JPH04141818A - Magnetic recording medium and production thereof - Google Patents
Magnetic recording medium and production thereofInfo
- Publication number
- JPH04141818A JPH04141818A JP26399590A JP26399590A JPH04141818A JP H04141818 A JPH04141818 A JP H04141818A JP 26399590 A JP26399590 A JP 26399590A JP 26399590 A JP26399590 A JP 26399590A JP H04141818 A JPH04141818 A JP H04141818A
- Authority
- JP
- Japan
- Prior art keywords
- binder
- adsorbed
- magnetic
- crosslinking agent
- metal 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.)
- Granted
Links
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 62
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000011230 binding agent Substances 0.000 claims abstract description 73
- 239000000843 powder Substances 0.000 claims abstract description 47
- 230000005294 ferromagnetic effect Effects 0.000 claims abstract description 38
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000002835 absorbance Methods 0.000 claims abstract description 17
- 239000006229 carbon black Substances 0.000 claims abstract description 17
- 229920005749 polyurethane resin Polymers 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims description 44
- 239000002184 metal Substances 0.000 claims description 44
- 239000003973 paint Substances 0.000 claims description 24
- -1 abrasive Substances 0.000 claims description 13
- 229920006026 co-polymeric resin Polymers 0.000 claims description 8
- 239000000314 lubricant Substances 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 2
- 241000872198 Serjania polyphylla Species 0.000 claims 1
- 238000009736 wetting Methods 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 11
- 239000011347 resin Substances 0.000 abstract description 11
- 238000001179 sorption measurement Methods 0.000 abstract description 10
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract 4
- 238000007259 addition reaction Methods 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 18
- 238000000034 method Methods 0.000 description 12
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 229920001228 polyisocyanate Polymers 0.000 description 9
- 239000005056 polyisocyanate Substances 0.000 description 9
- 239000006228 supernatant Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 8
- 239000012046 mixed solvent Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 229920002635 polyurethane Polymers 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000000703 high-speed centrifugation Methods 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 240000000662 Anethum graveolens Species 0.000 description 1
- PVNIQBQSYATKKL-UHFFFAOYSA-N Glycerol trihexadecanoate Natural products CCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCC PVNIQBQSYATKKL-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- WIBFFTLQMKKBLZ-SEYXRHQNSA-N n-butyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCCCC WIBFFTLQMKKBLZ-SEYXRHQNSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
- Magnetic Record Carriers (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、磁性粉として強磁性体金属粉末を用いた塗布
型の磁気テープ、磁気ディスク等の磁気記録媒体および
その製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a magnetic recording medium, such as a coated magnetic tape or magnetic disk, using ferromagnetic metal powder as magnetic powder, and a method for manufacturing the same.
従来の技術
一般に磁気記録媒体は、磁性粉およびバインダーを主成
分とする磁性塗料をポリエチレンテレフタレート等の非
磁性支持体上に塗布、乾燥、硬化することによって製造
される。2. Description of the Related Art Magnetic recording media are generally manufactured by applying a magnetic paint containing magnetic powder and a binder as main components onto a non-magnetic support such as polyethylene terephthalate, followed by drying and curing.
近年高密度記録への要求が高まり、ビデオテープレコー
ダ（ＶＴＲ） 、オーディオ機器およびコンピュータ等
に用いられる磁気テープ、磁気ディスク等の磁気記録媒
体では、記録波長とトラック幅の微小化、磁性層ならび
に支持体の薄膜化を実現することが必要不可欠となって
きている。In recent years, the demand for high-density recording has increased, and magnetic recording media such as magnetic tapes and magnetic disks used in video tape recorders (VTRs), audio equipment, computers, etc. are becoming smaller in recording wavelength and track width, as well as magnetic layers and supports. It has become essential to realize thinner bodies.
このため従来の酸化物系磁性粉末に比べて、保磁力（Ｈ
ｃ）および飽和磁化（σＳ）が大きく、しかも微粒子化
している強磁性体金属粉末が採用されるようになってき
た。Therefore, compared to conventional oxide-based magnetic powder, coercive force (H
c) Ferromagnetic metal powders with large saturation magnetization (σS) and fine particles have come to be used.
しかしながら強磁性体金属粉末は硬度が低いため、これ
を用いた磁気記録媒体の磁性層の走行耐久性あるいは磁
性層の耐摩耗性が不充分となり、磁性層表面の傷の発生
ならびに強磁性体金属粉末の磁性層からの脱落などが起
こりやすく、その結果としてドロップアウト等の問題が
発生しやすくなった。However, since ferromagnetic metal powder has low hardness, the running durability of the magnetic layer or the wear resistance of the magnetic layer of a magnetic recording medium using this powder is insufficient, causing scratches on the surface of the magnetic layer and ferromagnetic metal powder. The powder tends to fall off from the magnetic layer, and as a result, problems such as dropouts tend to occur.
さらに磁気記録再生装置のポータプル化、カメラ一体型
ＶＴＲ等の普及により、磁気記録媒体の使用環境は、今
まで以上に幅広く、過酷なものになることが予想される
ため、磁性層の耐久性をより向上させることが極めて重
要となる。Furthermore, with the proliferation of portable magnetic recording and reproducing devices and camera-integrated VTRs, the environments in which magnetic recording media are used are expected to become wider and harsher than ever before. It is extremely important to further improve this.
そこで従来より磁性層の耐久性を改善する目的で、複数
のバインダーを使用する方法が用いられてきた。さらに
特開昭６０−１１１３２５号公報に開示されているよう
にバインダーの機械的強度（引張り強度、破断伸び）を
特定することや、特開昭６０５９５２２号公報に開示さ
れているようにバインダーの分子量（Ｍｎ）を特定する
ことが提案されている。Therefore, in order to improve the durability of the magnetic layer, a method of using a plurality of binders has been conventionally used. Furthermore, it is possible to specify the mechanical strength (tensile strength, elongation at break) of the binder as disclosed in JP-A-60-111325, and to determine the molecular weight of the binder as disclosed in JP-A-6059522. It has been proposed to specify (Mn).
発明が解決しようとする課題
しかしながら上記のように複数のバインダーを用いた方
法でしっ才も、単にバインダー個々の特性を特定するだ
けでは、バインダーの架橋剤との反応性の違い、あるい
は強磁性体金属粉末表面への吸着能力の違いなどから予
期した効果が得られない場合が多く、磁性層の耐久性を
改善する平文ては試行錯誤にたよる以外困難であるとい
う問題を有していた。Problems to be Solved by the Invention However, although the method using multiple binders as described above is effective, it is not possible to simply identify the characteristics of each binder, and it is difficult to detect differences in the reactivity of the binder with the crosslinking agent or ferromagnetic properties. In many cases, the expected effect cannot be obtained due to differences in adsorption ability to the surface of the magnetic layer, and the problem is that it is difficult to improve the durability of the magnetic layer other than through trial and error. .
本発明は、単に１つ１つのバインダーの特性を特定する
だけでなく、磁性塗料中の強磁性体金属粉末研磨剤およ
びカーボンブラックに吸着されていない非吸着バインダ
ーと架橋剤との反応率（ＮＣＯ基の吸光度変化率）を調
節することにより、塗膜強度を向上させ、磁性層の耐久
性を真に改善できる磁気記録媒体を提供しようとするも
のである。The present invention not only specifies the characteristics of each binder, but also the reaction rate (NCO The present invention aims to provide a magnetic recording medium in which the strength of the coating film can be improved and the durability of the magnetic layer can be truly improved by adjusting the absorbance change rate of the base.
さらに強磁性体金属粉末の分散性を悪化させることなく
、磁性層の耐久性（走行耐久性、スチル特性）を向上さ
せるための製造方法の提供を目的とする。Furthermore, it is an object of the present invention to provide a manufacturing method for improving the durability (running durability, still characteristics) of a magnetic layer without deteriorating the dispersibility of ferromagnetic metal powder.
課題を解決するための手段
上記の目的を達成するために本発明は、強磁性体金属粉
末表面への吸着量が１ｌ１０ｌ１／ｇ以上である塩化ビ
ニル系共重合樹脂と架橋剤（ポリイソシアネート化合物
）との反応率（ＮＧＯ基の吸光度変化率）が３０％以上
であるポリウレタン樹脂を用い、しかも磁性塗料中の強
磁性体金属粉末、研磨剤およびカーボンブラックに吸着
されていない非吸着バインダーと架橋剤との反応率が１
０％以上であること、さらに磁性塗料製造時に、上記２
種類のバインダーの添加順序を、塩化ビニル系共重合樹
脂、ポリウレタン樹脂の順とすることを必須の要件とし
て構成するものである。Means for Solving the Problems In order to achieve the above objects, the present invention provides a vinyl chloride copolymer resin and a crosslinking agent (polyisocyanate compound) whose adsorption amount on the surface of ferromagnetic metal powder is 1l10l1/g or more. A non-adsorbing binder and a cross-linking agent are used that have a reaction rate (rate of change in absorbance of NGO groups) of 30% or more with the ferromagnetic metal powder, abrasive, and carbon black in the magnetic paint. The reaction rate with
0% or more, and the above 2.
The essential requirement is that the order of addition of the different types of binders is the vinyl chloride copolymer resin and the polyurethane resin.
作用
本発明は上記した構成により、強磁性体金属粉末とバイ
ンダーとの相互作用が増大するとともに、強磁性体金属
粉末表面に吸着していないバインダーについても官能基
間（水酸基とイソシアネート基）の付加反応によって、
溶剤に不溶不融である三次元網目構造が形成されるため
、塗膜が強靭となる。Effect The present invention has the above-described structure, which increases the interaction between the ferromagnetic metal powder and the binder, and also prevents the addition of functional groups (hydroxyl groups and isocyanate groups) to the binder that is not adsorbed to the surface of the ferromagnetic metal powder. By the reaction,
A three-dimensional network structure that is insoluble and infusible in solvents is formed, making the coating tough.
さらに磁性塗料製造時に、２種類のバインダーの添加順
序を、塩化ビニル系共重合樹脂、ポリウレタン樹脂の順
とすることにより、架橋剤との反応性が良好であるポリ
ウレタン樹脂を強磁性体金属粉末表面に強く吸着固定さ
れることなく、強磁性体金属粉末表面への吸着量が多い
塩化ビニル系共重合樹脂で先に磁性粒子分散に有効な吸
着層を形成させる。Furthermore, when producing magnetic paint, by adding the two types of binders in the order of vinyl chloride copolymer resin and polyurethane resin, the polyurethane resin, which has good reactivity with the crosslinking agent, can be added to the surface of the ferromagnetic metal powder. First, an adsorption layer effective for dispersing magnetic particles is formed using a vinyl chloride copolymer resin that has a large adsorption amount on the surface of the ferromagnetic metal powder without being strongly adsorbed and fixed.
実施例 以下本発明の実施例について詳しく説明する。Example Examples of the present invention will be described in detail below.
なお実施例および比較例において、材料の各部数は強磁
性体金属粉末を１００とした場合の重量部数を示す。In the Examples and Comparative Examples, each part of the material indicates the number of parts by weight based on 100 parts of the ferromagnetic metal powder.
実施例１
強磁性体金属粉末 ・・・ １００部（
平均長軸径０．１８μ閣、平均軸比 １ ： １０）バ
インダー ■ ・・・ １０部（塩化
ビニル−酢酸ビニル共重合体樹脂）バインダー ■
・・・ ８部（ポリウレタン樹脂）
研磨剤 ・・・ ７部（α−
Ａｔｚｏ＋）
カーボンブラック ・・・ ３部潤滑
剤 ・・・ ５部ステアリン
酸 ・・・ ２部パルミチン
・・・ ２部オレイン酸−ｎ−ブチル ・
・・ １部架橋剤 ・・・
５部ポリイソシアネート化合物（日本ポリウレタン社製
：コロネートＬ）
混合溶剤 ・・・ ３００部メ
チル・エチル・ケトン（ＭＥＫ）／）ルエン／シクロヘ
キサノン＝３／２／１
上記の組成物のうち、強磁性体金属粉末およびカーボン
ブラックをプラネタリ−ミキサー（ＰＬＭ）に投入し、
まず混合溶剤３０部を用いて湿潤処理した後、バインダ
ー■、■の順に添加し、１０時間混線を行う。次に研磨
剤と混合溶剤２００部を添加し、サンドミルにより分散
を行い磁性塗料原液とした。さらに潤滑剤、架橋剤、混
合溶剤７０部を添加し、デイシルバーにて混合撹拌を行
い磁性塗料を製造した。その後、平均孔径０．４μ鋼の
フィルター（日本炉蓋製：ＨＴ−４０）により炉遇した
塗料を１０ＤＩｌｌ厚のポリエチレンテレフタレート（
ＰＥＴ）上に塗布し、配向、乾燥、スーパーカレンダー
による鏡面加工処理を施した。硬化処理を行った後、磁
性層と反対側のポリエチレンテレフタレート上にカーボ
ンブラックを主成分とするバックコート層を設け、８＋
ｍａ幅にスリットして８■ＶＴＲ用メタルテープを作成
した。Example 1 Ferromagnetic metal powder...100 parts (
Average major axis diameter 0.18μ, average axial ratio 1:10) Binder ■ ... 10 parts (vinyl chloride-vinyl acetate copolymer resin) Binder ■
... 8 parts (polyurethane resin) Abrasive ... 7 parts (α-
Atzo+) Carbon black... 3 parts Lubricant... 5 parts Stearic acid... 2 parts Palmitin
... 2-part n-butyl oleate ・
・・・ 1 part crosslinking agent ・・・
5 parts Polyisocyanate compound (manufactured by Nippon Polyurethane Co., Ltd.: Coronate L) Mixed solvent: 300 parts Methyl ethyl ketone (MEK)/) Luene/Cyclohexanone = 3/2/1 Among the above compositions, ferromagnetic material Put metal powder and carbon black into a planetary mixer (PLM),
First, after a wet treatment using 30 parts of a mixed solvent, binders ① and ② were added in this order, and the mixture was mixed for 10 hours. Next, 200 parts of an abrasive and a mixed solvent were added and dispersed using a sand mill to obtain a magnetic paint stock solution. Further, 70 parts of a lubricant, a crosslinking agent, and a mixed solvent were added, and the mixture was mixed and stirred using a day silver to produce a magnetic paint. Thereafter, the paint was treated with a 10 DIll thick polyethylene terephthalate (
PET), and subjected to orientation, drying, and mirror polishing treatment using a super calender. After the curing process, a back coat layer containing carbon black as a main component is provided on the polyethylene terephthalate on the opposite side of the magnetic layer.
An 8-inch VTR metal tape was made by slitting it to ma width.
ここで用いたバインダー■は強磁性体金属粉末表面への
吸着量が１１２■／ｇのものを用いた。The binder (2) used here had an adsorption amount of 112 /g on the surface of the ferromagnetic metal powder.
またバインダー■と架橋剤（ポリイソシアネート化合物
（日本ポリウレタン社製：コロネートＬ）との反応率（
ＮＧＯ基の吸光変化率）は３５％のものを用いた。In addition, the reaction rate between binder ■ and crosslinking agent (polyisocyanate compound (manufactured by Nippon Polyurethane Co., Ltd.: Coronate L)
The absorbance change rate of NGO group used was 35%.
また、磁性塗料中の強磁性体金属粉末研磨剤およびカー
ボンブラックに吸着されていない非吸着バインダーと架
橋剤との反応率は１２％であった。Further, the reaction rate between the crosslinking agent and the non-adsorbed binder that was not adsorbed to the ferromagnetic metal powder abrasive and carbon black in the magnetic paint was 12%.
実施例２
実施例１でのバインダーおよび架橋剤の代わりに
バインダー■ ・・・ ９部バインダー
■
（ポリウレタン樹脂）
架橋剤
９部
４部
を用い、その添加方法をバインダー■、■の順とする以
外は実施例１と同様な方法により、８ｍＶＴＲ用メタル
テープを作成した。Example 2 Instead of the binder and crosslinking agent in Example 1, binder ■ ... 9 parts Binder ■ (polyurethane resin) 9 parts and 4 parts of crosslinking agent were used, except that the addition method was in the order of binder ■ and ■ An 8 m VTR metal tape was prepared in the same manner as in Example 1.
ここで用いたバインダー■は強磁性体金属粉末表面への
吸着量が１２７■／ｇのものを用いた。The binder (2) used here had an adsorption amount of 127 /g on the surface of the ferromagnetic metal powder.
またバインダー■と架橋剤（ポリイソシアネート化合物
）武田薬品工業社製：タケネー）Ｄ−１６ＯＮ））との
反応率（ＮＧＯ基の吸光度変化率）は３３％のものを用
いた。Further, the reaction rate (rate of change in absorbance of NGO group) between the binder (1) and the crosslinking agent (polyisocyanate compound, manufactured by Takeda Pharmaceutical Co., Ltd.: D-16ON) was 33%.
また磁性塗料中の強磁性体金属粉末、研磨剤およびカー
ボンブラックに吸着されていない非吸着バインダーと架
橋剤との反応率は１１％であった。Furthermore, the reaction rate between the crosslinking agent and the non-adsorbed binder that was not adsorbed to the ferromagnetic metal powder, abrasive, and carbon black in the magnetic paint was 11%.
比較例１
実施例１でのバインダーの代わりに
バインダー■ ・・・ １部部く塩化ビ
ニル−酢酸ビニル共重合体樹脂〉バインダー■
・・・ ８部〈ポリウレタン樹脂〉
を用い、その添加方法をバインダー■、■の順とする以
外は実施例１と同様な方法により、８■■ＴＲ用メタル
テープを作成した。Comparative Example 1 Instead of the binder in Example 1, binder ■ ... 1 part vinyl chloride-vinyl acetate copolymer resin> Binder ■
... An 8■■TR metal tape was prepared in the same manner as in Example 1, except that 8 parts of polyurethane resin were used and the binders were added in the order of ① and ②.
ここで用いたバインダー■は強磁性体金属粉末表面への
吸着量が１１２■／ｇのものを用いた。The binder (2) used here had an adsorption amount of 112 /g on the surface of the ferromagnetic metal powder.
またバインダー■と架橋剤（ポリイソシアネート化合物
）日本ポリウレタン社製：コロネートＬ））との反応率
（ＮＧＯ基の吸光度変化率は１６％のものを用いた。Further, the reaction rate of the binder (1) and the crosslinking agent (polyisocyanate compound manufactured by Nippon Polyurethane Co., Ltd.: Coronate L) (the rate of change in absorbance of the NGO group was 16%) was used.
また磁性塗料中の強磁性体金属粉末、研磨剤およびカー
ボンブラックに吸着されていない非吸着バインダーと架
橋剤との反応率は４％であった。Furthermore, the reaction rate between the crosslinking agent and the non-adsorbed binder that was not adsorbed to the ferromagnetic metal powder, abrasive, and carbon black in the magnetic paint was 4%.
比較例２
実施例１でのバインダーの代わりに
バインダー■ ・・・ １０部バインダ
ー■ ・・・ ８部〈ポリウレタン樹脂
〉
を用い、その添加方法をバインダー■、■の順とする以
外は実施例１と同様な方法により８ ｍ Ｖ ＴＲ用メ
タルテープを作成した。Comparative Example 2 Example 1 except that binder ■ ... 10 parts binder ■ ... 8 parts (polyurethane resin) was used instead of the binder in Example 1, and the addition method was in the order of binder ■ and ■. An 8 m VTR metal tape was prepared in the same manner as above.
ここで用いたバインダー■は強磁性体金属粉末表面への
吸着量が１０４■／ｇのものを用いた。The binder (2) used here had an adsorption amount of 104 /g on the surface of the ferromagnetic metal powder.
またバインダー■と架橋剤（ポリイソシアネート化合物
（日本ポリウレタン社製：コロネートＬ））との反応率
（ＮＧＯ基の吸光度変化率）は３５％であった。The reaction rate (rate of change in absorbance of NGO group) between the binder (1) and the crosslinking agent (polyisocyanate compound (Coronate L, manufactured by Nippon Polyurethane Co., Ltd.)) was 35%.
また磁性塗料中の強磁性体金属粉末、研磨剤およびカー
ボンブラックに吸着されていない非吸着バインダーと架
橋剤との反応率は１４％であった。Furthermore, the reaction rate between the crosslinking agent and the non-adsorbed binder that was not adsorbed to the ferromagnetic metal powder, abrasive, and carbon black in the magnetic paint was 14%.
比較例３
実施例１でのバインダーの添加方法をバインダー■、■
の順に変更する以外は実施例１と同様な方法により、８
ｍ Ｖ Ｔ Ｒ用メタルテープを作成した。Comparative Example 3 The method of adding binder in Example 1 was changed to binder ■, ■
8 by the same method as in Example 1 except for changing the order of
A metal tape for VTR was created.
この場合、磁性塗料中の強磁性体金属粉末、研磨剤およ
びカーボンブラックに吸着されていない非吸着バインダ
ーと架橋剤との反応率は５％であった。In this case, the reaction rate between the crosslinking agent and the non-adsorbed binder that was not adsorbed to the ferromagnetic metal powder, abrasive, and carbon black in the magnetic paint was 5%.
比較例４
実施例２でのバインダー添加方法をバインダーので括投
入（バインダー■、■の同時添加）に変更する以外は実
施例２と同様な方法により、８ｍＶＴＲ用メタルテープ
を作成した。Comparative Example 4 An 8 m VTR metal tape was prepared in the same manner as in Example 2, except that the binder addition method in Example 2 was changed to adding the binder all at once (binders ① and ① were added simultaneously).
二の場合磁性塗料中の強磁性体金属粉末、研磨剤および
カーボンブラックに吸着されていない非吸着バインダー
と架橋剤との反応率は８％であった。In case 2, the reaction rate between the crosslinking agent and the non-adsorbed binder that was not adsorbed to the ferromagnetic metal powder, abrasive and carbon black in the magnetic paint was 8%.
上記した強磁性体金属粉末表面に吸着するバインダー量
（吸着バインダー量）の測定方法、ならびにポリウレタ
ン樹脂と架橋剤（ポリイソシアネート化合物）との反応
率（ＮＧＯ基の吸光度変化率）の測定方法、および磁性
塗料中の強磁性体金属粉末、研磨剤およびカーボンブラ
ックに吸着されていない非吸着バインダーと架橋剤との
反応率ＣＮＣ０基の吸光度変化率）の測定方法を以下に
示す。A method for measuring the amount of binder adsorbed on the surface of the ferromagnetic metal powder (amount of adsorbed binder), and a method for measuring the reaction rate (rate of change in absorbance of NGO groups) between the polyurethane resin and the crosslinking agent (polyisocyanate compound), and The method for measuring the reaction rate (rate of change in absorbance of CNC0 group) between the crosslinking agent and the non-adsorbed binder that is not adsorbed to the ferromagnetic metal powder, abrasive, and carbon black in the magnetic paint is shown below.
（１）強磁性体金属粉末表面に吸着するバインダー量（
吸着バインダー量）
５抛ｌのポリ容器に強磁性体金属粉末１０ｇ、バインダ
ー（塩化ビニル系共重合樹脂）２ｇ、混合溶剤（ＭＥＫ
／）ルエン／シクロヘキサノン＝３／２／ １ ） 、
３ｍｒａφのＳＵＳビーズを投入しくこの際、固形分
濃度を３０％に設定する。）シェイカーを用いて４時間
振とうさせ、磁性塗料を調整する。(1) Amount of binder adsorbed on the surface of ferromagnetic metal powder (
Adsorption binder amount) 10 g of ferromagnetic metal powder, 2 g of binder (vinyl chloride copolymer resin), mixed solvent (MEK
/) Luene/cyclohexanone = 3/2/1),
SUS beads of 3 mraφ are introduced, and at this time, the solid content concentration is set to 30%. ) Shake using a shaker for 4 hours to adjust the magnetic paint.
次に別の５０ｍ ｌのポリ容器に、分散終了後の塗料１
０ｇと混合溶剤（ＭＥＫ／トルエン／シクロへキサノン
＝３／２／１）２０ｇを投入し、シエイカーを用いて１
５分搬上うさせる。その後、この希釈塗料を遠心骨Ｒ（
４Ｘ１０”ｒｐｍの条件にて３０分）する。Next, put paint 1 after dispersion into another 50ml plastic container.
0g and 20g of mixed solvent (MEK/toluene/cyclohexanone = 3/2/1), and use a shaker to
Let it rise for 5 minutes. Then, apply this diluted paint to the distal bone R (
30 minutes at 4×10” rpm).
さらに遠心分離後の上澄み液を遠心管に採取し、高速遠
心分離（２Ｘ １０’ｒｐｍの条件にて２時間）を行う
。高速遠心分層後の上澄み液１０１をアルミカップに採
取し、その重量を測定する。次にこの上澄み液をホット
プレート上で蒸発乾固させ、再度重量を測定する。以上
の操作より、上澄み液中のバインダー量（非吸着バイン
ダー量）が算出でき、総バインダー量（配合バインダー
量）からこの上澄み液中のバインダー量（非吸着バイン
ダー量を差し引いたバインダー量を強磁性体金属粉末表
面に吸着しているバインダー量（吸着バインダー量）と
した。Furthermore, the supernatant liquid after centrifugation is collected into a centrifuge tube and subjected to high-speed centrifugation (2 hours at 2×10'rpm). The supernatant liquid 101 after high-speed centrifugation is collected into an aluminum cup, and its weight is measured. Next, this supernatant liquid is evaporated to dryness on a hot plate, and the weight is measured again. Through the above operations, the amount of binder in the supernatant liquid (amount of non-adsorbed binder) can be calculated. The amount of binder adsorbed on the surface of the body metal powder (adsorbed binder amount) was defined as the amount of binder adsorbed on the surface of the body metal powder.
（２）ポリウレタン樹脂と架橋剤（ポリイソシアネート
化合物）との反応率（ＮＧＯ基の吸光度変化率）
５０ｍ ｌのポリ容器に、ポリウレタン樹脂１０ｇ、架
橋剤２ｇ、混合溶剤（ＭＥＫ／トルエン／シクロヘキサ
ノン＝３／２／１） 、３＋ｍａφのＳＵＳビーズを投
入しくこの際、樹脂溶液の固形濃度を２０％に設定する
。）、シェイカーを用いて１５分搬上うさせる。次に２
ｔｓｉｌのブレードにて、樹脂塗膜（クリアー塗膜）を
作製する。乾燥直後の樹脂塗膜をマグネチックホルダー
にセットし、フーリエ変換赤外分光分析装置（ＦＴ−Ｉ
Ｒ）により２２７０Ｃ１ｌ刊〜２２８０ｃｍ−’に存
在するＮＧＯ基の吸収スペクトルの吸光度を測定する。(2) Reaction rate between polyurethane resin and crosslinking agent (polyisocyanate compound) (rate of change in absorbance of NGO group) In a 50ml polyethylene container, 10g of polyurethane resin, 2g of crosslinking agent, and mixed solvent (MEK/toluene/cyclohexanone = 3 /2/1), 3+maφ SUS beads are introduced, and at this time, the solid concentration of the resin solution is set to 20%. ), and let it rise for 15 minutes using a shaker. Next 2
A resin coating film (clear coating film) is produced using a tsil blade. Immediately after drying, the resin coating was placed in a magnetic holder and placed in a Fourier transform infrared spectrometer (FT-I).
R) to measure the absorbance of the absorption spectrum of the NGO group present at 2270 C1l~2280 cm-'.
さらに６０℃×２４時間の熱処理（硬化処理）を行った
樹脂塗膜について、同様の・測定を行う。以上の測定結
果より、ポリウレタン樹脂と架橋剤（ポリイソシアネー
ト化合物）との反応率（ＮＧＯ基の吸光度変化率）を算
出する。Furthermore, similar measurements are performed on a resin coating film that has been heat treated (hardening treatment) at 60° C. for 24 hours. From the above measurement results, the reaction rate (rate of change in absorbance of NGO group) between the polyurethane resin and the crosslinking agent (polyisocyanate compound) is calculated.
（３）磁性塗料を遠心分離した後の上澄み液中に含有す
るバインダーと架橋剤との反応率（ＮＧＯ基の吸光度変
化率）
５０ｍ ｌのポリ容器に各実施例、比較例にて調整した
１０ｇと混合溶剤（ＭＥＫ／）ルエン／シクロヘキサノ
ン＝３／２／１）２０ｇを投入し、シェイカーを用いて
１５分搬上うさせる。その後、この希釈塗料を遠心分離
（４Ｘ １１０３ｒｐの条件にて３０分）する。さらに
遠心分離後の上澄み液を遠心管に採取し、高速遠心骨ｊ
ｅ！ （２Ｘ ＩＯ’ｒｐｔａの条件にて２時間）を行
う。高速遠心分離後の上澄み液をスポイトを用いて採取
し、２ ａｉｌのブレードにて、樹脂塗膜を作製する。(3) Reaction rate between the binder and crosslinking agent contained in the supernatant liquid after centrifuging the magnetic paint (rate of change in absorbance of NGO groups) 10 g prepared in each example and comparative example in a 50 ml plastic container and 20 g of a mixed solvent (MEK/) luene/cyclohexanone = 3/2/1) and stirred for 15 minutes using a shaker. Thereafter, this diluted paint is centrifuged (30 minutes at 4×1103 rpm). Furthermore, the supernatant liquid after centrifugation was collected into a centrifuge tube, and the supernatant liquid was collected into a centrifuge tube and
e! (2 hours under 2X IO'rpta conditions). The supernatant liquid after high-speed centrifugation is collected using a dropper, and a resin coating film is produced using a 2-ail blade.
乾燥直後の樹脂塗膜をマグネチックホルダーにセットし
、フーリエ変換赤外分光分析装置（ＦＴ−ＩＲ）により
、２２７０ｃｍ−’〜２２８０ｃｍ伺に存在するＮＧＯ
基の吸収スペクトルの吸光度を測定する。さらに６０°
Ｃ×２４時間の熱処理（硬化処理）を行った樹脂塗膜に
ついて、同様の測定を行う。以上の測定結果より、磁性
塗料を遠心分離した後の上澄み液中に含有するバインダ
ーと架橋剤との反応率（ＮＧＯ基の吸光度変化率）を算
出する。Immediately after drying, the resin coating was set in a magnetic holder, and a Fourier transform infrared spectrometer (FT-IR) was used to detect NGOs existing at a distance of 2270 cm to 2280 cm.
Measure the absorbance of the absorption spectrum of the group. Another 60°
Similar measurements are performed on a resin coating film that has been heat treated (hardening treatment) for C×24 hours. From the above measurement results, the reaction rate (rate of change in absorbance of NGO groups) between the binder and crosslinking agent contained in the supernatant liquid after centrifuging the magnetic paint is calculated.
以上の実施例および比較例にて得られた各８ｍＶＴＲメ
タルテープについて以下の測定を行った。The following measurements were performed on each of the 8m VTR metal tapes obtained in the above Examples and Comparative Examples.
（１） Ｃ／Ｎ （５，０ＭＨｚ／４．５ ＭＨｚ
）５．０ＭＨｚにおける信号と４．５ＭＨｚにおけるノ
イズの比を測定した。Ｃ／Ｎ測定用８ｗｔｎ Ｖ Ｔ
ＲとしてＭＶＳ−５０００（ＫＯＤＡＫ社製）を用いた
。(1) C/N (5.0MHz/4.5MHz
) The ratio of the signal at 5.0 MHz to the noise at 4.5 MHz was measured. 8wtn V T for C/N measurement
MVS-5000 (manufactured by KODAK) was used as R.
また記録再生ヘッドはアモルファス合金を使用し、実施
例１の８ＩＩＩＩＩＶＴＲ用メタルテープのＣ／Ｎを基
準（ＯｄＢ）として相対値にて示した。Further, the recording/reproducing head used an amorphous alloy, and the C/N of the 8IIIVTR metal tape of Example 1 was used as a reference (OdB), and relative values are shown.
（２） ドロップアウト
Ｃ／Ｎ測定用と同様の８ ｍ Ｖ Ｔ Ｒを用い、各ビ
デオテープ試料を４０°Ｃ−８０％ＲＨの環境下で２０
０パス走行させる（耐久試験）。耐久試験前後の各ビデ
オテープ試料について、１５μｓにわたって１６ｄＢ以
上の出力低下が発生する１分間あたりの個数を測定した
。(2) Using an 8 m VTR similar to that used for dropout C/N measurement, each videotape sample was exposed to 20°C under an environment of 40°C and 80% RH.
Run 0 pass (durability test). For each videotape sample before and after the durability test, the number of pieces per minute at which an output drop of 16 dB or more occurred over 15 μs was measured.
（３）ヘッド粉付着
上記（２）による耐久試験後の磁気ヘッド、シリンダ一
部の粉付着量を顕微鏡で観察し、粉付着の程度について
の５段階評価を行った。評価として粉付着が見られず、
実用上全く問題のないものを５とし、粉付着量が多く、
実用上問題を有るものを１とした。(3) Head Powder Adhesion After the durability test according to (2) above, the amount of powder adhesion on a part of the magnetic head and cylinder was observed using a microscope, and the degree of powder adhesion was evaluated on a five-point scale. As an evaluation, no powder adhesion was observed.
A rating of 5 means that there is no practical problem at all, and there is a large amount of powder adhesion.
Items with practical problems were given a rating of 1.
（４）走行傷
上記（２ンによる耐久試験後のテープ磁性層面の走行傷
を目視で観察し、走行傷の程度についての５段階評価を
行った。評価として走行傷が見られず、実用上全く問題
のないものを５とし、走行傷が多く、実用上問題を有す
るものを１とした。(4) Running scratches The running scratches on the surface of the tape magnetic layer after the above (2-inch durability test) were visually observed, and the degree of running scratches was evaluated on a 5-grade scale. A score of 5 indicates that there is no problem at all, and a score of 1 indicates that there are many running scratches and there are practical problems.
（５）スチルライフ
スチル測定用に改造した８ｍｍ Ｖ Ｔ Ｒを用い、１
０°Ｃ１３０ｇ荷重の条件で、あらかじめ録画しておい
た静止画を再生し、その画像信号が６ｄＢ落ち込むまで
の時間を示した。次の表に上記の結果を示す。(5) Still life Using an 8mm VTR modified for still measurement, 1
A still image recorded in advance was played back under conditions of 0°C and 130g load, and the time required for the image signal to drop by 6dB is shown. The following table shows the above results.
（以下余白）
なお上記の実施例では、８ ｍ Ｖ Ｔ Ｒ用メタルテ
ープのみについて説明したが、強磁性体金属粉末を用い
た他の塗布型の磁気テープ、磁気ディスク等の磁気記録
媒体についても同様に適用できる。(Left below) In the above example, only a metal tape for an 8 m VTR was explained, but other magnetic recording media such as coated magnetic tapes and magnetic disks using ferromagnetic metal powder can also be described. The same applies.
発明の効果
以上のように本発明による磁気記録媒体は、磁性塗料中
の強磁性体粉末、研磨剤およびカーボンブラックに吸着
されていない非吸着バインダーと架橋剤との反応率が１
０％以上であり、さらに磁性塗料製造時に、これら２種
類のバインダーの添加順序を、塩化ビニル系共重合樹脂
、ポリウレタン樹脂の順とすることにより、耐久性に優
れた磁性層を有する磁気記録媒体の提供を可能とするも
のである。Effects of the Invention As described above, in the magnetic recording medium according to the present invention, the reaction rate between the crosslinking agent and the non-adsorbed binder that is not adsorbed to the ferromagnetic powder, abrasive, and carbon black in the magnetic paint is 1.
0% or more, and by adding these two types of binders in the order of vinyl chloride copolymer resin and polyurethane resin during the production of magnetic paint, a magnetic recording medium having a magnetic layer with excellent durability can be obtained. This makes it possible to provide the following.
Claims (2)
ーボンブラック、バインダー、潤滑剤、架橋剤を含む磁
性塗料を塗布して磁性層を構成する磁気記録媒体であっ
て、上記バインダーとして塩化ビニル系共重合樹脂とポ
リウレタン樹脂を用い、上記強磁性体金属粉末、研磨剤
およびカーボンブラックに吸着されないバインダー（非
吸着バインダー）と上記架橋剤との反応率（ＮＣＯ基の
吸光度変化率）が１０％以上であることを特徴とする磁
気記録媒体。(1) A magnetic recording medium in which a magnetic layer is formed by coating a magnetic paint containing ferromagnetic metal powder, an abrasive, carbon black, a binder, a lubricant, and a crosslinking agent on a nonmagnetic support, wherein the binder Using a vinyl chloride copolymer resin and a polyurethane resin, the reaction rate (rate of change in absorbance of NCO group) between the binder that is not adsorbed by the ferromagnetic metal powder, abrasive, and carbon black (non-adsorbing binder) and the crosslinking agent is determined. A magnetic recording medium characterized in that: 10% or more.
にて湿潤させた後、塩化ビニル系共重合樹脂を添加し混
練を行い、次にポリウレタン樹脂を添加し混線分散を行
い、さらに研磨剤を添加し分散を行った後、潤滑剤、架
橋剤を添加し混合撹拌を行うことにより磁性塗料とし、
上記磁性塗料中の強磁性体金属粉末、研摩剤およびカー
ボンブラックに吸着されないバインダー（非吸着バイン
ダー）と架橋剤との反応率（ＮＣＯ基の吸光度変化率）
が１０％以上とすることを特徴とする磁気記録媒体の製
造方法。(2) After wetting the ferromagnetic metal powder and carbon black with a solvent, add a vinyl chloride copolymer resin and knead it, then add a polyurethane resin and perform cross-dispersion, and then add an abrasive. After dispersing, a lubricant and a crosslinking agent are added and mixed and stirred to create a magnetic paint.
Reaction rate (rate of change in absorbance of NCO group) between the binder that is not adsorbed by the ferromagnetic metal powder, abrasive, and carbon black in the magnetic paint (non-adsorbing binder) and the crosslinking agent
1. A method for producing a magnetic recording medium, characterized in that: 10% or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2263995A JP3000650B2 (en) | 1990-10-01 | 1990-10-01 | Magnetic recording medium and method of manufacturing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2263995A JP3000650B2 (en) | 1990-10-01 | 1990-10-01 | Magnetic recording medium and method of manufacturing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04141818A true JPH04141818A (en) | 1992-05-15 |
| JP3000650B2 JP3000650B2 (en) | 2000-01-17 |
Family
ID=17397084
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2263995A Expired - Fee Related JP3000650B2 (en) | 1990-10-01 | 1990-10-01 | Magnetic recording medium and method of manufacturing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3000650B2 (en) |
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| WO2013165166A1 (en) * | 2012-04-30 | 2013-11-07 | Lg Innotek Co., Ltd. | Magnetic sheet having wireless charging radiator function, method of manufacturing the same, and wireless charging device using the same |
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|---|---|---|---|---|
| JP6083840B1 (en) * | 2015-10-22 | 2017-02-22 | 久美代 森田 | Shirt holder with portable stand collar |
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1990
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013165166A1 (en) * | 2012-04-30 | 2013-11-07 | Lg Innotek Co., Ltd. | Magnetic sheet having wireless charging radiator function, method of manufacturing the same, and wireless charging device using the same |
| CN104335299A (en) * | 2012-04-30 | 2015-02-04 | Lg伊诺特有限公司 | Magnetic sheet having wireless charging radiator function, method of manufacturing the same, and wireless charging device using the same |
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| JP3000650B2 (en) | 2000-01-17 |
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