒体が丁ぐれた特性を有することを知見し
、本発明に到達した。
The present inventor has solved the above-mentioned problems and succeeded in developing a film that has flatness, ease of slipping, and abrasion resistance that can be applied to the field of high-quality magnetic recording, and has developed an i-formed film. The present invention was achieved based on the discovery that a magnetic recording medium of the type described above has distinct characteristics.

本発明の目的は、高蜜度記録が可能で、^品質でしかも
繰返し使用に耐え得る磁気配録媒体を提供することにあ
り、更にdベースフィルムにおいて、(1)拠−に大き
な突起はな(、平坦であるがドロップアウト等のノイズ
の原因とならない種度の微小な突起が存在しており、(
2)繰り返し走行時の摩擦係数が小さく、(3)磁気記
録媒体のJ工工程及び磁気記録再生装置の部分との接触
によるベースフィルムの削れ烏が極めて少なく、継続的
使用における耐久性が良好な磁気記録媒体を提供するこ
とにある。
An object of the present invention is to provide a magnetic recording medium that is capable of high-density recording, has high quality, and can withstand repeated use, and furthermore, in a d-base film, (1) there are no large protrusions on the base. (Although it is flat, there are some small protrusions that do not cause noise such as dropouts.
2) The coefficient of friction during repeated running is small; (3) there is very little wear and tear on the base film due to contact with the J-processing process of the magnetic recording medium and the magnetic recording/reproducing device; it has good durability during continuous use. The purpose of this invention is to provide a magnetic recording medium.

〔発明のJlllhX、・効果〕[JlllhX of the invention, effect]

本発明の目的は、本発明によれば、平均粒径が0.3〜
4μm でありかつ粒径比(長径/短径)が1.0〜1
.2である球状シリカ粒子を0.01〜1j[t%分散
含有させてなる二軸配向ポリエステルフィルム、及び該
フィルムの少くとも片面上の磁性層からなる磁気記録媒
体によって達成される。
The object of the invention is that according to the invention, the average particle size is between 0.3 and 0.3.
4 μm and a particle size ratio (major axis/minor axis) of 1.0 to 1.
.. This is achieved by a magnetic recording medium comprising a biaxially oriented polyester film containing 0.01 to 1 j [t%] of spherical silica particles of No. 2 dispersed therein, and a magnetic layer on at least one side of the film.

ここで、シリカ粒子の長径0gi径1ml槓円相当径は
粒子表面に金薄膜層を蒸着したのち走査域電子顕微鏡に
て1万〜3万倍に拡大した像から求め、平均粒径1粒径
比を次式で求める。
Here, the long axis of the silica particle is 0 gi, and the equivalent diameter of a 1 ml circle is determined from an image magnified 10,000 to 30,000 times with a scanning area electron microscope after depositing a gold thin film layer on the particle surface, and the average particle size is 1 particle size. Find the ratio using the following formula.

平均粒径=測定粒子の面積円相当径の総和/測定粒子の
数粒径比=シリカ粒子の平均長径/核粒子の平均短径本
発明におけるポリエステルとは芳香族ジカルボン酸を主
たる威属分とし、脂肪族グリコールを主たるグリコール
成分とするポリエステルであΦ。かかるポリエステルは
実質的に線状であり、そしてフィルム形成性特に溶融成
形によるフィルム形成性を有する。芳香族ジカルボン酸
としては、例えばテレフタル酸、ナフタレンジカルボン
酸、イソフタル酸、ジフェニルエタンジカルボン酸、ジ
フェニルジカルボン酸、シフェニルエーテルジカルポン
酸、ジフェニルスルホンジカルボンrIll ジフェニ
ルグトンジカルポン酸、アンスラセンジカルボン#1等
を挙げることができる。脂肪族グリコールとしては、例
エバエチレングリコール、トリメキレングリコール、テ
トラメチレングリコール、ペンタメチレングリコール、
へ士すメチレングリコール。
Average particle diameter = Sum of area circle equivalent diameters of measured particles / Number of particle diameter ratio of measured particles = Average major diameter of silica particles / Average minor diameter of core particles The polyester in the present invention is a polyester containing aromatic dicarboxylic acid as the main component. , is a polyester whose main glycol component is aliphatic glycol. Such polyesters are substantially linear and have film forming properties, particularly by melt molding. Examples of aromatic dicarboxylic acids include terephthalic acid, naphthalene dicarboxylic acid, isophthalic acid, diphenylethane dicarboxylic acid, diphenyl dicarboxylic acid, diphenyl ether dicarboxylic acid, diphenylsulfone dicarboxylic acid, diphenylgutone dicarboxylic acid, and anthracene dicarboxylic acid #1 etc. can be mentioned. Examples of aliphatic glycols include evapoethylene glycol, trimekylene glycol, tetramethylene glycol, pentamethylene glycol,
Heshisu methylene glycol.

デカメチレングリコールの如き炭素数2〜10のポリメ
チレングリコールあるいはシクロへ千サンジメタツール
の如@脂環族ジオール等を挙げることかできる。
Examples include polymethylene glycols having 2 to 10 carbon atoms such as decamethylene glycol, and alicyclic diols such as cyclohesane dimetatool.

本発明において、ポリエステルとしては例えばアルキレ
ンテレフタレート及び/又はアルキレンナフタレートを
王たる構成取分とするものが好ましく用いられる。
In the present invention, polyesters containing, for example, alkylene terephthalate and/or alkylene naphthalate as a major constituent are preferably used.

かかるポリエステルのうちでも、例えばポリエチレンテ
レフタレート、ポリエチレン−2,6−す7タレートは
もちろんのこと、例えば全ジカルボン酸成分の80モル
%以上がテレ7グルレングリコールである共電合体が好
ましい。その際全酸成分の20モル%以下はテレフタル
酸及び/又は2.6−ナフタレンジカルボン酸以外の上
記芳香族ジカルボン酸であることができ、また例えばア
ジピン戚、セパチン酸の如き脂肪族ジカルボン酸;シク
ロヘキサン−1,4−ジカルボン酸の如き脂環族ジカル
ボン酸等であることができる。また、全グリコール成分
の20モル%以下は、エチレングリコール以外の上記グ
リコールであることができ、あるいは例えばノ1イドa
千ノン、レゾルシン、2.2−ビス(4−ヒドロキシフ
ェニル)プロパンの如き芳香族ジオールt、L4−ジL
ドロキシメチルベンゼンの如き芳香場を含む脂肪族ジオ
ール;ポリエチレングリコール、ポリプロピレングリコ
ール、ポリテトラメチレングリコールの如きポリアルキ
レングリフール(ポリオキシフルキレングリコール)等
であることもできる。
Among such polyesters, preferable examples include polyethylene terephthalate and polyethylene-2,6-su7talate, as well as coelectric polymers in which 80 mol % or more of the total dicarboxylic acid component is tere7 gullene glycol. In this case, up to 20 mol% of the total acid component can be the above-mentioned aromatic dicarboxylic acids other than terephthalic acid and/or 2,6-naphthalene dicarboxylic acid, and also aliphatic dicarboxylic acids such as adipine-related and cepatic acid; It can be an alicyclic dicarboxylic acid such as cyclohexane-1,4-dicarboxylic acid. Also, up to 20 mol% of the total glycol component can be the above-mentioned glycols other than ethylene glycol, or e.g.
Aromatic diols such as 1,4-diol, resorcinol, 2,2-bis(4-hydroxyphenyl)propane,
Aliphatic diols containing aromatic groups such as droxymethylbenzene; polyalkylene glycols (polyoxyfulkylene glycols) such as polyethylene glycol, polypropylene glycol, polytetramethylene glycol, and the like can also be used.

また1本発明で用いるポリエステルには、例えばヒトミ
キシ安息香酸の如き芳香族オキシ酸;ω−ヒドロキシカ
プロン酸の如き脂肪族オキシ酸等のオキシカルボンa!
に由来する成分を、ジカルボン酸成分およびオキシカル
ボン鈑成分のm*に対し20モル5以下で共1合或は結
合するものも包含される。
In addition, the polyester used in the present invention includes, for example, aromatic oxyacids such as human mixybenzoic acid; oxycarboxylic acids such as aliphatic oxyacids such as ω-hydroxycaproic acid;
It also includes those in which components derived from the above are combined or combined in an amount of 20 mol 5 or less with respect to m* of the dicarboxylic acid component and the oxycarboxylic acid component.

さらに本発明におけるポリエステルには実質的に線状で
ある範囲の麓、例えば全酸成分に対し2モル%以下の童
で、3官能以上のポリカルだものをも包含される。
Furthermore, the polyester in the present invention also includes polycarboxylic acids at the base of the substantially linear range, such as trifunctional or higher functional polycarboxylic acids having a content of 2 mol % or less based on the total acid component.

上記ポリエステルは、それ自体公知であり、且つそれ自
体公知の方法で製造することができる。
The above polyester is known per se, and can be produced by a method known per se.

上記ポリエステルとしては、0−りaaミツエノールの
溶液として35℃で測定して求めた固有粘度が約0.4
〜約0.9のものが好ましい。
The above polyester has an intrinsic viscosity of about 0.4 as measured at 35°C as a solution of 0-lyaa mitsuenol.
~0.9 is preferred.

本発明の二軸延伸ポリエステルフイルムハソのフィルム
表面に多数の微細な突起を有している。それらの多数の
微細な突起は本発明によればポリエステル中に分散して
含有される多数の球状シリカ粒子に由来する。
The biaxially stretched polyester film of the present invention has many fine protrusions on its surface. According to the invention, these large numbers of fine protrusions originate from a large number of spherical silica particles dispersed and contained in the polyester.

球状シリカ粒子を分散含有するポリエステルは、通常ポ
リエステルを形成するための反応時、例えばエステル交
換法による場合のエステル交換反応中あるいは1#合反
応中の任意の時期、泳り直接電合法による場合の任意の
時期に、球状シリカ粒子(好ましくはグリコール甲のス
ラリーとしC)を反応系中に添加することにより製造す
ることができる。好ましくは、ム扁合反応の初期例えば
固有粘度が約0.3に至るまでの間に、球状シリカ粒子
を反応系中に添加するのか好ましい。
Polyester containing dispersed spherical silica particles is usually used at any time during the reaction to form polyester, for example, during the transesterification reaction when using the transesterification method or during the 1# synthesis reaction when using the swimming direct electrolysis method. It can be produced by adding spherical silica particles (preferably glycol A slurry C) to the reaction system at any time. Preferably, the spherical silica particles are added to the reaction system at the initial stage of the molarization reaction, for example, until the intrinsic viscosity reaches about 0.3.

本発明においてポリエステル中に分散含有させる球状シ
リカ粒子は平均粒径が0.3〜4μmでありかつ粒径比
(−Ik径/短径)が1.0−1.2であるシリカ粒子
である。この球状シリカ粒子は個々の形状が極めて真球
に近い球状であって、従来から滑剤として知られている
シリカ粒子が10 sp程度の超微細な翼状粒子か、こ
れらがシ集して0,5μ8度のlik集物(凝集粒子)
を形成しているのとは著しく異なる点に時機がある。
In the present invention, the spherical silica particles dispersed and contained in polyester are silica particles having an average particle diameter of 0.3 to 4 μm and a particle diameter ratio (-Ik diameter/breadth diameter) of 1.0 to 1.2. . These spherical silica particles have individual shapes that are extremely close to true spheres, and the silica particles conventionally known as lubricants are ultrafine wing-shaped particles of about 10 sp, or they are aggregated into particles of 0.5 μ8. degree of lik agglomeration (agglomerated particles)
There is a point in time that is markedly different from what is currently being formed.

球状クリ力程子の平均粒径は好ましくは0.3〜3μm
5更に好ましくは0.3〜2μmである。この平均粒径
が0.3μm 未満では滑り性や、耐削れ性の向上効果
が不光分であり、好ましくない。
The average particle diameter of the spherical chestnut is preferably 0.3 to 3 μm.
5, more preferably 0.3 to 2 μm. If the average particle size is less than 0.3 μm, the effect of improving slipperiness and abrasion resistance will be insufficient, which is not preferable.

また平均粒径が4μm を起えるとフィルム表面か粗れ
すぎて好ましくない。また球状シリカ粒子の粒径比は好
1しくは1.0〜1.15、更に好ましくは1.0〜1
.1である。
Moreover, if the average particle diameter is 4 μm, the surface of the film becomes too rough, which is not preferable. The particle size ratio of the spherical silica particles is preferably 1.0 to 1.15, more preferably 1.0 to 1.
.. It is 1.

また、球状シリカ粒子は粒径分布がシャープであること
が好ましく、分布の急峻度を表わす相対樟準4A差が0
.5以下、更にFio、4以下、特に0.3以下である
ことが好ましい。
Further, it is preferable that the spherical silica particles have a sharp particle size distribution, and the relative camphor 4A difference representing the steepness of the distribution is 0.
.. Fio is preferably 5 or less, more preferably 4 or less, particularly 0.3 or less.

この相対標準偏差は次式で表わされる。This relative standard deviation is expressed by the following formula.

ここで、Dl二個々の粒子の面積円相当径(μm)D 
:粒子の6111定116!fl t表わす。
Here, Dl2 The area circle equivalent diameter (μm) of each individual particle D
: 6111 constant 116 of particles! fl t is expressed.

相対標4偏差が0.5以下の球状シリカ粒子を用いると
、該粒子が球状で且つ粒度分布が極めて急峻であること
から、フィルム表面突起の^さが極め【均一となる。史
にフィルム次面の個個の突起は、滑剤周辺のボイドが小
さいために突起形状が非常にシャープであり、従って同
じ突起の数であつ℃も滑り性が極めて良好となる。
When spherical silica particles with a relative standard deviation of 0.5 or less are used, since the particles are spherical and have an extremely steep particle size distribution, the protrusions on the film surface become extremely uniform. Historically, the individual protrusions on the surface of the film have very sharp protrusions because the voids around the lubricant are small, and therefore, even with the same number of protrusions, the slipperiness is extremely good even at ℃.

球状シリカ粒子は、上述の条件を満せば、その製法、そ
の他に何ら限定されるものでにない。
As long as the spherical silica particles satisfy the above-mentioned conditions, there are no limitations on the manufacturing method or the like.

例えば球状シリカ粒子は、オルトケイ酸エチル(5i(
OCl)(、)、 )の加水分解から含水シリカ(St
 (Of()4 )単分散球をつくり、更にこの含水シ
リカ単分散球を脱水化処理し【シリカ結合(!Sk −
0−8tミ〕を三次元的に成長させること’2−1を造
できる(日本化学会誌’81./$119゜P、150
3) 。
For example, spherical silica particles are made of ethyl orthosilicate (5i(
Hydrous silica (St
(Of()4) Monodisperse spheres are made, and the hydrous silica monodisperse spheres are further dehydrated to [Silica bond (!Sk −
0-8t Mi] can be grown three-dimensionally to produce '2-1' (Journal of the Chemical Society of Japan '81./$119゜P, 150
3).

S i (QC,H,)、 + 48.O→S i (
01()4+ 40.H,0H=Si−OH+HQ−8
tジ→==st−o−stヨ+H1O本発明において球
状シリカ粒子の龜加意は、ポリエステルに対しCO40
1〜t、oat%とする必費があり、好ましくriO,
01〜0,5貞t%、更に好ましくは0.05〜0.3
重重%である。祭加濾が0,01J[菫%未勇では、滑
り性や酎削れ性の向上効果が不光分となり、一方1.O
A[111%な越えるとa面平坦注が低下し、好ましく
なし・。
S i (QC, H,), + 48. O→S i (
01()4+ 40. H,0H=Si-OH+HQ-8
tdi→==st-o-styo+H1O In the present invention, the effect of spherical silica particles is to reduce CO40 to polyester.
There is a necessary cost of 1 to t, oat%, preferably riO,
01-0.5 t%, more preferably 0.05-0.3
Weight%. When the festival filter is 0.01J [Sumiyu% Miyu, the improvement effect on slipperiness and shaving property becomes a non-light component, while 1. O
A [If it exceeds 111%, the a-plane flatness will decrease, which is not preferable.

本発明の二軸配回ポリエステルフィルムは従来から蓄積
された二@延伸フィルムの裂遺法にj誤じて製造できろ
。例えば、球状シリカ粒子を含有するポリエステルを溶
融製膜して非晶質σ)未延伸フィルムとし、次いで鉄未
延伸フィルムをニ一方向に延伸し、熱固定し、必要であ
れば弛緩熱処理することによって製造される。その際、
フィルム次面特性は、球状シリカ粒子の粒径9重等によ
って、また延伸条件によって変化するので従来の低伸条
件から適宜選択する。またt!!度、熱収jilI!′
4等も延伸、熱処理時の温度。
The biaxially oriented polyester film of the present invention can be manufactured using the conventional method of splitting the bi-stretched film. For example, a polyester containing spherical silica particles is melt-formed to form an amorphous σ) unstretched film, then an iron unstretched film is stretched in two directions, heat set, and if necessary subjected to relaxation heat treatment. Manufactured by. that time,
The lateral properties of the film vary depending on the particle size of the spherical silica particles (nine folds) and the stretching conditions, so they are appropriately selected from conventional low stretching conditions. T again! ! degree, heat absorption! ′
4th grade also shows the temperature during stretching and heat treatment.

@軍、速F!L等によって変化するので、これらの特性
を同時に満足する条件を定める。例えば、延伸温度は1
段目延伸温度(例えば縦方向延伸温度:T、)か(Tg
−10)〜(Tg+45)℃のm囲(但し、’rg :
ポリエステルのガラス転移温度)から、2段目延伸温良
(例えは慣方向延伸温x:’r*)が(’r、+ 15
 ) 〜(’r、+40 ) ℃(1)範Jから選択す
るとよい。また、延伸倍率はm一方向の延伸倍率が2.
5以上、符に3Wr以上でかつ面積倍率が8倍以上、特
に10倍以上となる範囲から選択するとよい。史にまた
、熱固定温度は180〜250℃、丈には200〜23
0℃の範囲から選択するとよい。フィルム厚みは1〜1
00μが好ましい。
@Military, fast F! Since it changes depending on L, etc., conditions are set to satisfy these characteristics at the same time. For example, the stretching temperature is 1
The stage stretching temperature (e.g. longitudinal stretching temperature: T) or (Tg
−10) to (Tg+45)°C (where 'rg:
From the glass transition temperature of polyester), the second-stage stretching temperature (for example, inertial direction stretching temperature x: 'r*) is ('r, + 15
) to ('r, +40) °C (1) It is preferable to select from range J. In addition, the stretching ratio in one direction is m.
It is preferable to select from a range of 5 or more, 3Wr or more, and an area magnification of 8 times or more, particularly 10 times or more. Historically, the heat setting temperature is 180-250℃, and the length is 200-23℃.
It is preferable to select from the range of 0°C. Film thickness is 1-1
00μ is preferred.

本発明の二軸配向ポリエステルフィルムは、従来のもの
く比してボイドの極めて小さいフィルムであるが、この
ボイドが小さい理由は、球状シリカ粒子のポリエステル
への親和性の良さと、更に粒子そのものが極めて真球に
近いことから、延伸におい?滑剤周辺の応力が均等に伝
播し、ポリエステルと滑剤の界面の一部に応力が県中し
ないことによると推−jされる。
The biaxially oriented polyester film of the present invention has extremely small voids compared to conventional films.The reason why the voids are small is that the spherical silica particles have good affinity for polyester, and the particles themselves are Because it is extremely close to a true sphere, does it smell like stretching? This is thought to be due to the fact that the stress around the lubricant propagates evenly and the stress is not distributed all over the interface between the polyester and the lubricant.

本発明の二軸配向ポリエステルフィルムは、均一な凹凸
表面特性、すぐれた滑り性及び耐削れ性を有し、すりき
す、白粉等の発生量が著しく少ないといつ特徴を有する
。本発明においては、この二11tl配向ポリエステル
フィルムのこれらの特性を活かして磁気記録媒体例えは
ビデオテープ、オーディオテープ、コンピューターテー
プ、フロッピーディスク等とするから、該磁気記録媒体
は優れた*m変換時性、滑り性、走行耐久性等を有する
The biaxially oriented polyester film of the present invention has uniform uneven surface characteristics, excellent slipperiness and abrasion resistance, and is characterized in that it generates significantly less scum, white powder, and the like. In the present invention, these characteristics of the 211tl oriented polyester film are utilized to produce magnetic recording media such as video tapes, audio tapes, computer tapes, floppy disks, etc., so that the magnetic recording media have an excellent *m conversion time. It has properties such as flexibility, slipperiness, and running durability.

本発明において二軸配向ポリエステルフィルムの少なく
とも片面、すなわち片面又は両面に設げる磁性層は塗布
製磁性層でもよく、また金ける方法はそれ自体公知であ
り、本発明にお(Sても公知の磁性層およびそれを設け
る方法な採用することができる。
In the present invention, the magnetic layer provided on at least one side of the biaxially oriented polyester film, that is, on one side or both sides, may be a coated magnetic layer. A magnetic layer and a method for providing the same can be employed.

例えば、磁性層をベースフィルム上に磁性塗料を塗布す
る方法によって設ける場合には、磁性層に用いられる強
磁性粉体としてはr Fetus *Cn を有のr 
 Fetus e Fe504 * Co含有のFe1
Oa IC,O,、バリタム7エライト等、公知の強磁
性体が使用できる。磁性粉俸と共に使用されるバインダ
ーとしては、公知の熱可塑性11脂、熱硬化性樹脂9反
応#1樹脂又はこれらの混曾物である。
For example, when a magnetic layer is provided by coating a magnetic paint on a base film, the ferromagnetic powder used for the magnetic layer is r Fetus *Cn.
Fetus e Fe504 * Co-containing Fe1
Known ferromagnetic materials such as Oa IC, O, and Baritum 7 Elite can be used. The binder used with the magnetic powder is a known thermoplastic 11 resin, thermosetting resin 9 reaction #1 resin, or a mixture thereof.

これらの樹脂としては例えば、塩化ビニル−咋醒ビニル
共重合体、ポリウレタンエラストマー等があげられろ。
Examples of these resins include vinyl chloride-reactive vinyl copolymers, polyurethane elastomers, and the like.

磁性塗料は、さらに研!II剤例えばα−AltOs→
、導電剤例えばカーボンブランク等、分散剤例えばレシ
チン等、潤滑剤例えばn−メチルステアレート、レシチ
ン酸等、硬化剤例えばエポーaシ樹m、溶媒例えばメチ
ル二チルグトン、メチルインプチルグトン、トルエン等
を含有することができる。
Magnetic paint is further polished! Agent II, e.g. α-AltOs→
, conductive agent such as carbon blank, dispersant such as lecithin, lubricant such as n-methyl stearate, lecithic acid, curing agent such as epoxy resin, solvent such as methyl ditylgtone, methyl imptylgtone, toluene, etc. can contain.

磁性層を、ベースフィルム上に金属4膜な形成させる方
法によって設ける場合には、それ自体公知の真窒/Ik
N法、スパッタ法、イオンブレーティング法、  C,
V、D、 (Chemical Vapouri)ep
osition )法、無電解メッキ法等の方法を採用
することができる。金属としては、鉄、コノ〈ルト、ニ
ッケルおよびそれらの合金(例えがCo−N1−P合金
、 Co −Nt−Fe合金、 Go−Cr合金又はC
o−1’H会金4り等を例示できる。
When the magnetic layer is provided by a method of forming four metal films on a base film, a well-known true nitrogen/Ik
N method, sputtering method, ion blating method, C,
V, D, (Chemical Vapori) ep
A method such as an electroless plating method or an electroless plating method can be employed. Examples of metals include iron, metal, nickel, and alloys thereof (for example, Co-N1-P alloy, Co-Nt-Fe alloy, Go-Cr alloy or C
An example is o-1'H meeting fee 4.

〔実施例〕〔Example〕

以下、実施例を掲げて本発明を更に説明する。 The present invention will be further explained below with reference to Examples.

なお本発明における撞々の物性値および特性は以下の如
(測定されたものである。
The physical property values and characteristics of the present invention are as follows (measured).

(1)粒子の粒径 粒子粒径の#1定には次の状態がある。(1) Particle size of particles The #1 constant of particle size has the following conditions.

l)シリカ粉体から、平均粒径1粒径比等を求める場合 2)フィルム中のシリカ粒子の平均粒径9粒径比等を求
めろ場合 l)シリカ粉体からの場合二 電顕試料台上にシリカ粉体を個々の粒子ができるだけ点
らないように散在せしめ、金スパッター装置によりこの
表面に金薄膜蒸着層を厚み200A〜300Aで形成せ
しめ、走査屋電子w!i微鋭にて10000〜3000
0倍で観察し、日本レギュレーター■裂ルーゼツクス5
00にて、少なくとも100個の粒子の長径(DJi)
、短径(Dsi)及び山積円相当径(Di)を求める。
l) When calculating the average particle size 1 particle size ratio etc. from silica powder 2) When calculating the average particle size 9 particle size ratio etc. of silica particles in the film l) When using silica powder 2 electron microscopy sample Silica powder was scattered on a table so that individual particles would not be scattered as much as possible, and a thin gold film deposited layer with a thickness of 200 to 300 A was formed on the surface using a gold sputtering device. 10,000-3,000 at i-wei-kei
Observe at 0x magnification, Japan Regulator ■Rusetux 5
At 00, the major diameter of at least 100 particles (DJi)
, the short axis (Dsi) and the equivalent diameter of the piled circle (Di) are determined.

そして、これらの次式で表わされる数平均値をもって、
シリカ粒子の長径(1)J)、短径(Ds)。
Then, with the number average value expressed by these following formulas,
Long axis (1) J) and short axis (Ds) of silica particles.

平均粒径(D)を樅わす。Determine the average particle size (D).

2)フィルム中のシリカ粒子の場合: 試料フィルム小片を走fm電子顕微鏡用試料台に固定し
、日本電子■袈スパッターリング装置it (JFC−
1100型イオンスパツターリング装置)を用いてフィ
ルム表面に下記条件にてイオンエツチング処理を施した
。条件はペルジャー内に試料を設置し、約10−” T
orrの臭窒状悪まで真!![を上げ、電圧0.25k
Y、電(it 12.5 mA  にてilO分間イオ
ンエンチング1に実施した。更に同装置に℃フィルム表
面に金スパッターを施し、走f!i電子−微虜にて10
000〜30000倍で観察し、8不しギュレーター■
袈ルーゼンクス500にて少な(とも100個の粒子の
長径(Dji)、短径(Dsi)及び面積円相当径(D
i)を求める。以下、上記l)と同様に行なう。
2) In the case of silica particles in a film: A small piece of sample film was fixed on a sample stage for a scanning FM electron microscope, and sputtered using a JEOL sputtering device it (JFC-
The surface of the film was subjected to ion etching using an ion sputtering device (Model 1100) under the following conditions. The conditions were to place the sample in a Pel jar and set it at approximately 10-” T.
Even the odor-like evil of orr is true! ! [Increase the voltage to 0.25k
Ion etching was carried out for 1 min at 12.5 mA.Furthermore, gold sputtering was performed on the film surface at °C using the same equipment, and the etching was performed at 12.5 mA for 10 min at 12.5 mA.
Observe at 000 to 30000 times magnification and use an 8-magulator ■
The long axis (Dji), short axis (Dsi), and area circle equivalent diameter (D
Find i). The following steps are carried out in the same manner as in 1) above.

(2)フィルム表面粗さくR&) 中心線平均粗さくR&)としてJ I S −BO60
1で定義される値であり、本発明では■小礪研究所の触
針式表面粗さ針(SURFCORDER8E−30C)
を用いて測定する。#j定条件等は次の通りである。
(2) Film surface roughness R&) Center line average roughness R&) JIS-BO60
1, and in the present invention ■Stylus type surface roughness needle (SURFCORDER8E-30C) from Kozubo Research Institute
Measure using. #j conditions etc. are as follows.

(&)  置針先端半径 :  2μ篤(bl  測定
圧力   : 30キ (c)  カットオフ  :   0,25m(dl 
  測  足  長    ’     U、5   
tm(el  デーグーのまとめ方 同−試料について5回繰返し測定し、最も大きい値を1
つ除き、残り4つのデーグーの平均値の小数点以下4桁
目を四捨五入し、小数点以下3桁目まで表示する。
(&) Needle tip radius: 2 μm (bl) Measurement pressure: 30 m (c) Cutoff: 0.25 m (dl)
Measurement length 'U, 5
tm (el) How to summarize the sample - Measure the sample 5 times and take the largest value as 1.
Round off the average value of the remaining four Daeghus to the fourth decimal place and display it to the third decimal place.

(3)  ボイド比 上記tll−2)  の方法に従ってフィルム中(−面
ンの滑剤周辺を暴露し、少な(とも50個の固体微粒子
の長径とボイドの長径を測定し、次式 で求めるボイド比の数平均値で表わす。
(3) Void ratio According to the method of tll-2) above, expose the area around the lubricant in the film, measure the long axis of 50 solid particles and the long axis of the void, and calculate the void ratio using the following formula. Expressed as the numerical average value.

(4)フィルムの摩擦係数(μk) 温度20℃、湿度60%の環境で、巾1/2インチに裁
断したフィルムを、固定棒(表面粗さ0.3μ麓)に角
度θ=152/180にラジアン(152°)で接触さ
せて毎分200αの速さで移動(摩!11)させる。入
口テンションT1が35/どなるようにテンションコン
トローラーをdA榮した時の出口テンション、(TJ:
y)tフィルムが90m送行したのちに出ロテンション
慣出機で検出し1次式で走行摩擦係数μkft算出する
(4) Film friction coefficient (μk) In an environment with a temperature of 20°C and a humidity of 60%, a film cut to a width of 1/2 inch is placed on a fixed rod (surface roughness 0.3μ) at an angle θ = 152/180. It is brought into contact with radians (152°) and moved at a speed of 200α per minute (mo!11). The exit tension when the tension controller is operated so that the entrance tension T1 is 35/(TJ:
y) After the t-film has traveled 90 m, the output rotation is detected by a run-in machine and the running friction coefficient μkft is calculated using a linear equation.

μに=(2,303/θ) log (Tt/ T。μ = (2,303/θ) log (Tt/T.

=0.868 log (Tt/ 35 )(5)  
削れ性 ベースフィルムの走行mlの削れ性を5段のミニスーパ
ーカレンダーを使用して評価した。
=0.868 log (Tt/35) (5)
Scrapability The scratchability of the base film in terms of running ml was evaluated using a 5-stage mini super calendar.

カレンダーはナイロンロールとスチールクールの5段カ
レンダーであり、処j!1!温度は80℃、フィルムに
がかる線圧は200 kII/CIL s フィルムス
ピードは50s/分で走行させた。
The calendar is a 5-tier calendar made of nylon rolls and steel cool, and it's amazing! 1! The temperature was 80° C., the linear pressure applied to the film was 200 kII/CIL s, and the film speed was 50 s/min.

走行フィルムは全長2000m走行させた時点でカレン
ダーのトップクーラーに付着する汚れでベースフィルム
の削れ性′ljt評価した。
The running film was run for a total length of 2,000 m, and the abrasion resistance of the base film was evaluated based on dirt adhering to the top cooler of the calendar.

(4!Pi判定ン Qfイロンー−ルの汚れ全くなし Oナイロンロールの汚れほとんどなし X ナイロンミールが非常に汚れる ××ナイaンロールがひど(汚れる (6)電磁変換特性(クロマS/N )市販の家産用V
TRを用いて50%白レベル信号(100%白レベル信
号はピーク二ッー:ピークの電圧が0.714ボルトで
ある)に、100%クロマレベル信号を′IIL*シた
信号を記録し、その再生信号をシバツクノイズメーター
Type 925 Rな用いて測定を行う。クロマS/
Hの定義はシバツクの定−に従い次の通りである。
(4! Pi Judgment Qf No stains on the iron roll O Almost no stains on the nylon roll Household V
Using the TR, record a signal obtained by adding the 100% chroma level signal to the 50% white level signal (the 100% white level signal has a peak voltage of 0.714 volts), and The reproduced signal is measured using a noise meter Type 925R. Chroma S/
The definition of H is as follows according to Sibak's definition.

ここでgs(p−p)  は白レベル信号の再生信号の
ピーク:ツー:ピークの電圧走(p−p)である。
Here, gs(p-p) is the peak-to-peak voltage run (p-p) of the reproduction signal of the white level signal.

k:8(p−p)=0.714V(p−p)また、gN
(rmm )  はりσマレベル信号の再生信号のピー
クの電圧の平方根値である。
k: 8 (p-p) = 0.714V (p-p) Also, gN
(rmm) is the square root value of the peak voltage of the reproduced signal of the beam σma level signal.

EN(rms)=AMノイズ央効値電圧(V)(7) 
 ドロップアクト 市販のドロップアウトカウンター(例えばシバツクVH
ulBZBil)にて5 p&ccX 10 dBのド
ロップアウトをカクントし、1分間のカタント畝を算出
した。
EN (rms) = AM noise median voltage (V) (7)
DropAct Commercially available dropout counters (e.g. Shibatsu VH
A dropout of 5 p & cc x 10 dB was calculated using ulBZBil), and the catant ridge for 1 minute was calculated.

(8)  スクラッチ判定 ベースフィルムIF:t/2インチ中にスリットシ、上
記(4)の**謙a#J足と同時に固定棒に152°の
角度までフィルムをかげ、20α/嵩のフィルム速度で
10m走行させ、これを50同−返した後の1/2イン
チ巾ベースフィルムの表面に入ったスクラッチの太さ、
深さ・↓ 数を総合して、久の5段I¥I判定した。
(8) Scratch judgment base film IF: slit in t/2 inch, simultaneously with the **Ken a#J leg of (4) above, shade the film to a fixed rod up to an angle of 152°, and film at a film speed of 20α/bulk. The thickness of the scratch on the surface of the 1/2 inch wide base film after running it for 10 meters and returning it 50 times.
By combining the depth and ↓ numbers, I determined Ku's 5th Dan I¥I.

く5段階判定〉 ◎ 1/2インチ叩ベースフィルムに全くスクラッチが
認められない Q172インチ巾ベースフィルムにほ とんどスクラッチが認められない Δ 1/2 インチ巾ベースフィルムにスクラッチが艷
められる。(何本か) X  l/2インチ巾ベースフィルムに太いスクラッチ
が何本か認められる。
5-level judgment> ◎ No scratches are observed on the 1/2 inch beaten base film.Q Almost no scratches are observed on the 172 inch wide base film.Δ Scratches are observed on the 1/2 inch wide base film. (Several) X Several thick scratches are observed on the 1/2 inch wide base film.

xxl/2インチ巾ベースフィルムに太く深いスクラッ
チが多数全図に認め られる。
Many thick and deep scratches are observed on the xxl/2 inch wide base film in all images.

比較例1 ジメチルテレフタレートとエチレングリコールとを、エ
ステル交換触媒として酢酸マンガンを、産金触媒として
三酸化アンチ七ンを、安定剤として亜燐酸を、更に滑剤
として平均a径0.7μm 粒径比10.Oのカオリン
を用いて常法ニヨり重合し、固有粘度(オルンクロロフ
ェノール、35℃) 0.62のポリエチレンテレフタ
ンートを得た。
Comparative Example 1 Dimethyl terephthalate and ethylene glycol were transesterified, manganese acetate was used as a transesterification catalyst, antiseptane trioxide was used as a gold-producing catalyst, phosphorous acid was used as a stabilizer, and average a diameter was 0.7 μm as a lubricant. Particle size ratio 10 .. Polyethylene terephthanate having an intrinsic viscosity (orne chlorophenol, 35° C.) of 0.62 was obtained by carrying out conventional polymerization using kaolin of O.

このポリエチレンテレフタレート≠≠手程半尋暗≠今の
ペレットを170℃、3時間乾燥後押出機ホッパーに供
給し、I@融温度280〜300℃で浴解し、この溶融
ポリマー1mのスリット状ダイを通して表面仕上げ0.
3 S程度、表面温[2000回転冷却ドラム上に形成
押出し、200μ票 の未延伸フィルムを得た。
This polyethylene terephthalate≠≠half-dark≠The present pellets were dried at 170°C for 3 hours, then supplied to the extruder hopper, and bath-melted at a melting temperature of 280-300°C. Through surface finish 0.
The film was formed and extruded on a cooling drum with a surface temperature of about 3 S and 2,000 revolutions to obtain an unstretched film of 200 μm size.

このようにして得られた未延伸フィルムを80℃にて予
熱し、更に低速、^速のa−ル間で15m上方より90
0℃の次面@度のIRヒーター1本にて加熱して3.5
倍に延伸し、急冷し、続いてステンターに供給し105
℃にて横方向に3.7倍に延伸した。得られた二軸配向
フィルムを205℃の温度で5抄閲熱固定し、厚み15
μm の熱固定二軸配向フィルムを得た。
The unstretched film thus obtained was preheated at 80°C, and further stretched 90°C from 15m above between low and high speeds.
Heated with one IR heater at 0°C to 3.5°.
Stretched to double, rapidly cooled, and then fed to a stenter 105
It was stretched 3.7 times in the transverse direction at °C. The obtained biaxially oriented film was heat-fixed at a temperature of 205°C for 5 times to a thickness of 15°C.
A heat-set biaxially oriented film of μm was obtained.

得られたフィルムはボイド比1.7であり、且つカレン
ダーでに良好であったが、スクラッチか悪く、不満足な
ものであった。このフィルムの特性を第1表に示す。
The obtained film had a void ratio of 1.7 and had good calendering properties, but was unsatisfactory with poor scratches. The properties of this film are shown in Table 1.

史に、このフィルム上に、下記組成 Co含有酸化tc粉末     1001重部エスレツ
クA(積水化学製塩叱 ビニル−rn酸ビニル共嵐合体)    10   β
ニラボラン2304(日本ボリクレ タン製ボリクレタンエラストマー)  lOム童部コa
ネートL(日本ポリウレタン製 ポリインシアネート)         5  #レシ
チン           1 #メチルエチルグトン
     75 〃メチルインプチルグトン   75
 #トルエン          75 #添加剤(潤
滑剤、シリコンw脂)0.15#を持つ磁性粉末塗料ケ
グラビアクールにより塗布し、トリターナイフにより磁
性塗料層をスムージングし、磁性ll!科の未だ乾かめ
間に常法により磁気配向させ、しかる後オープンに導び
いの磁性層を形成した172インチ巾の磁気テープを作
成した。この磁気テープの特性を第1戎に示す。
In addition, on this film, Co-containing TC oxide powder with the following composition: 1001 parts of ESLETSUKU A (Sekisui Chemical Co., Ltd.'s vinyl salt-vinyl rnate co-arashi combination) 10 β
Niboran 2304 (Nippon Polycretan elastomer) lOmu Dobeko a
Nate L (polyinsyanate manufactured by Nippon Polyurethane) 5 #Lecithin 1 #Methyl ethyl gluten 75 〃Methyl emptyl gluten 75
#Toluene 75 #Magnetic powder paint with additives (lubricant, silicone w fat) 0.15 # Apply with Kegravure Cool, smooth the magnetic paint layer with a triter knife, and magnetic ll! While the material was still dry, it was magnetically oriented using a conventional method, and then a 172 inch wide magnetic tape was prepared with an open guiding magnetic layer formed thereon. The characteristics of this magnetic tape are shown in the first panel.

比較例2 カオリンの代りに平均粒径0.6μm 9粒逆比1.5
の炭酸カルシウムを用いる以外は比較例1と同様にし℃
、ポリエチレンテレフタレートのペレットを得た。
Comparative Example 2 Instead of kaolin, average particle diameter 0.6 μm, 9-grain inverse ratio 1.5
The procedure was the same as in Comparative Example 1 except that calcium carbonate was used at ℃
, pellets of polyethylene terephthalate were obtained.

このペレットを用いて、比較例1と同様にして厚み15
μm の二軸配向フィルムを得た。このフィルムはボイ
ド比2.0であり、走行性は良いものの、カレンタ一工
程にて白粉が発生した。
Using this pellet, the thickness was 15 mm in the same manner as in Comparative Example 1.
A biaxially oriented film of μm was obtained. Although this film had a void ratio of 2.0 and had good runnability, white powder was generated in the first step of the calender.

このフィルムの特性を第1機に示す。The characteristics of this film are shown in the first machine.

更に、このフィルムを用いる以外は、比較例1と同様に
行ってffl気テープを作成した。この磁気テープの特
性を第l弐に示す。
Furthermore, an ffl air tape was prepared in the same manner as in Comparative Example 1 except for using this film. The characteristics of this magnetic tape are shown in Part 2.

比較例3 カオリンの代りに平均粒径0.6μ電 9粒径比1.5
0災酸カルシウムを用いる以外は比較例1と同様にして
、ポリエチレンテレフタレートのペレットを得た。
Comparative Example 3 Instead of kaolin, average particle size is 0.6μ, 9 particle size ratio is 1.5
Pellets of polyethylene terephthalate were obtained in the same manner as in Comparative Example 1 except that calcium oxide was used.

このペレットを用いて170℃、3時間乾燥後、押出機
ホッパーに供給し、溶融温度280C〜300℃で溶解
し、この溶融ポリマーを1絽のスリット状ダイより押出
し、次面仕上げo、asa度、次面温度20℃の回転冷
却ドラム上に形成押出し、200μ肌 の未延伸フィル
ムを得た。このようにして得られた未延伸フィルムを1
05℃に予熱し、低速ロール、高速ロール間で実質1.
5倍に延伸し、次いで40℃機度に冷却し、再度クール
列間でll0Cのロール列を約3.0秒間接触し、引き
続いて800に表向温度のコントロールされた低速クー
ルと内部を冷却水が循還させ藺速ロール間にフィルム面
上15鶏に赤外線ヒーター3本をf&直し、実質2.6
倍に延伸した。延伸したフィルムを更にステンターに供
給し、105℃にて横方向に3.5倍延伸し、厚み15
μの二411延伸フィルムを得た。このフィルムはボイ
ドが完全にはなくならず、カレンダー特性もあまり艮(
なっていない。
After drying this pellet at 170°C for 3 hours, it is supplied to an extruder hopper and melted at a melting temperature of 280°C to 300°C, and this molten polymer is extruded through a 1-hole slit-shaped die, and the next surface finish is o, asa degree. The film was formed and extruded on a rotating cooling drum with a surface temperature of 20° C. to obtain an unstretched film with a thickness of 200 μm. The unstretched film thus obtained was
Preheat to 0.5°C and maintain substantially 1.0°C between the low speed roll and high speed roll.
Stretched 5 times, then cooled to 40°C, again brought into contact with a roll row of 10°C for about 3.0 seconds between the cooling rows, and then cooled the inside with controlled slow cooling to 800°C. The water is circulated between the speed rolls and 3 infrared heaters are installed on the film surface for 15 minutes, and the actual 2.6
Stretched twice. The stretched film was further fed to a stenter and stretched 3.5 times in the transverse direction at 105°C to a thickness of 15
A μ2411 stretched film was obtained. This film does not completely eliminate voids, and its calendar properties are not very good (
is not.

更に、このフィルムを用いる以外は比較例1と同様に行
って6気テープを作成した。この磁気テープの特性をi
1表に示す。
Furthermore, a 6-layer tape was prepared in the same manner as in Comparative Example 1 except for using this film. The characteristics of this magnetic tape are i
It is shown in Table 1.

比較例4 比較例2と1er1様にして未延伸フィルムを得たが、
更KM方向の強度を高めるために70℃に表面温度をコ
ントロールされた低速ロールで未延伸フィルムを予熱し
、高速ロールとの関に赤外M(IR)ヒーターを3本設
置し、延伸WI軍4.5倍に延伸し、次いでステンター
に通し105℃に予熱してから横方向に3.51f延押
した。このフィルムはボイド比が2.5と大きく、カレ
ンダー削れもはげしく、滴足出来るものではなかった。
Comparative Example 4 An unstretched film was obtained in the same manner as Comparative Example 2 and 1er1, but
Furthermore, in order to increase the strength in the KM direction, the unstretched film is preheated with a low speed roll whose surface temperature is controlled at 70°C, and three infrared M (IR) heaters are installed between the high speed roll and the stretched film is stretched. It was stretched 4.5 times, then passed through a stenter, preheated to 105°C, and then stretched and pressed for 3.51 f in the transverse direction. This film had a high void ratio of 2.5, was severely calendered, and was not suitable for use.

更に、このフィルムを用いる以外は比較例1と同様に行
って磁気テープを作成した。この磁気テープの特性を第
1表に示す。
Furthermore, a magnetic tape was prepared in the same manner as in Comparative Example 1 except for using this film. The characteristics of this magnetic tape are shown in Table 1.

比較例5 カオリンの代りに平均粒40.4μm 9粒径比1.7
の慮化チタンを用いる以外は比較例1と同様にして、厚
み15μm のポリエチレンデレフグレートニ軸延伸フ
ィルム及び磁気テープを得た。
Comparative Example 5 Instead of kaolin, average particle 40.4 μm 9 particle size ratio 1.7
A 15 μm thick polyethylene delphate biaxially stretched film and a magnetic tape were obtained in the same manner as in Comparative Example 1, except that titanium chloride was used.

このフィルムのボイド比は1.7であり、表面平坦のた
め電特に回上出米だものの、卓島係数が尚く、カレンダ
ー削れも恣(、磁気配録媒体として満足のいくものでに
なかった。
The void ratio of this film was 1.7, and although the surface was flat and the film was particularly popular, it had a low Takushima coefficient and suffered from arbitrary calendar scraping (and was not satisfactory as a magnetic recording medium). Ta.

実施例1〜3 外は比較例1と同様に行つ℃ポリエチレンテレフタレー
トのペレットを得た。
Examples 1 to 3 The process was otherwise carried out in the same manner as in Comparative Example 1 to obtain pellets of polyethylene terephthalate.

このペレットを用いる以外は比較例1と同様に行って厚
み15μm の熱固定二軸配向ポリエステルフィルムを
得た。このフィルムの時性ヲ第1表に示す。
A heat-set biaxially oriented polyester film having a thickness of 15 μm was obtained in the same manner as in Comparative Example 1 except for using these pellets. The time characteristics of this film are shown in Table 1.

↓ 更に、このフィルムを用いる以外は比較例と同様に行っ
て磁気テープを作成した。この磁気テープの特性を第1
機に示す。
↓ Furthermore, a magnetic tape was prepared in the same manner as in the comparative example except for using this film. The first characteristic of this magnetic tape is
Shown on the machine.

^施例で得た磁気テープは、ベースフィルムがいずれも
表ml平坦であるにも拘らず凌れた滑り性を示すととも
に、表面平坦に出来ること力1ら電龜変換特性も極めて
改良され、しかもカレンダーにも傾く、割れがほとんど
認められず、従ってテープの削れから光生するD/Qも
減じ極めて曳好である。
^ The magnetic tapes obtained in the examples showed excellent slipperiness despite the fact that the base film was flat on the surface, and the electromagnetic conversion characteristics were also extremely improved due to the fact that the surface was flat. Moreover, there is almost no inclination or cracking in the calendar, and therefore, the D/Q caused by scratches on the tape is reduced, making it extremely easy to roll.

手続補正書 昭和62年6月7日Procedural amendment June 7, 1986

Claims (1)

【特許請求の範囲】 1、平均粒径が0.3〜4μmでありかつ粒径比(長径
/短径)が1.0〜1.2である球状シリカ粒子を0.
01〜1重量%分散含有させてなる二軸配向ポリエステ
ルフィルム、及び該フィルムの少くとも片面上の磁性層
からなる磁気記録媒体。 2、球状シリカ粒子の下記式で表わされる相対標準偏差
が0.5以下である特許請求の範囲第1項記載の磁気記
録媒体。 相対標準偏差=▲数式、化学式、表等があります▼ ここで、Di:個々の粒子の面積円相当径(μm)@D
@:面積円相当径の平均値▲数式、化学式、表等があり
ます▼ n:粒子の個数 を表わす。
[Scope of Claims] 1. Spherical silica particles having an average particle diameter of 0.3 to 4 μm and a particle size ratio (major axis/breadth axis) of 1.0 to 1.2 are 0.0 μm.
1. A magnetic recording medium comprising a biaxially oriented polyester film containing 0.01 to 1% by weight dispersed therein, and a magnetic layer on at least one side of the film. 2. The magnetic recording medium according to claim 1, wherein the relative standard deviation of the spherical silica particles expressed by the following formula is 0.5 or less. Relative standard deviation = ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼ Where, Di: Area circle equivalent diameter of individual particles (μm) @D
@: Average value of area circle equivalent diameter ▲ Numerical formulas, chemical formulas, tables, etc. are available ▼ n: Represents the number of particles.
JP62000547A 1987-01-07 1987-01-07 Magnetic recording medium Expired - Lifetime JPH0628099B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62000547A JPH0628099B2 (en) 1987-01-07 1987-01-07 Magnetic recording medium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62000547A JPH0628099B2 (en) 1987-01-07 1987-01-07 Magnetic recording medium

Publications (2)

Publication Number Publication Date
JPS63168818A true JPS63168818A (en) 1988-07-12
JPH0628099B2 JPH0628099B2 (en) 1994-04-13

Family

ID=11476752

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62000547A Expired - Lifetime JPH0628099B2 (en) 1987-01-07 1987-01-07 Magnetic recording medium

Country Status (1)

Country Link
JP (1) JPH0628099B2 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63317533A (en) * 1987-06-19 1988-12-26 Diafoil Co Ltd Polyester film
JPH04105922A (en) * 1990-08-27 1992-04-07 Teijin Ltd Polyester film for use in metal bonding process
EP0723259A1 (en) * 1995-01-20 1996-07-24 Cheil Synthetics Incorporation Biaxially oriented polyester films for magnetic recording media

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS55108926A (en) * 1979-02-16 1980-08-21 Teijin Ltd Oriented polyester film for magnetic tape
JPS59171623A (en) * 1983-03-18 1984-09-28 Teijin Ltd Biaxially stretched polyester film
JPS60166435A (en) * 1984-02-09 1985-08-29 Toyobo Co Ltd Oriented polyester film
JPS615431A (en) * 1984-06-19 1986-01-11 Toray Ind Inc Polyester film for magnetic recording medium
JPS61236852A (en) * 1985-04-15 1986-10-22 Toyobo Co Ltd Oriented polyester film
JPS62207356A (en) * 1986-03-07 1987-09-11 Nippon Shokubai Kagaku Kogyo Co Ltd Method of improving slipperiness
JPS62252522A (en) * 1986-04-25 1987-11-04 Toray Ind Inc Base film for magnetic recording medium
JPS63112631A (en) * 1986-10-30 1988-05-17 Teijin Ltd Biaxially oriented polyester film
JPS63247913A (en) * 1987-04-03 1988-10-14 Diafoil Co Ltd Polyester film for magnetic recording medium

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS55108926A (en) * 1979-02-16 1980-08-21 Teijin Ltd Oriented polyester film for magnetic tape
JPS59171623A (en) * 1983-03-18 1984-09-28 Teijin Ltd Biaxially stretched polyester film
JPS60166435A (en) * 1984-02-09 1985-08-29 Toyobo Co Ltd Oriented polyester film
JPS615431A (en) * 1984-06-19 1986-01-11 Toray Ind Inc Polyester film for magnetic recording medium
JPS61236852A (en) * 1985-04-15 1986-10-22 Toyobo Co Ltd Oriented polyester film
JPS62207356A (en) * 1986-03-07 1987-09-11 Nippon Shokubai Kagaku Kogyo Co Ltd Method of improving slipperiness
JPS62252522A (en) * 1986-04-25 1987-11-04 Toray Ind Inc Base film for magnetic recording medium
JPS63112631A (en) * 1986-10-30 1988-05-17 Teijin Ltd Biaxially oriented polyester film
JPS63247913A (en) * 1987-04-03 1988-10-14 Diafoil Co Ltd Polyester film for magnetic recording medium

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63317533A (en) * 1987-06-19 1988-12-26 Diafoil Co Ltd Polyester film
JPH04105922A (en) * 1990-08-27 1992-04-07 Teijin Ltd Polyester film for use in metal bonding process
JP2528204B2 (en) * 1990-08-27 1996-08-28 帝人株式会社 Polyester film for metal laminating molding
EP0723259A1 (en) * 1995-01-20 1996-07-24 Cheil Synthetics Incorporation Biaxially oriented polyester films for magnetic recording media

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