JPH0457215A - Magnetic recording medium - Google Patents
Magnetic recording mediumInfo
- Publication number
- JPH0457215A JPH0457215A JP2165262A JP16526290A JPH0457215A JP H0457215 A JPH0457215 A JP H0457215A JP 2165262 A JP2165262 A JP 2165262A JP 16526290 A JP16526290 A JP 16526290A JP H0457215 A JPH0457215 A JP H0457215A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic
- magnetic layer
- recording medium
- magnetic recording
- resin
- 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
Links
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- 239000011230 binding agent Substances 0.000 claims abstract description 28
- 239000001257 hydrogen Substances 0.000 claims abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 3
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- 229910052736 halogen Inorganic materials 0.000 claims description 3
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- QMMJWQMCMRUYTG-UHFFFAOYSA-N 1,2,4,5-tetrachloro-3-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=C(Cl)C(Cl)=CC(Cl)=C1Cl QMMJWQMCMRUYTG-UHFFFAOYSA-N 0.000 description 2
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- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
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- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- NTXGQCSETZTARF-UHFFFAOYSA-N buta-1,3-diene;prop-2-enenitrile Chemical compound C=CC=C.C=CC#N NTXGQCSETZTARF-UHFFFAOYSA-N 0.000 description 1
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- QHIWVLPBUQWDMQ-UHFFFAOYSA-N butyl prop-2-enoate;methyl 2-methylprop-2-enoate;prop-2-enoic acid Chemical compound OC(=O)C=C.COC(=O)C(C)=C.CCCCOC(=O)C=C QHIWVLPBUQWDMQ-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 229920006217 cellulose acetate butyrate Polymers 0.000 description 1
- 229940090961 chromium dioxide Drugs 0.000 description 1
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 1
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- AYTAKQFHWFYBMA-UHFFFAOYSA-N chromium(IV) oxide Inorganic materials O=[Cr]=O AYTAKQFHWFYBMA-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229940125898 compound 5 Drugs 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 230000006866 deterioration Effects 0.000 description 1
- 125000005265 dialkylamine group Chemical group 0.000 description 1
- 125000005442 diisocyanate group Chemical group 0.000 description 1
- JXCHMDATRWUOAP-UHFFFAOYSA-N diisocyanatomethylbenzene Chemical compound O=C=NC(N=C=O)C1=CC=CC=C1 JXCHMDATRWUOAP-UHFFFAOYSA-N 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229920002457 flexible plastic Polymers 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 150000002314 glycerols Chemical class 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000004356 hydroxy functional group Chemical group O* 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- FTQWRYSLUYAIRQ-UHFFFAOYSA-N n-[(octadecanoylamino)methyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCNC(=O)CCCCCCCCCCCCCCCCC FTQWRYSLUYAIRQ-UHFFFAOYSA-N 0.000 description 1
- 125000005487 naphthalate group Chemical group 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
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- 235000021313 oleic acid Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- 125000005496 phosphonium group Chemical class 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920005670 poly(ethylene-vinyl chloride) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 150000007519 polyprotic acids Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 235000017709 saponins Nutrition 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000011115 styrene butadiene Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
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- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium group Chemical class [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
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- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229920006163 vinyl copolymer Polymers 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は非磁性支持体上に磁性層を設けた磁気記録媒体
に関し、特に広範囲の温湿度条件において走行性、耐久
性および保存安定性に優れる磁気記録媒体に関するもの
である。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a magnetic recording medium having a magnetic layer provided on a non-magnetic support, and particularly relates to a magnetic recording medium having a magnetic layer provided on a non-magnetic support. This invention relates to an excellent magnetic recording medium.
磁気記録媒体は、録音用テープ、ビデオテープあるいは
フロッピーディスクなどとして広く用いられている。磁
気記録媒体は、基本的には、強磁性粉末が結合剤（バイ
ンダー）中に分散された磁性層が非磁性支持体上に積層
されてなる。Magnetic recording media are widely used as recording tapes, video tapes, floppy disks, and the like. A magnetic recording medium basically consists of a magnetic layer in which ferromagnetic powder is dispersed in a binder, which is laminated on a non-magnetic support.
基本的に、磁気記録媒体は、電磁変換特性、走行耐久性
および走行性能などの緒特性において高いレベルにある
ことが必要とされる。殊に、最近の８ミリビデオテープ
レコーダーなどの普及に伴ない、ビデオテープは、ビデ
オ出力が高く、そして原画再生能力が優れていることな
ど特に電磁変換特性が優れているものであることが要求
されている。Basically, magnetic recording media are required to have high levels of performance, such as electromagnetic conversion characteristics, running durability, and running performance. In particular, with the recent spread of 8mm video tape recorders, video tapes are required to have particularly excellent electromagnetic conversion characteristics, such as high video output and excellent original picture playback ability. has been done.
磁気記録媒体においては、より高密度記録の要求が高ま
り、電磁変換特性を改良するためのその一つの対応手段
として磁性層の表面を平滑にすることが知られている。In magnetic recording media, there is an increasing demand for higher density recording, and it is known that one way to improve electromagnetic conversion characteristics is to smooth the surface of the magnetic layer.
また強磁性薄膜型磁気記録媒体も次世代の媒体として開
発されている。Furthermore, ferromagnetic thin film magnetic recording media are also being developed as next-generation media.
しかしながら以上のような媒体において、電磁変換特性
向上のため磁性層の表面を平滑にすると磁気記録媒体の
走行中において磁性層と装置系との接触の摩擦係数が増
大する結果、短期間の使用で磁気記録媒体の磁性層が損
傷を受け、あるいは磁性層が剥離する傾向がある。However, in the above-mentioned media, if the surface of the magnetic layer is smoothed to improve the electromagnetic conversion characteristics, the friction coefficient of the contact between the magnetic layer and the device system increases while the magnetic recording medium is running, and as a result, it becomes difficult to use it for a short period of time. The magnetic layer of the magnetic recording medium tends to be damaged or peeled off.
このような問題に対処するために磁性塗布液中に潤滑剤
を添加する方法、あるいは磁性層表面に潤滑剤を塗布す
る方法が知られている。In order to deal with such problems, methods are known in which a lubricant is added to the magnetic coating liquid or a method is applied to the surface of the magnetic layer.
潤滑剤としては従来、鉱物油、シリコンオイル、高級ア
ルコール、高級脂肪酸、脂肪酸エステル、牛脂、鯨油、
鯨油の動物油あるいは植物油などが用いられてきた。Conventional lubricants include mineral oil, silicone oil, higher alcohol, higher fatty acid, fatty acid ester, beef tallow, whale oil,
Animal oils such as whale oil or vegetable oils have been used.
上記に示す従来の潤滑剤が少ない場合には潤滑効果が低
（、効果を高めるため潤滑剤を多くすると、磁性塗膜の
機械的強度は弱くなり磁性層が削れ、削れ粉が走行性経
路を汚したり、あるいは十分なスチル再生の耐久性が得
られなかったりした。If the amount of the conventional lubricant shown above is small, the lubrication effect is low (If the amount of lubricant is increased to increase the effect, the mechanical strength of the magnetic coating will be weakened, the magnetic layer will be scraped, and the shavings will interfere with the running path). Either it got dirty, or it didn't have enough durability for still playback.
スチル再生の耐久性を向上させるためには特公昭２８−
２８３６７号、特公昭５１−３９０８１号等に開示され
るように、ステアリン酸ブチルの如き脂肪酸エステルと
ミリスチン酸の如き脂肪酸を混合して用いることが知ら
れている。しかしながらこれらの開示例を用いると高温
状態で走行させたとき摩擦が大きくなり磁気テープの走
行テンションが大きくなるという欠点が生じた。In order to improve the durability of still playback,
As disclosed in Japanese Patent Publication No. 28367, Japanese Patent Publication No. 51-39081, etc., it is known to use a mixture of a fatty acid ester such as butyl stearate and a fatty acid such as myristic acid. However, when these disclosed examples are used, there is a drawback that when the tape is run at high temperatures, friction increases and the running tension of the magnetic tape increases.
脂肪酸は単独で使用した場合は、画質の向上には有効で
あるが、滑性を得るためには、多量に用いる必要があり
、この場合には可塑化効果により磁性層が軟らかくなり
、機械的強度が低下し、スチル再生の耐久性が劣化する
欠点があった。When fatty acids are used alone, they are effective in improving image quality, but in order to obtain lubricity, it is necessary to use large amounts, and in this case, the plasticizing effect softens the magnetic layer and causes mechanical There were drawbacks such as a decrease in strength and a deterioration in the durability of still playback.
又特開平１−２４８３１５号では走行性耐久性の改良の
ため高級脂肪酸のＮ、Ｎジアルキルアミ案されている。Further, in JP-A-1-248315, N,N dialkylamides of higher fatty acids are proposed for improving running properties and durability.
しかし以下のような問題があった。However, there were the following problems.
すなわち再生出力は良好であるが低温低湿（５℃、１０
％ＲＨ）、及び高温高温（４５℃、９０％ＲＨ）で摩擦
係数が上昇する傾向があり、特に高温高温での摩擦係数
が上昇した。In other words, the playback output is good, but at low temperature and low humidity (5℃, 10℃)
%RH), and the friction coefficient tended to increase at high temperatures (45° C., 90% RH), and the friction coefficient particularly increased at high temperatures.
又特公昭５５−２２８５１号では、潤滑剤として可塑剤
的な効果を有しない高級脂肪酸のスチルンビスアミド（
ＣＮＨ−ＣＨｚ ＮＨＣ）を磁性層に用いることを提
案している。In addition, in Japanese Patent Publication No. 55-22851, styrene bisamide, a higher fatty acid that does not have a plasticizing effect as a lubricant, is used as a lubricant.
It is proposed to use CNH-CHz NHC) for the magnetic layer.
しかし低温低湿、高温高温で摩擦係数上昇は改良できな
かった。However, the increase in friction coefficient could not be improved at low temperature and low humidity, and at high temperature and high temperature.
最近ＶＴＲやパーソナルコンピューターまたはワードプ
ロセッサ用といった民生用のフレキシブルディスクドラ
イブ装置が普及・−膜化するにいたり、磁気記録媒体の
使用条件も低温下での使用、あるいは高温高湿下での使
用等広きにわたるようになってきた。従って、磁気記録
媒体は予測される種々の、条件下においてもその走行耐
久性が変動することがないような安定したものでなけれ
ばならないがこのように従来知られているような潤滑剤
では十分ではなく性能劣化するという問題があった。Recently, as flexible disk drive devices for consumer use such as VTRs, personal computers, and word processors have become popular and have become film-based, the usage conditions for magnetic recording media have also expanded, such as use at low temperatures or use at high temperatures and high humidity. It's starting to look like this. Therefore, magnetic recording media must be stable so that their running durability does not change under various expected conditions, but conventionally known lubricants are not sufficient. However, the problem was that the performance deteriorated.
また走行耐久性を向上させるための別の対策としては、
磁性層に研磨材（硬質粒子）を添加する方法が提案・実
施されているが、磁性層の走行耐久性を向上させる目的
で磁性層に研磨材を添加する場合には、研磨材を相当量
に添加しなければその添加効果が現れにくい。すなわち
、電磁変換特性・ヘッド摩耗性を犠牲にすることなく走
行耐久性を得ることは究極的には難しい。In addition, as another measure to improve running durability,
A method of adding abrasives (hard particles) to the magnetic layer has been proposed and implemented, but when adding an abrasive to the magnetic layer for the purpose of improving the running durability of the magnetic layer, it is necessary to add a considerable amount of the abrasive. If it is not added, the effect of the addition is unlikely to appear. That is, it is ultimately difficult to obtain running durability without sacrificing electromagnetic conversion characteristics and head wear resistance.
そこで本発明者らは磁性粉末塗布型や金属薄膜型の問題
点を解消するような潤滑剤について鋭意検討した結果、
尿素誘導体を磁性層に含有又は保持させることにより従
来の潤滑剤では到底達成できなかった優れた耐久性・環
境適応性を得ることができることを見出し、本発明をな
すに至ったものである。Therefore, the inventors of the present invention conducted extensive studies on lubricants that would solve the problems of magnetic powder coated type and metal thin film type lubricants.
The inventors have discovered that by containing or holding a urea derivative in the magnetic layer, it is possible to obtain excellent durability and environmental adaptability that could never be achieved with conventional lubricants, and have thus come up with the present invention.
（発明の目的）
本発明の目的は電磁変換特性に優れると共に高温高温、
低温低温のような苛酷な条件下でも常に安定した走行耐
久性が得られる磁気記録媒体を提供することである。(Object of the Invention) The object of the present invention is to provide excellent electromagnetic conversion characteristics and high-temperature,
It is an object of the present invention to provide a magnetic recording medium that can always provide stable running durability even under severe conditions such as low and low temperatures.
（発明の構成）
本発明の上記目的は非磁性支持体と該支持体上に磁性層
を設けた磁気記録媒体において、前記磁性層が下記一般
式で表わされる尿素誘導体を含有又は保持することを特
徴とする磁気記録媒体によって達成できる。(Structure of the Invention) The above object of the present invention is to provide a magnetic recording medium comprising a non-magnetic support and a magnetic layer on the support, in which the magnetic layer contains or holds a urea derivative represented by the following general formula. This can be achieved using a magnetic recording medium with special characteristics.
（一般式）
％式％
（但しＲ１は、炭素数１０以上２６以下の炭化水素基Ｒ
ｚ、Ｒａは、同じあるいは異なる水素あるいは１以上２
６以下の炭化水素基Ｒ３は、炭素数１以上２６以下の炭
化水素基）
又更に好ましくは前記磁性層は強磁性粉末と結合剤を含
み、かつ該結合剤の全樹脂のうち５ｗｔ％以上を占める
樹脂の少なくとも１種の樹脂がエポキシ基、−ＣＯＯＭ
、−０Ｈ１−ＮＲ２、ＮＲ３Ｘ、 ＳＯｓ Ｍ、
０３Ｏｚ Ｍ。(General formula) % formula % (However, R1 is a hydrocarbon group R having 10 to 26 carbon atoms
z, Ra are the same or different hydrogens or 1 or more 2
6 or less hydrocarbon group R3 is a hydrocarbon group having 1 to 26 carbon atoms) More preferably, the magnetic layer contains a ferromagnetic powder and a binder, and the binder accounts for 5 wt% or more of the total resin. At least one resin of the occupying resin is an epoxy group, -COOM
, -0H1-NR2, NR3X, SOs M,
03Oz M.
Ｐ Ｏｓ Ｍｚ 、ＯＰ Ｏｘ Ｍｚのうち少な（とも
１種の極性基（ここでＭは水素、アルカリ金属、または
置換、未置換のアンモニウムであり、一つの基の中に複
数のＭがあるときは、互いに異なってもよい。Ｘはハロ
ゲンイオンを示す。Ｒは水素又はアルキル基である。）
を樹脂１グラム当り１０−７〜１０−３当量導入した樹
脂であることを特徴とする磁気記録媒体によって達成で
きる。The least of P Os Mz and OP Ox Mz (both are one kind of polar group (here, M is hydrogen, an alkali metal, or substituted or unsubstituted ammonium, and when there is more than one M in one group) , may be different from each other. X represents a halogen ion. R is hydrogen or an alkyl group.)
This can be achieved by a magnetic recording medium characterized in that it is a resin into which 10<-7> to 10<-3> equivalents are introduced per gram of resin.
又前記磁性層が斜め蒸着による強磁性金属薄膜であるこ
とを特徴とする磁気記録媒体によって達成できる。Furthermore, this can be achieved by a magnetic recording medium characterized in that the magnetic layer is a ferromagnetic metal thin film formed by oblique deposition.
すなわち本発明の尿素誘導体の極性基である尿素基は、
酸性はカルボン酸、スルホン酸および燐酸等に比べ弱い
が、分子内で分極しているため無機材料と親和性が高い
、そのため金属材料を腐食させることなく表面に固着し
、疎水鎖の炭化水素基が表面に配向するため、良好な潤
滑性能を示す。That is, the urea group which is the polar group of the urea derivative of the present invention is
Although its acidity is weaker than that of carboxylic acids, sulfonic acids, and phosphoric acids, it has a high affinity with inorganic materials because it is polarized within the molecule.Therefore, it adheres to the surface of metal materials without corroding them, and the hydrocarbon groups in the hydrophobic chain is oriented on the surface, exhibiting good lubrication performance.
また、本発明の尿素誘導体は、塗布型磁気記録媒体の酸
性が弱いため強磁性粉末にほとんど吸着せず、かつ結合
剤と親和性があるため、表面に配向しやすい。その中で
も特に極性基含有の結合剤（バインダー）を用いた場合
、その効果を顕著に奏するものである。Further, the urea derivative of the present invention is hardly adsorbed to the ferromagnetic powder because the acidity of the coated magnetic recording medium is weak, and since it has an affinity for the binder, it is easily oriented on the surface. Among these, particularly when a polar group-containing binder is used, the effect is remarkable.
なぜなら、本発明の化合物の極性基と非常に強くインク
ラクションを持つためそのアンカー効果によって潤滑性
能を維持することが出来る。これに対してカルボン酸、
燐酸およびスルホン酸等は、強磁性粉末に強く吸着する
ため表面に出てこない。This is because it has a very strong inclination with the polar group of the compound of the present invention, and its anchoring effect allows it to maintain lubricating performance. On the other hand, carboxylic acid,
Phosphoric acid, sulfonic acid, etc. are strongly adsorbed to the ferromagnetic powder and do not come out to the surface.
このように本発明の尿素誘導体は塗布型媒体にあっては
結合剤とのインクラクション、特に結合剤の極性基との
インクラクションが強く、アンカ効果があり、かつμ値
低減効果があるため低温低湿高温高湿のような状況下で
も優れた潤滑効果を発揮し、かつその効果が持続する。As described above, the urea derivative of the present invention has a strong inclination with the binder, especially the polar group of the binder, and has an anchoring effect and a μ value reduction effect when used as a coating type medium. It exhibits an excellent lubricating effect even under conditions of low humidity, high temperature, and high humidity, and this effect lasts for a long time.
又金属薄膜型媒体にあっては本発明の尿素誘導体が分子
内分極のため無機材料との親和性が高く、一方酸性では
ないので金属を腐食せずかつ表面で配向しているため、
良好な潤滑特性を有し、その効果が持続するものである
。In addition, in the case of metal thin film type media, the urea derivative of the present invention has high affinity with inorganic materials due to intramolecular polarization, and on the other hand, since it is not acidic, it does not corrode the metal and is oriented on the surface.
It has good lubricating properties and its effect lasts for a long time.
本発明の尿素誘導体としてＲ１は、１０以上２６以下の
炭化水素基の尿素誘導体であれば、分子量、分岐構造、
不飽和結合、異性体構造によらず選択することができる
が、好ましくは、非芳香族系炭化水素基（但し、アラル
キル基等は包含される。）であり、特に、直鎖アルキル
基が好ましい。As the urea derivative of the present invention, if R1 is a urea derivative having 10 or more and 26 or less hydrocarbon groups, the molecular weight, branched structure,
Although it can be selected regardless of the unsaturated bond or isomer structure, it is preferably a non-aromatic hydrocarbon group (however, aralkyl groups, etc. are included), and straight-chain alkyl groups are particularly preferred. .
この場合、炭素数が９以下あるいは２７以上であると疎
水鎖が短すぎるあるいは長すぎるため配向しずらくなり
潤滑性を発揮しない。In this case, if the number of carbon atoms is 9 or less or 27 or more, the hydrophobic chain is too short or too long, making it difficult to orient and not exhibiting lubricity.
またＲ２については、水素あるいは１以上２６以下の炭
化水素基の尿素誘導体であれば分子量、分岐構造、不飽
和結合、異性体構造によらず選択することができるが、
好ましくは、非芳香族系炭化水素基（但し、アラルキル
基等は包含される。）であり、特に、直鎖アルキル基が
好ましい、その中でも、更に好ましくは、水素あるいは
炭素数が１以上４以下のアルキル基であるものが疎水鎖
を高密度に配向させるという観点から望ましい。Regarding R2, as long as it is hydrogen or a urea derivative of 1 to 26 hydrocarbon groups, it can be selected regardless of molecular weight, branched structure, unsaturated bond, and isomer structure.
Preferably, it is a non-aromatic hydrocarbon group (however, aralkyl group etc. are included), and straight-chain alkyl group is particularly preferable.Among these, hydrogen or a group having 1 or more and 4 or less carbon atoms is more preferable. An alkyl group is preferable from the viewpoint of highly densely oriented hydrophobic chains.
またＲ３については、１以上２６以下の炭化水素基の尿
素誘導体であれば分子量、分岐構造、不飽和結合、異性
体構造によらず選択することができるが、好ましくは、
非芳香族系炭化水素基（但し、アラルキル基等は包含さ
れる。）であり、特に、直鎖アルキル基が好ましい。そ
の中でも、更に好ましくは、炭素数が４以下あるいは炭
素数が１０以上２６以下のアルキル基であるものが疎水
鎖を高密度に配向させるという観点から望ましい。Regarding R3, it can be selected regardless of molecular weight, branched structure, unsaturated bond, or isomer structure as long as it is a urea derivative with 1 or more and 26 or less hydrocarbon groups, but preferably,
It is a non-aromatic hydrocarbon group (however, aralkyl groups and the like are included), and particularly preferred is a straight-chain alkyl group. Among these, an alkyl group having 4 or less carbon atoms or 10 or more and 26 or less carbon atoms is more preferable from the viewpoint of highly densely oriented hydrophobic chains.
またＲ４については、１以上２６以下の炭化水素基の尿
素誘導体であれば分子量、分岐構造、不飽和結合、異性
体構造によらず選択することができるが、好ましくは、
非芳香族系炭化水素基（但し、アラルキル基等は包含さ
れる。）であり、特に、直鎖アルキル基が好ましい。そ
の中でも、更に好ましくは、炭素数が４以下あるいは炭
素数が１０以上２６以下のアルキル基であるものが疎水
鎖を高密度に配向させるという観点から望ましい。Regarding R4, it can be selected regardless of molecular weight, branched structure, unsaturated bond, or isomer structure as long as it is a urea derivative with 1 or more and 26 or less hydrocarbon groups, but preferably,
It is a non-aromatic hydrocarbon group (however, aralkyl groups and the like are included), and particularly preferred is a straight-chain alkyl group. Among these, an alkyl group having 4 or less carbon atoms or 10 or more and 26 or less carbon atoms is more preferable from the viewpoint of highly densely oriented hydrophobic chains.
また全体の炭素数としては４４以下が好ましい。Further, the total number of carbon atoms is preferably 44 or less.
４４以上だと溶剤及びバインダーへの熔解性が悪くなる
ため表面に析出したり、また配向しすらくなり潤滑性を
発揮しづらくなるからである。This is because if it is 44 or more, the solubility in solvents and binders becomes poor, so that it may precipitate on the surface or become oriented, making it difficult to exhibit lubricity.
具体的には
ＣＨ，Ｃ）Ｉｃ８． ０
／
３Ｃ
ＣＨ２
φ Ｏ
ＨｔＧＨｚ
ＣＨｓ（ＣＨｚ）＋ｓ
Ｃ８゜
ＣＨ，化合物５
これらの化合物はたとえばモノあるいはジ塩化アルキル
カルバモイルを溶剤（アルコール−アセトン、アルコー
ル−ベンゼン、アルコール−ベンゼンＭＥＫ等）に溶か
し、モノあるいはジアルキルアミンをそのままあるいは
溶剤（アルコール、ＭＥＫ）に溶かしたものを塩化アン
モニウムの沈澱が生じなくなるまで、滴下、混合したあ
と濾別し、溶剤（ＭＥＫ、ベンゼン）で抽出後、再結晶
することにより得ることが出来る。Specifically, CH, C) Ic8. 0 / 3C CH2 φ O HtGHz CHs(CHz)+s C8°CH, Compound 5 These compounds can be prepared by dissolving, for example, mono- or di-alkylcarbamoyl chloride in a solvent (alcohol-acetone, alcohol-benzene, alcohol-benzene MEK, etc.). Alternatively, dialkylamine as it is or dissolved in a solvent (alcohol, MEK) is added dropwise until no ammonium chloride precipitates occur, mixed, filtered, extracted with a solvent (MEK, benzene), and then recrystallized. You can get it.
使用量は通常の塗布型磁気記録媒体の磁性層に内添する
場合、強磁性粉末に対して０．１〜８重量％が適当であ
る。塗布型磁気記録媒体の磁性層の表面にトップコート
する場合は２〜５０ｗｇ／ｃｄが適当である。When added internally to the magnetic layer of a general coated magnetic recording medium, the appropriate amount is 0.1 to 8% by weight based on the ferromagnetic powder. When topcoating the surface of the magnetic layer of a coated magnetic recording medium, a suitable amount is 2 to 50 wg/cd.
使用量がこの範囲をこえると表面の、尿素誘導体が過剰
になり、貼りつき、吸湿等の故障の原因になることがあ
るだけでな（、内添型の場合磁性層バインダーを可塑化
する作用により却って耐久性が低下する等の問題がある
。If the amount used exceeds this range, there will be an excess of urea derivative on the surface, which may cause problems such as sticking and moisture absorption. However, there are problems such as a decrease in durability.
使用量がこの範囲を下まわると当然のことながら表面量
が不十分となり効果が得られない。If the amount used is below this range, the surface amount will be insufficient and no effect will be obtained.
本発明においては、その他の潤滑剤を混在させてもよい
。In the present invention, other lubricants may be mixed.
併用できる潤滑剤としては、飽和、不飽和の脂肪酸（ミ
リスチン酸、ステアリン酸、オレイン酸等）金属石鹸、
Ｎ置換・Ｎ未置換の脂肪酸アミド、脂肪酸エステル（各
種モノエステルをはじめソルビタン、グリセリン、等多
価エステルの脂肪酸エステル、多塩基酸のエステル化物
等）、エーテル結合を有するエステル化合物、高級脂肪
族アルコール、モノアルキルフォスフェート、ジアルキ
ルフォスフェート、トリアル牛ルフォスフェート、パラ
フィン類、シリコーンオイル、動植物油、鉱油、高級脂
肪族アミン；グラファイト、シリカ、二硫化モリブデン
、二硫化タングステン等の無機微粉末；ポリエチレン、
ポリプロピレン、ポＩＪＪＩ化ビニル、エチレン−塩化
ビニル共重合体、ポリテトラフルオロエチレン等の樹脂
微粉末；αオレフイン重合物；常温で液体の不飽和脂肪
族炭化水素、末端変性または未変性のパーフルオロアル
キルポリエーテル、フルオロカーボン類等があげられる
。Lubricants that can be used in combination include saturated and unsaturated fatty acids (myristic acid, stearic acid, oleic acid, etc.), metal soaps,
N-substituted/N-unsubstituted fatty acid amides, fatty acid esters (including various monoesters, sorbitan, glycerin, fatty acid esters of polyesters such as glycerin, esters of polybasic acids, etc.), ester compounds with ether bonds, higher aliphatic alcohols , monoalkyl phosphate, dialkyl phosphate, trial bovine sulfate, paraffins, silicone oil, animal and vegetable oils, mineral oil, higher aliphatic amines; inorganic fine powders such as graphite, silica, molybdenum disulfide, tungsten disulfide; polyethylene ,
Resin fine powder such as polypropylene, polyvinyl chloride, ethylene-vinyl chloride copolymer, polytetrafluoroethylene; α-olefin polymer; unsaturated aliphatic hydrocarbon that is liquid at room temperature, terminally modified or unmodified perfluoroalkyl Examples include polyether and fluorocarbons.
これらの混在潤滑剤の好ましい使用量は使用態様によっ
て様々だが、おおむね、本発明の尿素誘導体の１／１０
〜２倍の使用量である。The preferred amount of these mixed lubricants to be used varies depending on the mode of use, but is generally 1/10 of the amount of the urea derivative of the present invention.
~2 times the amount used.
本発明において、尿素誘導体を磁性層に保持させる方法
としては、磁性層に含有させる方法と表面にトップコー
ト（材料を有機溶剤に溶解して基板に塗布あるいは噴霧
したのち乾燥する方法、材料を熔融して基板に塗着させ
る方法、有＃ｌ溶剤に材料を溶解した溶液に基板を浸漬
して材料を基板表面に吸着させる方法、ラングミュア−
プロジェット法などによる）する方法がある。In the present invention, methods for retaining the urea derivative in the magnetic layer include a method in which the urea derivative is contained in the magnetic layer, a method in which the surface is topcoated (a method in which the material is dissolved in an organic solvent, applied or sprayed on the substrate, and then dried, and a method in which the material is melted and A method of adsorbing the material to the substrate surface by immersing the substrate in a solution of the material dissolved in #1 solvent, a method of adsorbing the material to the substrate surface,
There are methods to do this (such as the project method).
本発明に用いられる強磁性粉末としては、強磁性酸化鉄
粉末、Ｃｏドープの強磁性酸化鉄粉末、強磁性二酸化ク
ロム粉末、強磁性金属粉末、強磁性合金粉末、バリウム
フェライトなどが使用できる。As the ferromagnetic powder used in the present invention, ferromagnetic iron oxide powder, Co-doped ferromagnetic iron oxide powder, ferromagnetic chromium dioxide powder, ferromagnetic metal powder, ferromagnetic alloy powder, barium ferrite, etc. can be used.
強磁性合金粉末の例としては、金属分が７５−ｔ％以上
であり、金属分の１３Ｑｗｔ％以上が少なくとも一種類
の強磁性金属あるいは合金（Ｆｅ。An example of a ferromagnetic alloy powder is one in which the metal content is 75-t% or more, and 13 Qwt% or more of the metal content is at least one ferromagnetic metal or alloy (Fe).
Ｃｏ、Ｎｉ、Ｆｅ−Ｃｏ Ｆｅ−Ｎｉ Ｃｏ −Ｎ
ｉ、Ｇｏ−Ｆｅ−Ｎｉなど）であり、該金属分の２０ｗ
ｔ％以下で他の成分（ＡＩ、Ｓｉ、ＳＳｃ、Ｔｉ、Ｖ、
Ｃｒ、Ｍｎ、Ｃｕ、Ｚｎ、Ｙ。Co, Ni, Fe-Co Fe-Ni Co -N
i, Go-Fe-Ni, etc.), and the metal content is 20w
Other components (AI, Si, SSc, Ti, V,
Cr, Mn, Cu, Zn, Y.
Ｍｏ、Ｒｈ、Ｐｄ、Ａｇ、Ｓｎ、Ｓｂ、Ｂ、Ｂａ。Mo, Rh, Pd, Ag, Sn, Sb, B, Ba.
Ｔａ、Ｗ、Ｒｅ、Ａｕ、Ｈｇ、Ｐｂ、Ｐ、Ｌａ。Ta, W, Re, Au, Hg, Pb, P, La.
Ｃｅ、Ｐｒ＋ Ｎｄ、’ｌ”ｅ、Ｂｉなど）を含むもの
を挙げることができる。また、上記強磁性金属分が少量
の水、水酸化物、または酸化物を含むものであってもよ
い。The ferromagnetic metal may also contain a small amount of water, hydroxide, or oxide.
これらの強磁性粉末の製法は既知であり、本発明で用い
られる強磁性粉末についても公知の方法にしたがって製
造することができる。Methods for producing these ferromagnetic powders are known, and the ferromagnetic powder used in the present invention can also be produced according to known methods.
強磁性粉末の形状・サイズは特に制限なく広く用いるこ
とができる。形状としては針状、米粒状、球状、立方体
状、板状等いずれでもよいが針状、板状が電磁変換特性
上好ましい。結晶子サイズ、比表面積もとくに権限はな
いが、結晶子サイズで４００Ａ以下、Ｓ ＢＥＴで３Ｏ
ｎ？／ｇ以上が好ましい。強磁性粉末のｐＨ１表面処理
はとくに制限なく用いる事ができる（チタン、珪素、ア
ルミニウム等の元素を含む物質で表面処理されていても
よいし、カルボン酸、スルホン酸、硫酸エステル、ホス
ホン酸、燐酸エステル、ベンゾトリアゾール等の含窒素
複素環をもつ吸着性化合物の様な有機化合物で処理され
ていてもよい。好ましいｐＨの範囲は５〜１０である０
強磁性酸化鉄微粉末の場合、２価の鉄／３価の鉄の比に
特に制限されることなく用いることができる。The shape and size of the ferromagnetic powder are not particularly limited and can be widely used. The shape may be needle-like, rice-grain-like, spherical, cubic, plate-like, etc., but needle-like and plate-like are preferable from the viewpoint of electromagnetic conversion characteristics. There is no particular authority regarding crystallite size and specific surface area, but crystallite size is 400A or less, and S BET is 3O.
n? /g or more is preferable. The pH 1 surface treatment of ferromagnetic powder can be used without particular restrictions (the surface may be treated with a substance containing elements such as titanium, silicon, aluminum, etc., or it can be treated with a substance containing elements such as carboxylic acid, sulfonic acid, sulfuric acid ester, phosphonic acid, phosphoric acid). It may be treated with an organic compound such as an adsorptive compound having a nitrogen-containing heterocycle such as ester or benzotriazole.The preferred pH range is 5 to 10.
In the case of ferromagnetic iron oxide fine powder, it can be used without any particular restriction on the ratio of divalent iron/trivalent iron.
本発明に用いられる結合剤は従来、磁気記録媒体用の結
合剤として使用されている公知の熱可塑性樹脂、熱硬化
性樹脂、放射線硬化性樹脂、反応型樹脂およびこれらの
混合物を使用することができる。As the binder used in the present invention, known thermoplastic resins, thermosetting resins, radiation-curable resins, reactive resins, and mixtures thereof, which have been conventionally used as binders for magnetic recording media, can be used. can.
上記樹脂のＴｇは一４０℃〜１５０℃、重量平均分子量
は１万〜３０万、好ましくは１万〜１０万である。The above resin has a Tg of -40°C to 150°C and a weight average molecular weight of 10,000 to 300,000, preferably 10,000 to 100,000.
上記熱可塑性樹脂としては、塩化ビニル・酢酸ビニル共
重合体、塩化ビニル、酢酸ビニルとビニルアルコール、
マレイン酸および／またはアクリル酸との共重合体、塩
化ビニル・塩化ビニリデン共重合体、塩化ビニル・アク
リロニトリル共重合体、エチレン・酢酸ビニル共重合体
などのビニル系共重合体、ニトロセルロース、セルロー
スアセテートプロピオネート、セルロースアセテートブ
チレート樹脂などのセルロース誘導体、アクリル樹脂、
ポリビニルアセタール樹脂、ポリビニルブチラール樹脂
、ポリエステルポリウレタン樹脂、ポリエーテルポリウ
レタン、ポリカーボネートポリウレタン樹脂、ポリエス
テル樹脂、ポリエーテル樹脂、ポリアミド樹脂、アミン
樹脂、スチレンブタジェン樹脂、ブタジェンアクリロニ
トリル樹脂等のゴム系樹脂、シリコーン系樹脂、フッ素
系樹脂を挙げることができる。Examples of the thermoplastic resin include vinyl chloride/vinyl acetate copolymer, vinyl chloride, vinyl acetate and vinyl alcohol,
Copolymers with maleic acid and/or acrylic acid, vinyl copolymers such as vinyl chloride/vinylidene chloride copolymers, vinyl chloride/acrylonitrile copolymers, ethylene/vinyl acetate copolymers, nitrocellulose, cellulose acetate Propionate, cellulose derivatives such as cellulose acetate butyrate resin, acrylic resin,
Rubber resins such as polyvinyl acetal resin, polyvinyl butyral resin, polyester polyurethane resin, polyether polyurethane, polycarbonate polyurethane resin, polyester resin, polyether resin, polyamide resin, amine resin, styrene butadiene resin, butadiene acrylonitrile resin, silicone resin Examples include resins and fluororesins.
これらの中で、塩化ビニル系樹脂は強磁性粉末の分散性
が高く好ましい。Among these, vinyl chloride resin is preferred because it has high dispersibility of ferromagnetic powder.
上記熱硬化性樹脂または、反応型樹脂としては加熱によ
り分子量がきわめて大きくなる物で、たとえばフェノー
ル樹脂、フッ素系樹脂、エポキシ樹脂、硬化型ポリウレ
タン樹脂、尿素樹脂、メラミン樹脂、アルキッド樹脂、
シリコン樹脂、アクリル系反応樹脂、エポキシ−ポリア
ミド樹脂、ニトロセルロースメラミン樹脂、高分子量ポ
リエステル樹脂とイソシアネートプレポリマーの混合物
、尿素ホルムアルデヒド樹脂、低分子量グリコール／高
分子量ジオール／ポリイソシアネートの混合物、ポリア
ミン樹脂、およびこれらの混合物があげられる。The above-mentioned thermosetting resins or reactive resins are those whose molecular weight becomes extremely large when heated, such as phenol resins, fluorine resins, epoxy resins, curable polyurethane resins, urea resins, melamine resins, alkyd resins,
silicone resins, acrylic reactive resins, epoxy-polyamide resins, nitrocellulose melamine resins, mixtures of high molecular weight polyester resins and isocyanate prepolymers, urea formaldehyde resins, mixtures of low molecular weight glycols/high molecular weight diols/polyisocyanates, polyamine resins, and Mixtures of these can be mentioned.
上記放射線硬化型樹脂としては上記熱可塑性樹脂に放射
線硬化官能基として炭素−炭素不飽和結合を有する基を
結合させたものが用いられる。好ましい官能基としては
アクリロイル基、メタクリロイル基などがある。The radiation-curable resin used is one in which a group having a carbon-carbon unsaturated bond is bonded to the thermoplastic resin as a radiation-curable functional group. Preferred functional groups include acryloyl and methacryloyl groups.
以上列挙の結合剤分子中に、極性基（エポキシ基、−Ｃ
ＯＯＭ、−ＯＨ，−ＮＲ２、−ＮＲ，Ｘ。In the binder molecules listed above, polar groups (epoxy group, -C
OOM, -OH, -NR2, -NR,X.
Ｓ Ｏｙ Ｍ、 −ＯＳ Ｏｗｌ Ｍ、 Ｐ Ｏ
ｓ ＭｚＯＰ Ｏｓ Ｍｚ 、ただしＭは水素、アルカ
リ金属または置換、未置換のアンモニウムであり、一つ
の基の中に複数のＭがあるときは互いに異なっていても
よい、Ｘはハロゲンイオンを示す。Ｒは水素またはアル
キル基である）を導入したものが強磁性粉末の分散性、
耐久性上好ましく本発明の尿素誘導体の添加効果が顕著
に現れる。極性基の含有量としてはポリマー１グラム当
り１０−７〜１０４当量が好ましく、さらには１０−６
〜１０−４当量が好ましい範囲である。S Oy M, -OS Owl M, P O
s MzOP Os Mz , where M is hydrogen, an alkali metal, or substituted or unsubstituted ammonium, and when there is a plurality of M's in one group, they may be different from each other, and X represents a halogen ion. R is hydrogen or an alkyl group), which improves the dispersibility of ferromagnetic powder,
The effect of adding the urea derivative of the present invention, which is preferable in terms of durability, is noticeable. The content of polar groups is preferably 10-7 to 104 equivalents per gram of polymer, more preferably 10-6
A preferred range is 10-4 equivalents.
極性基の含有量としては１０−’当量未満であると相互
作用する潤滑剤量が少なくなるため均一な配向膜を形成
するのが難しくなり滑り性が低下する。また１０−３当
量より多いと結合剤の粘度が上がり分散性が低下するた
め好ましくない。If the content of polar groups is less than 10-' equivalent, the amount of lubricant that interacts with the lubricant will be small, making it difficult to form a uniform alignment film and reducing slipperiness. Moreover, if the amount is more than 10@-3 equivalent, the viscosity of the binder increases and the dispersibility decreases, which is not preferable.
以上列挙の高分子結合剤は華独または数種混合で使用さ
れ、イソシアネート系の公知の架橋剤、および／あるい
は放射線硬化型ビニル系モノマーを添加して硬化処理す
ることができる。The polymeric binders listed above can be used alone or in combination, and can be cured by adding a known isocyanate-based crosslinking agent and/or a radiation-curable vinyl monomer.
イソシアネート系架橋剤としてはイソシアネート基を２
個以上有するポリイソシアネート化合物で、たとえばト
リレンジイソシアネート、４．４′ジフエニルメタンジ
イソシアネート、ヘキサメチレンジイソシアネート、キ
シリレンジイソシアネート、ナフチレン−１，５−ジイ
ソシア第一ト、０−トルイジンジイソシアネート、イソ
ホロンジイソシアネート、トリフェニルメタンジイソシ
アネートなどのイソシアネート類、これらのイソシアネ
ート類とポリアルコールとの反応生成物、及びこれらの
イソシアネート類の縮合により生成したポリイソシアネ
ートなどをあげられる。これらのポリイソシアネートは
日本ポ、リウレタン工業■カラコロネートし、コロネー
トＨＬ、 コロネートＨ，コロネートＥＨ，コロネート
２０１４、コロ不一）２０３０、コロネート２０３１、
コロ不一）２０３６、コロネート３０１５、コロネート
３０４０、コロネート３０４１、ミリオネートＭＲ、ミ
リオネートＭＴＬ、ダルトセフク１３５０、ダルトセフ
ク２１７０、ダルトセック２２８０、武田薬品工業−か
らタケネートＤ１０２、タケネートＤＩＩＯＮ、タケネ
ートＤ２００、タケネートＤ２０２、住友バイエル■か
ら、スミジュールＮ７５、***バイエル社からデスモジ
ュール上１デスモジユールＩＬ、デスモジモユールＮ、
デスモジュールＨＬ、大日本インキ化学工業−からバー
ノックＤ８５０、バーノックＤ８０２などの商品名で市
販されている。As an isocyanate-based crosslinking agent, two isocyanate groups are used.
Polyisocyanate compounds having at least 100% diisocyanate, such as tolylene diisocyanate, 4,4' diphenylmethane diisocyanate, hexamethylene diisocyanate, xylylene diisocyanate, naphthylene-1,5-diisocyanate, 0-toluidine diisocyanate, isophorone diisocyanate, Examples include isocyanates such as phenylmethane diisocyanate, reaction products of these isocyanates and polyalcohols, and polyisocyanates produced by condensation of these isocyanates. These polyisocyanates are manufactured by Nippon Polyurethane Industry Co., Ltd., Color Coronate, Coronate HL, Coronate H, Coronate EH, Coronate 2014, Coronate 2030, Coronate 2031,
Coro Fuji) 2036, Coronate 3015, Coronate 3040, Coronate 3041, Millionate MR, Millionate MTL, Daltosefuku 1350, Daltosefuku 2170, Daltosec 2280, Takeda Pharmaceutical - Takenate D102, Takenate DIION, Takenate D200, Takenate D202, Sumitomo Bay El ■ From, Sumidur N75, Desmodulur IL, Desmodulur N from West German Bayer,
Desmodur HL is commercially available from Dainippon Ink and Chemicals under trade names such as Burnock D850 and Burnock D802.
放射線硬化ビニル糸上ツマ−としては、放射線照射によ
って重合可能な化合物であって、炭素炭素不飽和結合を
分子中に１個以上有する化合物であり、（メタ）アクリ
ル酸エステル類、（メタ）アクリルアミド類、アリル化
合物、ビニルエーテル類、ビニルエステル類、ビニル異
節環化合物、Ｎ−ビニル化合物、スチレン、（メタ）ア
クリル酸、クロトン酸、イタコン酸、オレフィン類等が
あげられる。Radiation-cured vinyl yarn threads are compounds that can be polymerized by radiation irradiation and have one or more carbon-carbon unsaturated bonds in the molecule, such as (meth)acrylic esters and (meth)acrylamide. Examples include allyl compounds, vinyl ethers, vinyl esters, vinyl heterocyclic compounds, N-vinyl compounds, styrene, (meth)acrylic acid, crotonic acid, itaconic acid, and olefins.
これらのうち好ましいものとして（メタ）アクリロイル
基を２個以上有する、ジエチレングリコールジ（メタ）
アクリレート、トリエチレングリコールジ（メタ）アク
リレート、などのポリエチレングリコールの（メタ）ア
クリレート類、トリメチロールプロパントリ （メタ）
アクリレート、ペンタエリスリトールテトラ（メタ）ア
リクレート、ジペンタエリスリトールペンタ （メタ）
アクリレート、ジペンタエリスリトールヘキサ（メタ）
アクリレート、ポリイソシアネートとヒドロキシ（メタ
）アクリレート化合物との反応物、等がある。Among these, diethylene glycol di(meth) having two or more (meth)acryloyl groups is preferable.
(meth)acrylates of polyethylene glycol such as acrylate, triethylene glycol di(meth)acrylate, trimethylolpropane tri(meth)acrylate, etc.
Acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)
Acrylate, dipentaerythritol hexa(meth)
Examples include acrylates, reaction products of polyisocyanates and hydroxy (meth)acrylate compounds, and the like.
これらの架橋剤は、架橋剤を含む全結合剤のうち５から
４５ｗｔ％含むことが好ましい。These crosslinking agents preferably comprise 5 to 45 wt% of the total binder containing crosslinking agents.
本発明の磁性層における前記全結合剤（架橋剤も含む）
の配合は強磁性粉末に対し１０〜４゜ｗｔ％、好ましく
は１５〜３Ｑｗｔ％である。結合剤の配合割合が前記範
囲より多いと強磁性微粉末の充填度が低くｉ磁変換特性
が低下し、逆に少ないと走行耐久性が低下する。All the binders (including crosslinking agents) in the magnetic layer of the present invention
The content of ferromagnetic powder is 10 to 4% by weight, preferably 15 to 3% by weight. If the blending ratio of the binder is greater than the above range, the degree of filling of the ferromagnetic fine powder will be low and the i-magnetic conversion characteristics will be degraded, whereas if it is too small, the running durability will be degraded.
非磁性支持体の材質としては、ポリエチレンテレフタレ
ート、ポリエチレン２．６ナフタレートなどのポリエス
テル類；ポリエチレン、ポリプロピレンなどのポリオレ
フィン類、セルローストリアセレートなどのセルロース
誘導体、ポリカーボネート、ポリイミド、ポリアミドイ
ミド等の樹脂を用いることができ、必要に応じアルミニ
ウム等の金属でメタライズしてあってもよいし、あるい
はアルミ箔、ステンレス箔などの金属箔であってもよい
。As the material of the non-magnetic support, polyesters such as polyethylene terephthalate and polyethylene 2.6 naphthalate; polyolefins such as polyethylene and polypropylene; cellulose derivatives such as cellulose triacerate; resins such as polycarbonate, polyimide, and polyamideimide are used. If necessary, it may be metallized with a metal such as aluminum, or may be a metal foil such as aluminum foil or stainless steel foil.
また支持体の形態はテープ、ディスク、フィルム、シー
ト、カード、ドラムなどいずれでもよく、形態に応して
種々の材料が選択される。The support may be in any form such as a tape, disk, film, sheet, card, or drum, and various materials are selected depending on the form.
非磁性支持体の厚みは３〜１００μ、磁気テープとして
は好ましくは３〜２０μ、磁気ディスクとしては２０〜
１００μが通常使用される範囲である。The thickness of the non-magnetic support is 3 to 100μ, preferably 3 to 20μ for magnetic tape, and 20 to 20μ for magnetic disk.
100μ is a commonly used range.
本発明の磁気記録媒体の磁性層には、さらに研磨剤とし
てモース硬度５以上の無りｌ賞粒子を含有することが好
ましい。Preferably, the magnetic layer of the magnetic recording medium of the present invention further contains grains having a Mohs hardness of 5 or more as an abrasive.
使用される無機質粒子は、モース硬度が５以上であれば
特に制限はない、モース硬度が５以上の無機質粒子の例
としては、Ａ Ｉ ｘ ｏｘ （モース硬度９）、Ｔ
ｉ０（同６）、ＴｉＯ，（同６．５）Ｓｉｎｇ（同７）
、５ｎＯｔ （同６．５）。The inorganic particles used are not particularly limited as long as they have a Mohs hardness of 5 or more. Examples of inorganic particles having a Mohs hardness of 5 or more include A I x ox (Mohs hardness 9), T
i0 (6), TiO, (6.5) Sing (7)
, 5nOt (6.5).
ＣｒｚＯｓ（同９）、およびαＦ ＠ｚ Ｏｓ （同
５．５）を挙げることができ、これらを単独あるいは混
合して用いることができる。Examples include CrzOs (9) and αF@zOs (5.5), which can be used alone or in combination.
とくに好ましいのはモース硬度が８以上の無機質粒子で
ある。モース硬度が５よりも低い無機質粒子を用いた場
合には、磁性層から無機質粒子が脱落しやすく、またヘ
ッドの研磨作用も殆どないため、ヘッド目詰まりを発生
しゃすく、また走行耐久性も乏しくなる。Particularly preferred are inorganic particles having a Mohs hardness of 8 or more. When inorganic particles with a Mohs hardness lower than 5 are used, the inorganic particles tend to fall off from the magnetic layer and have almost no abrasive action on the head, resulting in head clogging and poor running durability. Become.
無機質粒子の含有量は、通常、強磁性粉末１゜０重量部
に対して０．１〜２０重量部の範囲であリ、好ましくは
１〜１０重量部の範囲である。The content of the inorganic particles is usually in the range of 0.1 to 20 parts by weight, preferably in the range of 1 to 10 parts by weight, per 10 parts by weight of the ferromagnetic powder.
また磁性層には上記の無機質粒子以外にも、カーボンブ
ラック（特に、平均粒径が１０〜３００ｎｍ（ナノメー
トル；１〇−雫ｍ）のもの）などを含有させることが望
ましい。In addition to the above-mentioned inorganic particles, the magnetic layer preferably contains carbon black (particularly one having an average particle size of 10 to 300 nm (nanometers; 10-drop m)).
つぎに本発明の磁気記録媒体を製造する方法の例を述べ
る。Next, an example of a method for manufacturing the magnetic recording medium of the present invention will be described.
まず、強磁性粉末と結合剤、必要に応じて、他の充填材
、添加剤などを溶剤と混練、分散し、磁性塗料を調製す
る。混練の際に使用する溶剤としては、磁性塗料の調製
に通常使用されている溶剤を使用することができる。First, a magnetic paint is prepared by kneading and dispersing ferromagnetic powder, a binder, and, if necessary, other fillers and additives in a solvent. As the solvent used during kneading, solvents commonly used for preparing magnetic paints can be used.
混線の方法にも特に制限はなく、また各成分の添加順序
などは適宜設定することができる。There is no particular restriction on the method of cross-talk, and the order of addition of each component can be set as appropriate.
例えば、潤滑剤・添加剤や架橋剤を有ｌｌ溶剤に溶解し
たものを用意しておき、溶剤・結合剤・強磁性粉末等で
調製した強磁性粉末分散液に塗布直前に添加することも
できる。For example, it is also possible to prepare lubricants, additives, and crosslinking agents dissolved in a suitable solvent and add them to a ferromagnetic powder dispersion prepared with a solvent, binder, ferromagnetic powder, etc. immediately before coating. .
磁性塗料を調製する際には、分散剤、帯電防止剤、潤滑
剤等の公知の添加剤を併せて使用することもできる。When preparing a magnetic paint, known additives such as dispersants, antistatic agents, lubricants, etc. can also be used.
分散剤の例としては、炭素数１２〜２２の脂肪酸、その
塩またはエステル化物およびその化合物の水素の一部あ
るいは全部をフッ素原子で置換した化合物、上記の肪族
酸のアミド、脂肪族アミン、高級アルコール、ポリアル
キレンオキサイドアルキル燐酸エステル、アルキル燐酸
エステル、アルキルホウ酸エステル、サルコシネート類
、アルキルエーテルエステル類、トリアルキルポリオレ
フィン、オキシ第４級アンモニウム塩およびレシチン、
低分子エポキシ化合物などの公知の分散剤を挙げること
ができる。Examples of dispersants include fatty acids having 12 to 22 carbon atoms, salts or esters thereof, compounds in which part or all of the hydrogen atoms of these compounds are replaced with fluorine atoms, amides of the above aliphatic acids, aliphatic amines, Higher alcohols, polyalkylene oxide alkyl phosphates, alkyl phosphates, alkyl borates, sarcosinates, alkyl ether esters, trialkyl polyolefins, oxyquaternary ammonium salts, and lecithin,
Known dispersants such as low molecular weight epoxy compounds can be used.
分散剤を使用する場合は、通常は使用する強磁性粉末１
００重量部に対し、０６１〜１０重量部の範囲で使用さ
れる。When using a dispersant, the ferromagnetic powder 1 usually used is
It is used in a range of 0.61 to 10 parts by weight per 0.00 parts by weight.
帯電防止剤の例としては、カーボンブランク、カーボン
ブラックグラフトポリマーなどの導電性微粉末；サポニ
ンなどの天然界面活性剤；アルキレンオキサイド系、グ
リセリン系およびグリシドール系などのノニオン系界面
活性剤；高級アルキルアミン類、第４級アンモニウム塩
類、ピリジンその他の複素環化合物の塩類、ホスホニウ
ムまたはスルホニウム類などのカチオン性界面活性剤：
カルボン酸、燐酸、硫酸エステル基、燐酸エステル基等
の酸性基を含むアニオン性界面活性剤ニアミノ酸類、ア
ミノスルホン酸類、アミノアルコールの硫酸または燐酸
エステル類等の両性界面活性剤等を挙げることができる
。帯電防止剤として上記の導電性微粉末を使用する場合
には、例えば強磁性粉末１００重量部に対し０．１〜１
０重量部の範囲で使用され、界面活性剤を使用する場合
にも同様に０．１２〜ＩＯ重量部の範囲で使用される。Examples of antistatic agents include conductive fine powders such as carbon blanks and carbon black graft polymers; natural surfactants such as saponins; nonionic surfactants such as alkylene oxides, glycerins, and glycidols; higher alkyl amines. Cationic surfactants such as quaternary ammonium salts, salts of pyridine and other heterocyclic compounds, phosphoniums or sulfoniums:
Examples include anionic surfactants containing acidic groups such as carboxylic acid, phosphoric acid, sulfuric acid ester groups, and phosphoric ester groups; amphoteric surfactants such as diamino acids, aminosulfonic acids, and sulfuric or phosphoric esters of amino alcohols; . When using the above conductive fine powder as an antistatic agent, for example, 0.1 to 1 part by weight per 100 parts by weight of ferromagnetic powder.
It is used in a range of 0 parts by weight, and when a surfactant is used, it is similarly used in a range of 0.12 to IO parts by weight.
なお、上述した分散剤、帯電防止剤、潤滑剤などの添加
剤は、厳密に上述した作用効果のみを有するものである
との限定の下に記載したものではなく、例えば、分散剤
が潤滑剤あるいは帯電防止剤として作用することも有り
うる。従って、上記分類により例示した化合物などの効
果作用が、上記分類に記載された事項に限定されないこ
とば勿論であり、また複数の作用効果を奏する物質を使
用する場合には、添加量は、その作用効果を考慮して決
定することが好ましい。Note that the above-mentioned additives such as dispersants, antistatic agents, and lubricants are not strictly limited to having only the above-mentioned effects; for example, if the dispersant is a lubricant, Alternatively, it may act as an antistatic agent. Therefore, it goes without saying that the effects of compounds etc. exemplified by the above classifications are not limited to those listed in the above classifications, and when using substances that have multiple effects, the amount added is determined by the effect. It is preferable to decide in consideration of the effect.
このようにして調製された磁性塗料は前述の非磁性支持
体上に塗布される。このとき複数の磁性塗料を逐次ある
いは同時に重ｌ！塗布してもよい。The magnetic paint thus prepared is applied onto the non-magnetic support described above. At this time, apply multiple magnetic paints sequentially or simultaneously! May be applied.
塗布は、前記非磁性支持体上に直接行なうことも可能で
あるが、また、接着剤層などの中間層を介して非磁性支
持体上に塗布することもできる。Coating can be performed directly onto the non-magnetic support, but it can also be applied onto the non-magnetic support via an intermediate layer such as an adhesive layer.
ここでいう中間層とは接着剤華独の層または結合剤中に
カーボン等の非磁性微粒子を分散してなる複合膜層であ
る。The intermediate layer herein refers to an adhesive layer or a composite film layer formed by dispersing non-magnetic fine particles such as carbon in a binder.
カーボンブランクを含有する中間層は結合剤として磁性
層に用いられる種々の結合剤のなかから任意に選ぶこと
ができる。カーボンブランクの粒径は１０〜５００ｎｍ
（ナノメートル； １０−９ｍ）のものが好ましく、結
合剤二カーボンブランクは重量比にし７１００：１０か
ら１００：１５０が好ましい、中間層の厚みは単なる接
着剤層の場合０．１〜２μｍ、非磁性粉末を含む複合層
の場合０．５〜４μｍが好ましい。The intermediate layer containing the carbon blank can be arbitrarily selected as a binder from among various binders used in magnetic layers. The particle size of carbon blank is 10 to 500 nm.
(nanometer; 10-9 m), and the weight ratio of the binder and carbon blank is preferably 7100:10 to 100:150. The thickness of the intermediate layer is 0.1 to 2 μm in the case of a simple adhesive layer, and In the case of a composite layer containing magnetic powder, the thickness is preferably 0.5 to 4 μm.
中間層にはこのほか磁性層に用いている潤滑剤と同じ、
または異なる潤滑剤を添加してもよい。In addition, the intermediate layer contains the same lubricant used for the magnetic layer.
Or a different lubricant may be added.
上記の強磁性粉末と結合剤の分散方法および支持体への
塗布方法などの詳細は特開昭５４−４６０１１号および
同５４−２１８０５号等の各公報に記載されている。Details of the method of dispersing the above-mentioned ferromagnetic powder and binder and the method of coating it on a support are described in Japanese Patent Laid-Open Publications No. 54-46011 and No. 54-21805.
このようにして塗布される磁性層の厚さは、乾燥後の厚
さで一般には約０．５〜１０μｍの範囲、通常は０．７
〜６．０μｍの範囲になるよう塗布される。The thickness of the magnetic layer applied in this way is generally in the range of about 0.5 to 10 μm, usually 0.7 μm after drying.
It is applied so that the thickness is in the range of ~6.0 μm.
非磁性支持体上に塗布された磁性層は磁気記録媒体がテ
ープ状で使用される場合通常、磁性層中の強磁性粉末を
配向させる処理、即ち磁場配向処理を施したあと、乾燥
される。また逆にディスク状媒体の場合は磁気特性をと
りのぞくために、磁場による無配向処理が施される。こ
ののち必要により表面平滑化処理が施された後、必要に
より熱硬化及び／あるいは放射線照射による硬化処理後
所望の形状に裁断する。When a magnetic recording medium is used in the form of a tape, the magnetic layer coated on the non-magnetic support is usually subjected to a treatment for orienting the ferromagnetic powder in the magnetic layer, that is, a magnetic field orientation treatment, and then dried. On the other hand, in the case of a disk-shaped medium, a non-orientation treatment using a magnetic field is applied to remove the magnetic properties. Thereafter, the surface is smoothed if necessary, and then cured by heat curing and/or radiation irradiation if necessary, and then cut into a desired shape.
非磁性支持体の磁性層が設けられてない側の面には、公
知のハ、り層が設けられていてもよい。A known adhesive layer may be provided on the side of the nonmagnetic support on which the magnetic layer is not provided.
本発明において斜め蒸着とは基体表面の法線に対し強磁
性金属材料の藤気流をある入射角θを持たせて入射させ
基体表面上に磁性薄膜を析出させる方法である。In the present invention, oblique deposition is a method of depositing a magnetic thin film on the surface of a substrate by making a stream of ferromagnetic metal material incident at a certain angle of incidence θ with respect to the normal to the surface of the substrate.
本発明において入射角としては一般には４５″〜９０°
が望ましく、特に入射角θｍａｘは６０゜〜９０″、入
射角θｍ ｉ ｎは４５°〜７５＠が望ましい。In the present invention, the incident angle is generally 45'' to 90°.
It is desirable that the angle of incidence θmax is 60° to 90″, and the angle of incidence θmin is preferably 45° to 75＠.
本発明に用いられる強磁性金属薄膜材料としては、Ｆｅ
、Ｃｏ、Ｎｉ等の金属、あるいはＦｅＣ０１Ｆｅ−Ｎｉ
、Ｃｏ−Ｎｉ５ Ｆｅ−Ｃｏ−Ｎｔ。As the ferromagnetic metal thin film material used in the present invention, Fe
, Co, Ni, or other metals, or FeC01Fe-Ni
, Co-Ni5Fe-Co-Nt.
Ｆｅ−Ｒｈ、、Ｆｅ−Ｃｕ、Ｃｏ−Ｃｕ、Ｃｏ−Ａｕ、
Ｃｏ−Ｙ％ Ｃｏ−Ｌａ、Ｃｏ−Ｐｒ、Ｃ。Fe-Rh, , Fe-Cu, Co-Cu, Co-Au,
Co-Y% Co-La, Co-Pr, C.
Ｇｄｓ Ｃｏ−３ｍ、Ｃｏ−Ｐｔ、Ｎｉ −Ｃｕ。Gds Co-3m, Co-Pt, Ni-Cu.
Ｍｎ−Ｂ １５Ｍｎ−３ｂ、Ｍｎ−Ａｊ！、Ｆｅ−Ｃｒ
、Ｃｏ−Ｃｒ、Ｎｉ−Ｃｒ、Ｆｅ−Ｃｏ−Ｃｒ。Mn-B 15Mn-3b, Mn-Aj! , Fe-Cr
, Co-Cr, Ni-Cr, Fe-Co-Cr.
Ｎｉ−Ｃｏ−Ｃｒ、Ｆｅ−Ｃｏ−Ｎｉ−Ｃｒ等の強磁性
合金である。特に好ましいのはＣＯあるいはＣＯを７５
重量％含有するような合金である。These are ferromagnetic alloys such as Ni-Co-Cr and Fe-Co-Ni-Cr. Particularly preferred is CO or CO 75
It is an alloy containing % by weight.
積層してなる強磁性金属薄膜の総厚は、磁気記録媒体と
して充分な出力を与え得る厚さおよび高密度記録の充分
行える薄さを必要とすることから一般には約０．０２μ
ｍから５．０μｍ、好ましくは０．０５μｍから２．０
μｍである。各磁性薄膜の厚さは等しく設計してもいい
し、基体に最も近い強磁性金属薄膜の±５０％の厚さで
設けても良い。The total thickness of the laminated ferromagnetic metal thin film is generally about 0.02μ because it needs to be thick enough to provide sufficient output as a magnetic recording medium and thin enough to perform high-density recording.
m to 5.0 μm, preferably 0.05 μm to 2.0
It is μm. The thickness of each magnetic thin film may be designed to be equal, or the thickness may be ±50% of the thickness of the ferromagnetic metal thin film closest to the substrate.
本発明における蒸着とは、上記米国特許第３３４２６３
２号の明細書等に述べられている通常の真空蒸着の他、
電界、磁界あるいは電子ビーム照射等により莫気流のイ
オン化、加速化等を行って蒸発分子の平均自由行程の大
きい雰囲気にて支持基体上に強磁性金属薄膜を形成させ
る方法をも含むものであって、例えば特開昭５１−１４
９００８号明細書に示されているような電界蒸着法、特
公昭４３−１１５２５号、特公昭４６−２９４８４号、
特公昭４７−２６５７９号、特公昭４９４５４３９号、
特開昭４９−３３８９０号、特開昭４９−３４ｔ８３号
、特開昭４９−５４２３５号公報に示されているような
イオン化蒸着法も本発明に用いられる。The vapor deposition in the present invention refers to the above-mentioned US Pat. No. 334,263.
In addition to the usual vacuum deposition described in the specification etc. of No. 2,
It also includes a method of forming a ferromagnetic metal thin film on a supporting substrate in an atmosphere in which the mean free path of evaporated molecules is large by ionizing or accelerating a magnetic current using an electric field, magnetic field, electron beam irradiation, etc. , for example, JP-A-51-14
Field vapor deposition method as shown in specification No. 9008, Japanese Patent Publication No. 43-11525, Japanese Patent Publication No. 46-29484,
Special Publication No. 47-26579, Special Publication No. 4945439,
Ionization vapor deposition methods such as those disclosed in JP-A-49-33890, JP-A-49-34-t83, and JP-A-49-54,235 can also be used in the present invention.
本発明の強磁性金属薄膜に用いられる基体としてはポリ
エチレンテレフタレート、ポリイミド、ポリアミド、ポ
リ塩化ビニル、三酢酸セルロース、ポリカーボネート、
ポリエチレンナフタレートのようなプラスチックベース
が好ましい、特に本発明においては表面粗さ（Ｒａ）が
０．０１２μｍ以下であるような上記可撓性プラスチッ
クベースが好ましい、ここで表面粗さ（Ｒａ）とはＪＩ
ＳＢＯ６０１の５項に示されている中心線平均粗さで、
カットオフは０．２５ｍとする。さらに上記プラスチッ
クベース上に下塗り層を設け、その表面粗さ（Ｒａ）を
０．０１２μｍ以下としたものを基体として用いても良
い。Substrates used in the ferromagnetic metal thin film of the present invention include polyethylene terephthalate, polyimide, polyamide, polyvinyl chloride, cellulose triacetate, polycarbonate,
A plastic base such as polyethylene naphthalate is preferred. In the present invention, the above-mentioned flexible plastic base having a surface roughness (Ra) of 0.012 μm or less is particularly preferred. Here, the surface roughness (Ra) is J.I.
With the centerline average roughness shown in item 5 of SBO601,
The cutoff shall be 0.25m. Further, an undercoat layer may be provided on the plastic base, and the surface roughness (Ra) of the undercoat layer may be set to 0.012 μm or less, and this may be used as the substrate.
さらに本発明においては、積層してなる強磁性金属材料
の間に非磁性層を介在させても良い、非磁性中間層とし
て好ましいのはＣｒ、Ｓｔ、ＡＩ、Ｍｎ、Ｂｉ、Ｔｉｓ
Ｓｎ、Ｐｂ、Ｉｎ、Ｚｎ。Furthermore, in the present invention, a non-magnetic layer may be interposed between the laminated ferromagnetic metal materials. Preferred non-magnetic intermediate layers include Cr, St, AI, Mn, Bi, and Ti.
Sn, Pb, In, Zn.
Ｃｕあるいはこれらの酸化物、窒化物より構成される。It is composed of Cu or oxides or nitrides thereof.
（発明の効果）
本発明の尿素誘導体は分子内分極のためか、塗布型媒体
にあっては、結合剤特に極性基を有する結合剤との親和
性が強く、分散性が向上しかつ尿素誘導体自体の良好な
潤滑特性によって再生出力に優れ、かつ低温低湿、高温
高温下でのμ値が改良される。又本発明の尿素誘導体は
分子内分極のためか金属薄膜型媒体にあっては無機材料
との親和性が高く、かつ酸性を示さないので、金属の腐
食を生じることがなく、従ってさびを生じないと共に低
温低湿、高温高温でのμ値が改良される。(Effects of the Invention) Perhaps due to intramolecular polarization, the urea derivative of the present invention has a strong affinity with binders, especially binders having polar groups, in coating media, improving dispersibility and Due to its own good lubrication properties, it has excellent regeneration output and improves the μ value under low temperature, low humidity, and high temperature conditions. In addition, the urea derivative of the present invention has a high affinity with inorganic materials in metal thin film media, probably due to its intramolecular polarization, and does not exhibit acidity, so it does not cause corrosion of metals and therefore does not cause rust. At the same time, the μ value is improved at low temperature and low humidity, and at high temperature and high temperature.
次に実施例をもって本発明を具体的に説明するが、本発
明はこれらに限定されるものではない。EXAMPLES Next, the present invention will be specifically explained with reference to Examples, but the present invention is not limited thereto.
なお、実施例中の「部」との表示は「重量部」を示すも
のとする。Note that "parts" in the examples indicate "parts by weight."
〔実施例１〕
下記の組成物をニーダ−とボールミルを用いて４８時間
混線分散したあと、これにポリイソシアネート５部を加
え、さらに１時間混線分散したあと、１μｍの平均孔径
を有するフィルタを用いてろ過し、磁性塗料を調製した
。得られた磁性塗料を乾燥後の厚さが４．０μｍになる
ように、厚さ１０μｍのポリエチレンテレフタレート支
持体の表面にリバースロールを用いて塗布した。[Example 1] After cross-dispersing the following composition for 48 hours using a kneader and a ball mill, 5 parts of polyisocyanate was added thereto, and after cross-dispersing for another hour, it was cross-dispersed using a filter having an average pore size of 1 μm. The mixture was filtered and a magnetic paint was prepared. The obtained magnetic paint was applied onto the surface of a polyethylene terephthalate support having a thickness of 10 μm using a reverse roll so that the thickness after drying was 4.0 μm.
磁性塗料組成 強磁性合金粉末（組成：Ｆｅ９４％、Ｚｎ４％。Magnetic paint composition Ferromagnetic alloy powder (composition: 94% Fe, 4% Zn.
Ｎｉ２％；抗磁カニ１５０００ｅ；比表面積５４■／ボ
） １００部塩化ヒニル／酢酸ビニル
／無水マレイン酸共重合体（日本ゼオン■製４００ｘｌ
ｌＯＡ、重合度４００） （Ａ
＞または
塩化ビニル／酢酸ビニル共重合体（重合度４゜Ｏ）
（Ｂ）１２部
ポリエステル系ポリウレタン（重量平均分子量４万、数
平均分子量２．５万極性基の種類および極性基の数は第
１表に記載） （Ｃ）５部
コロネートし ４部研磨材（
α−アルミナ、平均粒径０．３μｍ）５部
潤滑材 （第１表記載）オレイン
酸 １部ブチルステアレ
ート 工部カーボンブラック（平均
粒径４０ｎｍ） ２部メチルエチルケトン
３００部磁性塗料が塗布された非磁性支持体を
、磁性塗料が未乾燥の状態で３０００ガウスの磁石で磁
場配向を行ない、さらに乾燥後、スーパーカレンダー処
理を行なった後８鶴幅にスリットして、８１１ビデオテ
ープを製造した。Ni 2%; anti-magnetic crab 15000e; specific surface area 54 / Bo) 100 parts hinyl chloride/vinyl acetate/maleic anhydride copolymer (400xl manufactured by Nippon Zeon)
lOA, degree of polymerization 400) (A
> or vinyl chloride/vinyl acetate copolymer (degree of polymerization 4°O)
(B) 12 parts polyester polyurethane (weight average molecular weight 40,000, number average molecular weight 25,000, type and number of polar groups are listed in Table 1) (C) 5 parts coronate, 4 parts abrasive (
α-Alumina, average particle size 0.3 μm) 5 parts Lubricant (listed in Table 1) Oleic acid 1 part Butyl stearate Kobe carbon black (average particle size 40 nm) 2 parts Methyl ethyl ketone
A non-magnetic support coated with 300 parts of magnetic paint was oriented in a magnetic field with a 3000 Gauss magnet while the magnetic paint was not dry, and after drying, it was supercalendered and then slit into 8-inch widths. , produced 811 videotapes.
〔実施例２〕
１３μｍ厚のポリエチレンテレフタレートフィルム上に
コバルト−ニッケルｆｕｌｌ！ （ｌｌ［１５０部ｍ）
を斜め蒸着し、磁気記録媒体の原反を調製した。蒸発源
としては電子ビーム蒸発源を使用し、これにコバルト−
ニッケル合金（Ｃｏ ： ８０ｗｔ％、Ｎｉ：２０％）
をチャージし真空度５×１０−’Ｔｏ ｒ ｒ中にて酸
素気流中で入射角が５０度となるよう斜め蒸着を行った
。得られた磁気記録媒体の原反の磁性金属薄膜上に各種
材料をメチルエチルケトンに溶解して塗布、乾燥し調製
したサンプルを作製し試料陳２８〜４５とした（第２表
）。[Example 2] Cobalt-nickel full on a 13 μm thick polyethylene terephthalate film! (150 copies)
was obliquely deposited to prepare a raw material for a magnetic recording medium. An electron beam evaporation source is used as the evaporation source, and cobalt-
Nickel alloy (Co: 80wt%, Ni: 20%)
was charged, and oblique evaporation was performed in an oxygen stream at a vacuum level of 5×10-' Torr so that the incident angle was 50 degrees. Various materials dissolved in methyl ethyl ketone were coated on the magnetic metal thin film of the obtained magnetic recording medium, and samples were prepared by drying and designated as samples Nos. 28 to 45 (Table 2).
上記のようにして得られたビデオテープにＶＴＲ（富士
写真フィルム■： ＦＵＪ ｌＸ−８）を用いて７ＭＨ
２の信号を記録し、再生した。基準テープ（比較例１７
）に記録した７ＭＨ，の再生出力をＯｄＢとしたときの
ビデオテープの相対的な再生出力を測定した。The videotape obtained as above was recorded at 7MH using a VTR (Fuji Photo Film ■: FUJ 1X-8).
2 signals were recorded and played back. Standard tape (Comparative Example 17
) The relative playback output of the videotape was measured, assuming that the playback output of a 7MH, which was recorded on a video tape, was set to OdB.
得られたビデオテープとステンレスポールとを５０ｇの
張力（Ｔ１）で接触（巻きつけ角１８０°）させて、こ
の条件下で、ビデオテープを３． ３ｃｍ／Ｓの速度で
走行させるのに必要な張力（Ｔ２）を測定した。この測
定値をもとに、下記計算式によりビデオテープの、Ｎ！
ｓ係数μをもとめた。（第１表および第２表に記載）
ｐ＝ Ｉ／ｒ −１ｎ （Ｔｚ／Ｔ＋）尚、摩擦係数
のテストは、ａ、５℃、１０％ＲＨ，ｂ、４５℃、９０
％ＲＨの２条件で行なった。The obtained videotape and a stainless steel pole were brought into contact (wrapping angle 180°) with a tension of 50g (T1), and under these conditions, the videotape was 3. The tension (T2) required to run at a speed of 3 cm/S was measured. Based on this measurement value, the following calculation formula is used to calculate the N!
The s coefficient μ was determined. (Listed in Tables 1 and 2) p= I/r -1n (Tz/T+) The friction coefficient test was performed at a, 5°C, 10%RH, b, 45°C, 90°C.
The test was carried out under two conditions: %RH.
またテープの強磁性体への腐食を調べるため、温度を２
０℃から４０まで湿度を１０％から１００％まで変化す
るサーモに１週間放置したテープを顕微鏡で観察しさび
状況をサンプル３７を１００とし錆の量を相対比較した
。In addition, in order to investigate corrosion of the ferromagnetic material of the tape, the temperature was
The tape was left in a thermostat for one week at temperatures ranging from 0° C. to 40° C. and the humidity was varied from 10% to 100%, and the tape was observed under a microscope to determine the amount of rust, with Sample 37 set as 100.
第１表、第２表の結果より明白な如く、本発明の、尿素
誘導体を用いた実施例はいずれも出力が高（ａ、ｂ両条
件でも摩擦係数が低く、又金属薄膜にした場合にテープ
を腐食しないことがわかる。As is clear from the results in Tables 1 and 2, all examples using urea derivatives of the present invention have high output (low friction coefficient under both conditions a and b), and when made into a metal thin film. It can be seen that the tape does not corrode.
一方、本発明の化合物を使用せず、単に脂肪酸やエステ
ルのみを用いた場合は、再生出力も低く、また特に高温
、高１（ｂ条件）下での摩擦係数が大きい、スルホン酸
やホスホン酸はテープを腐食することがわかる。On the other hand, when only fatty acids and esters are used without using the compound of the present invention, the regeneration output is low, and sulfonic acids and phosphonic acids, which have a high friction coefficient especially at high temperatures and high 1 (b conditions) It can be seen that this corrodes the tape.
Claims (3)
記録媒体において、前記磁性層が下記一般式で表わされ
る尿素誘導体を含有又は保持することを特徴とする磁気
記録媒体。（一般式） ▲数式、化学式、表等があります▼ （但しＲ＿１は、炭素数１０以上２６以下の炭化水素基
Ｒ＿２、Ｒ＿４は、同じあるいは異なる水素あるいは１
以上２６以下の炭化水素基Ｒ＿３は、炭素数１以上２６
以下の炭化水素基）(1) A magnetic recording medium comprising a nonmagnetic support and a magnetic layer provided on the support, wherein the magnetic layer contains or holds a urea derivative represented by the following general formula. (General formula) ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼ (However, R_1 is a hydrocarbon group with 10 to 26 carbon atoms. R_2 and R_4 are the same or different hydrogen
The hydrocarbon group R_3 having 26 or more carbon atoms has 1 or more and 26 or more carbon atoms.
following hydrocarbon groups)
結合剤の全樹脂のうち５ｗｔ％以上を占める樹脂の少な
くとも１種の樹脂がエポキシ基、−ＣＯＯＭ、−ＯＨ、
−ＮＲ＿２、−ＮＲ＿３Ｘ、−ＳＯ＿３Ｍ、−ＯＳＯ＿
３Ｍ、−ＰＯ＿３Ｍ＿２、−ＯＰＯ＿３Ｍ＿２のうち少
なくとも１種の極性基（ここでＭは水素、アルカリ金属
、または置換、未置換のアンモニウムであり、一つの基
の中に複数のＭがあるときは、互いに異なってもよい。 Ｘはハロゲンイオンを示す。Ｒは水素又はアルキル基で
ある。）を樹脂１グラム当り１０＾−＾７〜１０＾−＾
３当量導入した樹脂であることを特徴とする請求項（１
）記載の磁気記録媒体。(2) The magnetic layer includes a ferromagnetic powder and a binder, and at least one resin accounting for 5 wt% or more of the total resins in the binder has an epoxy group, -COOM, -OH,
-NR_2, -NR_3X, -SO_3M, -OSO_
At least one polar group among 3M, -PO_3M_2, -OPO_3M_2 (where M is hydrogen, an alkali metal, or substituted or unsubstituted ammonium, and when there are multiple M's in one group, they are mutually may be different. X represents a halogen ion. R is hydrogen or an alkyl group.
Claim (1) characterized in that the resin is a resin into which 3 equivalents are introduced.
) Magnetic recording medium described.
ることを特徴とする請求項（１）記載の磁気記録媒体。(3) The magnetic recording medium according to claim (1), wherein the magnetic layer is a ferromagnetic metal thin film formed by oblique deposition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2165262A JPH0457215A (en) | 1990-06-22 | 1990-06-22 | Magnetic recording medium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2165262A JPH0457215A (en) | 1990-06-22 | 1990-06-22 | Magnetic recording medium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0457215A true JPH0457215A (en) | 1992-02-25 |
Family
ID=15808989
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2165262A Pending JPH0457215A (en) | 1990-06-22 | 1990-06-22 | Magnetic recording medium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0457215A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001507388A (en) * | 1996-12-27 | 2001-06-05 | エルヴェーエー−デーエーアー アクチエンゲゼルシャフト フィュール ミネラルオエル ウント ヒェミー | Liquid compositions and their use as magnetorheological liquids |
| US7463747B2 (en) | 2004-03-31 | 2008-12-09 | Panasonic Corporation | Loudspeaker system |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5385402A (en) * | 1976-12-31 | 1978-07-27 | Philips Nv | Magnetic recording medium* lubricant therefor* and method of making said lubricant |
| JPS5984407A (en) * | 1982-11-05 | 1984-05-16 | Hitachi Ltd | Magnetic recording medium |
| JPS6271026A (en) * | 1985-09-20 | 1987-04-01 | Toyobo Co Ltd | Magnetic recording medium |
| JPS6489022A (en) * | 1987-09-30 | 1989-04-03 | Fuji Photo Film Co Ltd | Magnetic recording medium |
-
1990
- 1990-06-22 JP JP2165262A patent/JPH0457215A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5385402A (en) * | 1976-12-31 | 1978-07-27 | Philips Nv | Magnetic recording medium* lubricant therefor* and method of making said lubricant |
| JPS5984407A (en) * | 1982-11-05 | 1984-05-16 | Hitachi Ltd | Magnetic recording medium |
| JPS6271026A (en) * | 1985-09-20 | 1987-04-01 | Toyobo Co Ltd | Magnetic recording medium |
| JPS6489022A (en) * | 1987-09-30 | 1989-04-03 | Fuji Photo Film Co Ltd | Magnetic recording medium |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001507388A (en) * | 1996-12-27 | 2001-06-05 | エルヴェーエー−デーエーアー アクチエンゲゼルシャフト フィュール ミネラルオエル ウント ヒェミー | Liquid compositions and their use as magnetorheological liquids |
| US7463747B2 (en) | 2004-03-31 | 2008-12-09 | Panasonic Corporation | Loudspeaker system |
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