JPS62236120A - Magnetic recording medium - Google Patents
Magnetic recording mediumInfo
- Publication number
- JPS62236120A JPS62236120A JP61079516A JP7951686A JPS62236120A JP S62236120 A JPS62236120 A JP S62236120A JP 61079516 A JP61079516 A JP 61079516A JP 7951686 A JP7951686 A JP 7951686A JP S62236120 A JPS62236120 A JP S62236120A
- Authority
- JP
- Japan
- Prior art keywords
- carboxylic acid
- thin film
- magnetic
- ester
- recording medium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 50
- -1 perfluoroalkyl ester Chemical class 0.000 claims abstract description 44
- 230000005294 ferromagnetic effect Effects 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000010409 thin film Substances 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims description 37
- 239000002184 metal Substances 0.000 claims description 37
- 239000000314 lubricant Substances 0.000 abstract description 19
- 150000002148 esters Chemical class 0.000 abstract description 9
- 230000001050 lubricating effect Effects 0.000 abstract description 7
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 abstract description 4
- AQYSYJUIMQTRMV-UHFFFAOYSA-N hypofluorous acid Chemical compound FO AQYSYJUIMQTRMV-UHFFFAOYSA-N 0.000 abstract description 2
- 150000001735 carboxylic acids Chemical class 0.000 abstract 3
- 239000010410 layer Substances 0.000 description 28
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 15
- 239000010408 film Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 8
- 235000014113 dietary fatty acids Nutrition 0.000 description 8
- 239000000194 fatty acid Substances 0.000 description 8
- 229930195729 fatty acid Natural products 0.000 description 8
- 229920005989 resin Polymers 0.000 description 8
- 239000011347 resin Substances 0.000 description 8
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 150000004665 fatty acids Chemical class 0.000 description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000003449 preventive effect Effects 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000007769 metal material Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- WFFZELZOEWLYNK-CLFAGFIQSA-N bis[(z)-octadec-9-enyl] hydrogen phosphate Chemical compound CCCCCCCC\C=C/CCCCCCCCOP(O)(=O)OCCCCCCCC\C=C/CCCCCCCC WFFZELZOEWLYNK-CLFAGFIQSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 150000002391 heterocyclic compounds Chemical class 0.000 description 3
- 238000005461 lubrication Methods 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 229920006254 polymer film Polymers 0.000 description 3
- 229920001021 polysulfide Polymers 0.000 description 3
- 239000005077 polysulfide Substances 0.000 description 3
- 150000008117 polysulfides Polymers 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 description 3
- 238000001771 vacuum deposition Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 2
- WSULSMOGMLRGKU-UHFFFAOYSA-N 1-bromooctadecane Chemical compound CCCCCCCCCCCCCCCCCCBr WSULSMOGMLRGKU-UHFFFAOYSA-N 0.000 description 2
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 229910020630 Co Ni Inorganic materials 0.000 description 2
- 229910002440 Co–Ni Inorganic materials 0.000 description 2
- 229910000599 Cr alloy Inorganic materials 0.000 description 2
- CETBSQOFQKLHHZ-UHFFFAOYSA-N Diethyl disulfide Chemical compound CCSSCC CETBSQOFQKLHHZ-UHFFFAOYSA-N 0.000 description 2
- YWHLKYXPLRWGSE-UHFFFAOYSA-N Dimethyl trisulfide Chemical compound CSSSC YWHLKYXPLRWGSE-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- NYHBQMYGNKIUIF-UUOKFMHZSA-N Guanosine Chemical compound C1=NC=2C(=O)NC(N)=NC=2N1[C@@H]1O[C@H](CO)[C@@H](O)[C@H]1O NYHBQMYGNKIUIF-UUOKFMHZSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 2
- AUNGANRZJHBGPY-SCRDCRAPSA-N Riboflavin Chemical compound OC[C@@H](O)[C@@H](O)[C@@H](O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-SCRDCRAPSA-N 0.000 description 2
- RYYWUUFWQRZTIU-UHFFFAOYSA-N Thiophosphoric acid Chemical class OP(O)(S)=O RYYWUUFWQRZTIU-UHFFFAOYSA-N 0.000 description 2
- DZBUGLKDJFMEHC-UHFFFAOYSA-N acridine Chemical compound C1=CC=CC2=CC3=CC=CC=C3N=C21 DZBUGLKDJFMEHC-UHFFFAOYSA-N 0.000 description 2
- 125000003342 alkenyl group Chemical group 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 125000006267 biphenyl group Chemical group 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- KMGBZBJJOKUPIA-UHFFFAOYSA-N butyl iodide Chemical compound CCCCI KMGBZBJJOKUPIA-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- GVPWHKZIJBODOX-UHFFFAOYSA-N dibenzyl disulfide Chemical compound C=1C=CC=CC=1CSSCC1=CC=CC=C1 GVPWHKZIJBODOX-UHFFFAOYSA-N 0.000 description 2
- JTXUVYOABGUBMX-UHFFFAOYSA-N didodecyl hydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(=O)OCCCCCCCCCCCC JTXUVYOABGUBMX-UHFFFAOYSA-N 0.000 description 2
- LJSQFQKUNVCTIA-UHFFFAOYSA-N diethyl sulfide Chemical compound CCSCC LJSQFQKUNVCTIA-UHFFFAOYSA-N 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- HCZHHEIFKROPDY-UHFFFAOYSA-N kynurenic acid Chemical compound C1=CC=C2NC(C(=O)O)=CC(=O)C2=C1 HCZHHEIFKROPDY-UHFFFAOYSA-N 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000004780 naphthols Chemical class 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 150000003014 phosphoric acid esters Chemical class 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 239000005033 polyvinylidene chloride Substances 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 238000006748 scratching Methods 0.000 description 2
- 230000002393 scratching effect Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- UIYCHXAGWOYNNA-UHFFFAOYSA-N vinyl sulfide Chemical compound C=CSC=C UIYCHXAGWOYNNA-UHFFFAOYSA-N 0.000 description 2
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 description 2
- MAOBFOXLCJIFLV-UHFFFAOYSA-N (2-aminophenyl)-phenylmethanone Chemical compound NC1=CC=CC=C1C(=O)C1=CC=CC=C1 MAOBFOXLCJIFLV-UHFFFAOYSA-N 0.000 description 1
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- UOFGSWVZMUXXIY-UHFFFAOYSA-N 1,5-Diphenyl-3-thiocarbazone Chemical compound C=1C=CC=CC=1N=NC(=S)NNC1=CC=CC=C1 UOFGSWVZMUXXIY-UHFFFAOYSA-N 0.000 description 1
- 239000005968 1-Decanol Substances 0.000 description 1
- MPPPKRYCTPRNTB-UHFFFAOYSA-N 1-bromobutane Chemical compound CCCCBr MPPPKRYCTPRNTB-UHFFFAOYSA-N 0.000 description 1
- OLYCCRFKXJIENQ-UHFFFAOYSA-N 1-bromopropane;phosphoric acid Chemical compound CCCBr.OP(O)(O)=O OLYCCRFKXJIENQ-UHFFFAOYSA-N 0.000 description 1
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 description 1
- ZNJOCVLVYVOUGB-UHFFFAOYSA-N 1-iodooctadecane Chemical compound CCCCCCCCCCCCCCCCCCI ZNJOCVLVYVOUGB-UHFFFAOYSA-N 0.000 description 1
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 1
- MTYGYDUMMAMTRV-KTKRTIGZSA-N 2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctyl (Z)-octadec-9-enoate Chemical compound FC(C(C(C(C(C(COC(CCCCCCC\C=C/CCCCCCCC)=O)(F)F)(F)F)(F)F)(F)F)(F)F)(C(F)(F)F)F MTYGYDUMMAMTRV-KTKRTIGZSA-N 0.000 description 1
- ZIMCZOLRXKPXLN-UHFFFAOYSA-N 2,2,4-trimethyl-4-(2,4,4-trimethylpentan-2-yldisulfanyl)pentane Chemical compound CC(C)(C)CC(C)(C)SSC(C)(C)CC(C)(C)C ZIMCZOLRXKPXLN-UHFFFAOYSA-N 0.000 description 1
- RQMWDQMALYNILJ-UHFFFAOYSA-N 2,3,4,5,5-pentachloropenta-2,4-dienoic acid Chemical compound OC(=O)C(Cl)=C(Cl)C(Cl)=C(Cl)Cl RQMWDQMALYNILJ-UHFFFAOYSA-N 0.000 description 1
- WOHLSTOWRAOMSG-UHFFFAOYSA-N 2,3-dihydro-1,3-benzothiazole Chemical compound C1=CC=C2SCNC2=C1 WOHLSTOWRAOMSG-UHFFFAOYSA-N 0.000 description 1
- YEVQZPWSVWZAOB-UHFFFAOYSA-N 2-(bromomethyl)-1-iodo-4-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=C(I)C(CBr)=C1 YEVQZPWSVWZAOB-UHFFFAOYSA-N 0.000 description 1
- NYLJHRUQFXQNPN-UHFFFAOYSA-N 2-(tert-butyltrisulfanyl)-2-methylpropane Chemical compound CC(C)(C)SSSC(C)(C)C NYLJHRUQFXQNPN-UHFFFAOYSA-N 0.000 description 1
- IHXKXSJKLJZXKZ-UHFFFAOYSA-N 2-aminocyclohexa-2,5-diene-1,4-dione Chemical compound NC1=CC(=O)C=CC1=O IHXKXSJKLJZXKZ-UHFFFAOYSA-N 0.000 description 1
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 1
- GPLIMIJPIZGPIF-UHFFFAOYSA-N 2-hydroxy-1,4-benzoquinone Chemical class OC1=CC(=O)C=CC1=O GPLIMIJPIZGPIF-UHFFFAOYSA-N 0.000 description 1
- VTWDKFNVVLAELH-UHFFFAOYSA-N 2-methylcyclohexa-2,5-diene-1,4-dione Chemical class CC1=CC(=O)C=CC1=O VTWDKFNVVLAELH-UHFFFAOYSA-N 0.000 description 1
- VSHVAOIJUGIMJM-UHFFFAOYSA-N 2-nitrocyclohexa-2,5-diene-1,4-dione Chemical compound [O-][N+](=O)C1=CC(=O)C=CC1=O VSHVAOIJUGIMJM-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- JSTCPNFNKICNNO-UHFFFAOYSA-N 4-nitrosophenol Chemical compound OC1=CC=C(N=O)C=C1 JSTCPNFNKICNNO-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical class [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ICPHWJOJNPWHQF-UHFFFAOYSA-N C(C(C)C)C1=C(C=CC=C1)S(=P([S-])([O-])[O-])CCCCCCCCC.[Zn+2].C(C(C)C)C1=C(C=CC=C1)S(=P([S-])([O-])[O-])CCCCCCCCC.[Zn+2].[Zn+2] Chemical compound C(C(C)C)C1=C(C=CC=C1)S(=P([S-])([O-])[O-])CCCCCCCCC.[Zn+2].C(C(C)C)C1=C(C=CC=C1)S(=P([S-])([O-])[O-])CCCCCCCCC.[Zn+2].[Zn+2] ICPHWJOJNPWHQF-UHFFFAOYSA-N 0.000 description 1
- DVBSUIROAVSLCA-UHFFFAOYSA-N C(C(C)C)S(=P([S-])([O-])[O-])CCCCC.[Zn+2].C(C(C)C)S(=P([S-])([O-])[O-])CCCCC.[Zn+2].[Zn+2] Chemical compound C(C(C)C)S(=P([S-])([O-])[O-])CCCCC.[Zn+2].C(C(C)C)S(=P([S-])([O-])[O-])CCCCC.[Zn+2].[Zn+2] DVBSUIROAVSLCA-UHFFFAOYSA-N 0.000 description 1
- VLYHYFWHKZDPON-UHFFFAOYSA-N CCCC(C)S(=P(O)(O)S)C(C)C Chemical compound CCCC(C)S(=P(O)(O)S)C(C)C VLYHYFWHKZDPON-UHFFFAOYSA-N 0.000 description 1
- BKKBEZCXJQVAKC-UHFFFAOYSA-N CCCCCCCC1=CC=CC([S+]=P([O-])(O)S)=C1CCCCCCC Chemical compound CCCCCCCC1=CC=CC([S+]=P([O-])(O)S)=C1CCCCCCC BKKBEZCXJQVAKC-UHFFFAOYSA-N 0.000 description 1
- PMHDXOLBAYDFKY-UHFFFAOYSA-N CCCCCCCCN.CCCCC(CC)COP(O)(O)=O Chemical compound CCCCCCCCN.CCCCC(CC)COP(O)(O)=O PMHDXOLBAYDFKY-UHFFFAOYSA-N 0.000 description 1
- KLXWMFXGEJFIGE-UHFFFAOYSA-N CCCCCCCS(=P(O)(O)S)C1=CC=CC=C1CC(C)C Chemical compound CCCCCCCS(=P(O)(O)S)C1=CC=CC=C1CC(C)C KLXWMFXGEJFIGE-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229920001747 Cellulose diacetate Polymers 0.000 description 1
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- HBEMHMNHYDTVRE-UHFFFAOYSA-N ClC(CCCCCCCCCCCCCCCCC(=O)OC)(Cl)Cl Chemical compound ClC(CCCCCCCCCCCCCCCCC(=O)OC)(Cl)Cl HBEMHMNHYDTVRE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910020707 Co—Pt Inorganic materials 0.000 description 1
- MIKUYHXYGGJMLM-GIMIYPNGSA-N Crotonoside Natural products C1=NC2=C(N)NC(=O)N=C2N1[C@H]1O[C@@H](CO)[C@H](O)[C@@H]1O MIKUYHXYGGJMLM-GIMIYPNGSA-N 0.000 description 1
- AUNGANRZJHBGPY-UHFFFAOYSA-N D-Lyxoflavin Natural products OCC(O)C(O)C(O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Lubricants (AREA)
- 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、真空蒸着やスパッタリング等の真空薄膜形成
技術等の手法により非磁性支持体上に強磁性金rsfl
i膜を磁性層として形成した、いわゆる強磁性金属薄膜
型の磁気記録媒体に関するものである。Detailed Description of the Invention [Industrial Field of Application] The present invention is directed to the production of ferromagnetic gold rsfl on a non-magnetic support by vacuum thin film forming techniques such as vacuum evaporation and sputtering.
The present invention relates to a so-called ferromagnetic metal thin film type magnetic recording medium in which an i-film is formed as a magnetic layer.
本発明は、非磁性支持体上に強磁性金属薄膜を磁性層と
して形成してなる磁気記録媒体において、磁性層である
強磁性金属薄膜上にカルボン酸パーフルオロアルキルエ
ステル及び極圧剤を含むトップコート層を形成し、
あらゆる使用条件下においても優れた走行性。The present invention provides a magnetic recording medium in which a ferromagnetic metal thin film is formed as a magnetic layer on a non-magnetic support, and a top layer containing a carboxylic acid perfluoroalkyl ester and an extreme pressure agent on the ferromagnetic metal thin film as the magnetic layer. Forms a coating layer that provides excellent running performance under all conditions of use.
耐摩耗性、耐久性を発揮する磁気記録媒体を提供しよう
とするものである。The objective is to provide a magnetic recording medium that exhibits wear resistance and durability.
従来より磁気記録媒体としては、非磁性支持体上にr−
F6g03.coを含有するr F e z O、。Conventionally, as a magnetic recording medium, r-
F6g03. r F ez O, containing co.
Fe5Oe+Coを含有するF esoa、T −F
e zOxとFe5O4とのベルトライド化合物、Co
を含有するベルトライド化合物、Crag等の酸化物強
磁性粉末あるいはFe、Co、Ni等を主成分とする合
金磁性粉末等の粉末磁性材料を塩化ビニル−酢酸ビニル
系共重合体、ポリエステル樹脂、ポリウレタン横腹等の
有機バインダー中に分散せしめた磁性塗料を塗布・乾燥
することにより作製される塗布型の磁気記録媒体が広く
使用されている。Fesoa containing Fe5Oe+Co, T-F
e Bertolide compound of zOx and Fe5O4, Co
Powder magnetic materials such as ferromagnetic powders such as ferromagnetic oxide powders such as Bertolide compounds and Crag, or alloy magnetic powders containing Fe, Co, Ni, etc. as main components are combined with vinyl chloride-vinyl acetate copolymers, polyester resins, and polyurethane. Coating-type magnetic recording media, which are manufactured by coating and drying a magnetic paint dispersed in an organic binder such as a side surface, are widely used.
これに対して、高密度磁気記録への要求の高まりととも
に、Co−Ni合金等の強磁性金属材料を、メッキや真
空薄膜形成技術(真空蒸着法やスパッタリング法、イオ
ンブレーティング法等)によってポリエステルフィルム
やポリイミドフィルム等の非磁性支持体上に直接被着し
た、いわゆる強磁性金属薄膜型の磁気記録媒体が提案さ
れ、注目を集めている。この強磁性金属薄膜型磁気記録
媒体は、抗磁力や角形比等に優れ、短波長での電磁変換
特性に優れるばかりでなく、磁性層の厚みを極めて薄く
することが可能であるため記ii減磁や再生時の厚み損
失が著しく小さいこと、磁性層中に非磁性材である有機
バインダーを混入する必要がないため磁性材料の充填密
度を高めることができること等、数々の利点を有してい
る。On the other hand, with the increasing demand for high-density magnetic recording, ferromagnetic metal materials such as Co-Ni alloys have been made into polyester by plating or vacuum thin film formation technology (vacuum evaporation, sputtering, ion blating, etc.). A so-called ferromagnetic metal thin film type magnetic recording medium, which is directly deposited on a non-magnetic support such as a film or a polyimide film, has been proposed and is attracting attention. This ferromagnetic metal thin film magnetic recording medium not only has excellent coercive force and squareness, and excellent electromagnetic conversion characteristics at short wavelengths, but also has the ability to reduce the magnetic layer thickness by making it extremely thin. It has a number of advantages, including extremely low thickness loss during magnetization and reproduction, and the ability to increase the packing density of the magnetic material because there is no need to mix an organic binder, which is a non-magnetic material, into the magnetic layer. .
しかしながら、上述の強磁性金属薄膜型の磁気記録媒体
では、磁性層表面の平滑性が極めて良好であるために実
質的な接触面積が大きくなり、凝着現象(いわゆるはり
つき)が起こり易くなったりPj!擦係数が大きくなる
等、耐久性や走行性等に欠点が多く、その改善が大きな
課題となっている。However, in the above-mentioned ferromagnetic metal thin film type magnetic recording medium, the surface smoothness of the magnetic layer is extremely good, so the substantial contact area is large, and adhesion phenomena (so-called sticking) are likely to occur. ! It has many shortcomings in terms of durability, running performance, etc., such as a large coefficient of friction, and improvement of these problems has become a major issue.
一般に、磁気記録媒体は磁気信号の記録・再生の過程で
磁気ヘッドとの高速相対運動のもとにおかれ、その際走
行が円滑に、かつ安定な状態で行われなければならない
、また、磁気ヘッドとの接触による摩耗や損傷はなるべ
く少ないほうがよい。In general, a magnetic recording medium is subjected to high-speed relative motion with a magnetic head during the process of recording and reproducing magnetic signals, and during this time, it must run smoothly and stably. It is better to minimize wear and damage caused by contact with the head.
そこで例えば、上記磁気記録媒体の磁性層、すなわち強
磁性金属薄膜上に潤滑剤を塗布して保護n々を形成する
ことにより、上記耐久性や走行性を改善することが試み
られている。For example, attempts have been made to improve the durability and runnability by coating the magnetic layer of the magnetic recording medium, that is, the ferromagnetic metal thin film, with a lubricant to form a protective film.
ところで、上述のように潤滑剤を塗布して保護膜を形成
した場合には、この保護膜が磁性層である強磁性金属″
1tlaに対して良好な密着性を示し、かつ高い潤滑効
果を発揮することが要求される。By the way, when a protective film is formed by applying a lubricant as described above, this protective film is a ferromagnetic metal that is a magnetic layer.
It is required to exhibit good adhesion to 1 tla and to exhibit a high lubricating effect.
また、これら密着性や潤滑効果は、熱帯、亜熱帯地方等
のように高温多湿の条件下でも、寒冷地のように低温の
条件下でも優れたものでなければならない。In addition, these adhesion properties and lubrication effects must be excellent both under hot and humid conditions, such as in tropical and subtropical regions, and under low-temperature conditions, such as in cold regions.
しかしながら、従来広く用いられている潤滑剤の使用温
度範囲は限られており、特に、O〜−5℃のような低温
下では固体化または凍結するものが多く、充分にその潤
滑効果を発揮させることができなかった。However, the operating temperature range of conventionally widely used lubricants is limited, and in particular, many of them solidify or freeze at low temperatures such as O to -5℃, so it is difficult to fully demonstrate their lubricating effect. I couldn't do that.
そこで本発明は1、如何なる使用条件下においても密着
性や潤滑性が保たれ、かつ長期に亘り潤滑効果が持続す
るトップコート層をI71!磁性金属薄膜上に形成する
ことにより、走行性、耐久性に優れた磁気記録媒体を提
供することを目的とする。Therefore, the present invention provides (1) a top coat layer that maintains adhesion and lubricity under any usage conditions and maintains a lubricating effect over a long period of time; The object of the present invention is to provide a magnetic recording medium having excellent running properties and durability by forming the magnetic recording medium on a magnetic metal thin film.
本発明者等は、上述の目的を達成せんものと鋭意研究の
結果、脂肪族カルボン酸とパーフルオロアルコールのエ
ステルであるカルボン酸パーフルオロアルキルエステル
中に各種の極圧剤を添加した潤滑剤が広い温度範囲に亘
って良好な潤滑効果を発揮することを見出し本発明を完
成するに至ったものであって、非磁性支持体上に強磁性
金属薄膜を形成し、前記強磁性金属薄膜上にカルボン酸
パーフルオロアルキルエステル及び極圧剤を含むトップ
コート層を形成したことを特徴とするものである。As a result of intensive research, the present inventors have discovered that a lubricant containing various extreme pressure agents added to carboxylic acid perfluoroalkyl ester, which is an ester of aliphatic carboxylic acid and perfluoroalcohol, has been developed. The present invention has been completed by discovering that a good lubrication effect can be exhibited over a wide temperature range. It is characterized in that a top coat layer containing a carboxylic acid perfluoroalkyl ester and an extreme pressure agent is formed.
本発明で潤滑剤として使用されるカルボン酸パーフルオ
ロフルキルエステルは、一般式%式%(1)
(但し、上記一般式において、m≦2n+l。The carboxylic acid perfluorofurkyl ester used as a lubricant in the present invention has the general formula % (1) (However, in the above general formula, m≦2n+l.
j≧0.に≧4である。)
で示される化合物である。ここで、カルボン酸のアルキ
ル基(−C,H,)は直鎖状1分枝状のいずれでもよく
、また二重結合を含んでいてもよい。j≧0. is ≧4. ) is a compound represented by Here, the alkyl group (-C, H,) of the carboxylic acid may be linear or monobranched, or may contain a double bond.
一方、パーフルオロアルキル基(−CkFz*、+)の
炭素数には4以上であるのが良いが、6以上とするのが
より好ましい。On the other hand, the number of carbon atoms in the perfluoroalkyl group (-CkFz*, +) is preferably 4 or more, and more preferably 6 or more.
カルボン酸パーフルオロアルキルエステルは、例えば相
当する酸塩化物と含フツ素アルコールとの反応によって
容易に合成される。反応式を示せば次のようなものであ
る。Carboxylic acid perfluoroalkyl esters are easily synthesized, for example, by reacting a corresponding acid chloride with a fluorine-containing alcohol. The reaction formula is as follows.
C11ItlICOCR+ CbF□、+(Cut)t
OH塩基
CIlIt−CoCl1It−Coo(CH+・・・+
11式
上記酸塩化物は、市販の脂肪族カルボン酸を五塩化リン
PCl5あるいは塩化チオニルSOC1gで塩素化する
ことによって容易に合成できる。特に、脂肪族カルボン
酸の炭素数nが小さいものについては、塩化チオニルS
OC1zで塩素化することによって合成できる0反応式
は下記の通りである。C11ItlICOCR+ CbF□, +(Cut)t
OH base CIlIt-CoCl1It-Coo (CH+...+
The above acid chloride of formula 11 can be easily synthesized by chlorinating a commercially available aliphatic carboxylic acid with 1 g of phosphorus pentachloride PCl5 or thionyl chloride SOC. In particular, for aliphatic carboxylic acids with small carbon number n, thionyl chloride S
The 0 reaction formula that can be synthesized by chlorination with OC1z is as follows.
Cl5
C,H,C0OH−Cl111.cOcl・・・(2)
式
一方、フッ素含有アルコールCJtk++ (Cut)
70Hについては、シモンズ法等によって得られたパ
ーフルオロカルボン酸をジメチルホルムアミド(DMF
)存在下で塩素化した後、還元剤によって還元すること
により容易に合成することができる。Cl5C,H,C0OH-Cl111. cOcl...(2)
Formula: On the other hand, fluorine-containing alcohol CJtk++ (Cut)
For 70H, perfluorocarboxylic acid obtained by the Simmons method etc. was mixed with dimethylformamide (DMF
) can be easily synthesized by chlorination in the presence of a compound, followed by reduction with a reducing agent.
反応式は下記の通りである。The reaction formula is as follows.
OC1g
DMF
・・・(3)式
そして、本発明においては、より厳しい使用条件に対処
し、かつ潤滑効果を持続させるために、上記カルボン酸
パーフルオロアルキルエステル中に重量比で30 ?
To〜70:30程度の配合比で極圧剤を併用する。OC1g DMF...Formula (3) And, in the present invention, in order to cope with more severe usage conditions and maintain the lubricating effect, the above carboxylic acid perfluoroalkyl ester is added at a weight ratio of 30?
An extreme pressure agent is used in combination at a blending ratio of about 70:30.
上記極圧剤は、境界潤滑領域において部分的に金属接触
を生じたとき、これに伴う摩擦熱によって金属面と反応
し、反応生成物被膜を形成することにより摩擦・摩耗防
止作用を行うものであって、リン系極圧剤、イオウ系極
圧剤、ハロゲン系極圧剤、を機金属系極圧剤、複合型極
圧剤等が知られている。When the extreme pressure agent makes partial metal contact in the boundary lubrication area, it reacts with the metal surface due to the accompanying frictional heat, forming a reaction product film to prevent friction and wear. Among these, phosphorus-based extreme pressure agents, sulfur-based extreme pressure agents, halogen-based extreme pressure agents, metal-based extreme pressure agents, composite type extreme pressure agents, etc. are known.
具体的に例示すれば、上記リン系極圧剤としては、トリ
ブチルホスフェート、トリオクチルホスフェート、トリ
ー2−エチルへキシルホスフェート、トリラウリルホス
フェート、トリオレイルホスフェート、ジブチルホスフ
ェート、ジオクチルホスフェート、ジー2−エチルへキ
シルホスフェート、ジラウリルホスフェート、ジオレイ
ルホスフェート等のリン酸エステル、トリブチルホスフ
ァイト、トリオクチルホスファイト、トリー2−エチル
へキシルホスファイト、トリラウリルホスファイト、ト
リオレイルホスファイト、ジブチルホスファイト ジオ
クチルホスファイト、ジー2−エチルへキシルホスファ
イト、ジラウリルホスファイト、ジオレイルホスファイ
ト等の亜リン酸エステル、ジブチルホスフェートブチル
アミン塩。Specifically, the phosphorus-based extreme pressure agents include tributyl phosphate, trioctyl phosphate, tri-2-ethylhexyl phosphate, trilauryl phosphate, trioleyl phosphate, dibutyl phosphate, dioctyl phosphate, and di-2-ethyl phosphate. Phosphate esters such as xyl phosphate, dilauryl phosphate, dioleyl phosphate, tributyl phosphite, trioctyl phosphite, tri-2-ethylhexyl phosphite, trilauryl phosphite, trioleyl phosphite, dibutyl phosphite, dioctyl phosphite , di-2-ethylhexyl phosphite, dilauryl phosphite, dioleyl phosphite and other phosphite esters, dibutyl phosphate butylamine salts.
ジブチルホスフェートオクチルアミン塩、ジブチルホス
フェ−1−ステアリルアミン塩、ジオクチルホスフェー
トブチルアミン塩、ジオクチルホスフェートオクチルア
ミン塩、ジオクチルホスフェートラウリルアミン塩、ジ
オクチルホスフェートステアリルアミン塩、ジー2−エ
チルへキシルホスフェートブチルアミン塩、ジー2−エ
チルヘキシルホスフェートオクチルアミン塩、ジー2−
エチルへキシルホスフェートラウリルアミン塩、ジー2
−エチルへキシルホスフェートステアリルアミン塩、ジ
ラウリルホスフェートブチルアミン塩。Dibutylphosphate octylamine salt, dibutylphosphate-1-stearylamine salt, dioctylphosphate butylamine salt, dioctylphosphate octylamine salt, dioctylphosphate laurylamine salt, dioctylphosphate stearylamine salt, di-2-ethylhexylphosphate butylamine salt, di-2-ethylhexylphosphate butylamine salt, 2-Ethylhexylphosphate octylamine salt, di-2-
Ethylhexylphosphate laurylamine salt, G2
-Ethylhexylphosphate stearylamine salt, dilaurylphosphate butylamine salt.
ジラウリルホスフェートオクチルアミン塩、ジラウリル
ホスフェートラウリルアミン塩、ジラウリルホスフェー
トステアリルアミン塩、ジオレイルホスフェートブチル
アミン塩、ジオレイルホスフェートオクチルアミン塩、
ジオレイルホスフェートラウリルアミン塩、ジオレイル
ホスフェートステアリルアミン塩等のリン酸エステルア
ミン塩が挙げられる。dilauryl phosphate octylamine salt, dilauryl phosphate traurylamine salt, dilauryl phosphate stearylamine salt, dioleyl phosphate butylamine salt, dioleyl phosphate octylamine salt,
Examples include phosphate ester amine salts such as dioleyl phosphate lauryl amine salt and dioleyl phosphate stearyl amine salt.
上記イオウ系極圧剤としては、硫化抹香鯨油、硫黄化ジ
ペンテン等不飽和結合を有する鉱油、油脂や脂肪酸等に
硫黄を加えて加熱することにより製造される硫化油脂類
、二硫化ジベンジル、二硫化ジフェニル、二硫化ジーも
一ブチル、二硫化ジー5ec−ブチル、二硫化ジ−n−
ブチル、二硫化ジ−t−オクチル、二硫化ジエチル等の
ジサルファイド類、硫化ベンジル、硫化ジフェニル、硫
化ジビニル、硫化ジメチル、硫化ジエチル、硫化ジ−t
−ブチル、硫化ジー5ec−ブチル、硫化ジ−n−ブチ
ル等のモノサルファイド類、三硫化ジメチル、三硫化ジ
−t−ブチル、ポリ硫化ジー1−ノニル、オレフィンポ
リサルファイド等のポリサルファイド類、一般式
%式%()
(但し、式中Rは炭化水素基を表す、)で示されるチオ
カーボネート類、元素硫黄等が挙げられる。The above-mentioned sulfur-based extreme pressure agents include mineral oils with unsaturated bonds such as sulfurized whale oil and sulfurized dipentene, sulfurized oils and fats produced by adding sulfur to fats and oils and fatty acids, and heating them, dibenzyl disulfide, and disulfide. Diphenyl, di-monobutyl disulfide, di-5ec-butyl disulfide, di-n-disulfide
Disulfides such as butyl, di-t-octyl disulfide, diethyl disulfide, benzyl sulfide, diphenyl sulfide, divinyl sulfide, dimethyl sulfide, diethyl sulfide, di-t-sulfide
- Monosulfides such as butyl, di-5ec-butyl sulfide, di-n-butyl sulfide, polysulfides such as dimethyl trisulfide, di-t-butyl trisulfide, di-1-nonyl polysulfide, and olefin polysulfide, general formula % Examples include thiocarbonates represented by the formula %( ) (wherein R represents a hydrocarbon group), elemental sulfur, and the like.
上記ハロゲン系極圧剤としては、臭化アリル。The halogen-based extreme pressure agent is allyl bromide.
臭化オクタデシル、臭化シクロヘキシル、臭化ステアリ
ル、臭化ベンジル等の臭素化合物、ヨウ化ベンジル、ヨ
ウ化アリル、ヨウ化ブチル、ヨウ化オクタデシル、ヨウ
化シクロヘキシル等のヨウ素化合物、ヘキサクロロエタ
ン、モノクロルエタン。Bromine compounds such as octadecyl bromide, cyclohexyl bromide, stearyl bromide, benzyl bromide, iodine compounds such as benzyl iodide, allyl iodide, butyl iodide, octadecyl iodide, cyclohexyl iodide, hexachloroethane, monochloroethane.
塩素化パラフィン、塩素化ジフェニル、塩素化油脂、メ
チルトリクロロステアレート、ペンタクロロペンタジェ
ン酸、ヘキサクロルナフテン酸化合物のエステル、ヘキ
サクロルナフテン酸化合物のイミドVA導体等の塩素化
合物が挙げられる。Examples include chlorine compounds such as chlorinated paraffin, chlorinated diphenyl, chlorinated oil and fat, methyl trichlorostearate, pentachloropentadienoic acid, ester of hexachloronaphthenic acid compound, and imide VA conductor of hexachloronaphthenic acid compound.
上記有機金属系極圧剤としては、ジイソブチルジチオリ
ン酸亜鉛、イソブチルペンチルジチオリン酸亜鉛、イソ
プロピル−1−メチルブチルジチオリン酸、イソブチル
ノニルフェニルジチオリン酸亜鉛、イソブチルヘプチル
フェニルジチオリン酸、ジヘプチルフェニルジチオリン
酸、ジノニルフェニルジチオリン酸亜鉛、モリブデンジ
チオフォスフェート等のチオリン酸塩類、ジメチルジチ
オカルバミン酸亜鉛、ジエチルジチオカルバミン酸亜鉛
、ジブチルジチオカルバミン酸亜鉛、エチルフェニルジ
チオカルバミン酸亜鉛、ジベンジルジチオカルバミン酸
亜鉛、ジメチルジチオカルバミン酸亜鉛、ジメチルジチ
オカルバミン鍍銅、ジメチルジチオカルバミン酸鉄、ジ
エチルジチオカルバミン酸セレン、ジエチルジチオカル
バミン酸銀等のチオカルバミン酸塩類、モリブデン、ア
ンチモン等の金属アルキルジチオカルバミン酸塩類、等
が挙げられる。Examples of the organometallic extreme pressure agents include zinc diisobutyldithiophosphate, zinc isobutylpentyldithiophosphate, isopropyl-1-methylbutyldithiophosphate, zinc isobutylnonylphenyldithiophosphate, isobutylheptylphenyldithiophosphate, diheptylphenyldithiophosphate, Zinc nonylphenyl dithiophosphate, thiophosphates such as molybdenum dithiophosphate, zinc dimethyldithiocarbamate, zinc diethyldithiocarbamate, zinc dibutyldithiocarbamate, zinc ethylphenyldithiocarbamate, zinc dibenzyldithiocarbamate, zinc dimethyldithiocarbamate, dimethyldithiocarbamate Examples include copper, thiocarbamates such as iron dimethyldithiocarbamate, selenium diethyldithiocarbamate, and silver diethyldithiocarbamate, and metal alkyldithiocarbamates such as molybdenum and antimony.
上記複合型極圧剤としては、ジー2−エチルヘキシルチ
オリン酸アミン等のジアルキルチオリン酸アミン類、塩
化プロピルホスフェート、臭化プロピルホスフェート、
ヨウ化プロピルホスフェート、塩化ブチルホスフェート
、臭化ブチルホスフェート、ヨウ化ブチルホスフェート
等に代表されるハロゲン化アルキルのリン酸エステル類
、クロロナフサザンテート等の他、一般式
(但し、各一般式中Rは水素原子またはアルキル基、ア
ルケニル基、アリール基を表す、)で示されるチオフォ
スフェート類、−a式(但し、式中Rは水素原子または
アルキル基、アルケニル基、アリール基を表す、)
で示されるチオフォスファイト類等が効果が高い。Examples of the composite extreme pressure agent include dialkylthiophosphate amines such as di-2-ethylhexylthiophosphate amine, propyl chloride, propyl bromide phosphate,
In addition to phosphoric acid esters of alkyl halides such as propyl iodide, butyl chloride, butyl bromide, butyl iodide, etc., chloronaphsasanthate, etc., general formulas (however, in each general formula, R represents a hydrogen atom or an alkyl group, an alkenyl group, or an aryl group); thiophosphates represented by the formula -a (wherein R represents a hydrogen atom or an alkyl group, an alkenyl group, or an aryl group) Thiophosphites, etc., are highly effective.
上述の極圧剤は単体で使用してもよいが、2種以上を混
合して使用することも可能である。The above-mentioned extreme pressure agents may be used alone, but it is also possible to use a mixture of two or more types.
上述のカルボン酸パーフルオロアルキルエステル及び極
圧剤の他、従来公知の潤滑剤を混合して用い、さらに使
用温度帯域の拡大等を図るようにしてもよい。In addition to the above-mentioned carboxylic acid perfluoroalkyl ester and extreme pressure agent, a conventionally known lubricant may be used in combination to further expand the usable temperature range.
使用される潤滑剤としては、脂肪酸またはその金属塩、
脂肪酸アミド、脂肪酸エステル、脂肪族アルコールまた
はそのアルコキシド、脂肪族アミン、多価アルコール、
ツルとタンエステル、マンニラタンエステル、硫黄化脂
肪酸、脂肪族メルカプタン、変性シリコーンオイル、パ
ーフルオロアルキルエチレンオキシド、パーフルオロポ
リエーテル類、高級アルキルスルホン酸またはその金属
塩、パーフルオロアルキルスルホン酸またはそのアンモ
ニウム塩あるいはその金属塩、パーフルオロアルキルカ
ルボン酸またはその金属塩、バーフルオロアルキルカル
ボン酸エステル等が例示される。The lubricants used include fatty acids or their metal salts;
Fatty acid amide, fatty acid ester, fatty alcohol or its alkoxide, fatty amine, polyhydric alcohol,
Vine and tan esters, manniratan esters, sulfurized fatty acids, aliphatic mercaptans, modified silicone oils, perfluoroalkyl ethylene oxides, perfluoropolyethers, higher alkyl sulfonic acids or their metal salts, perfluoroalkyl sulfonic acids or their ammonium salts Examples include metal salts thereof, perfluoroalkylcarboxylic acids or metal salts thereof, and perfluoroalkylcarboxylic acid esters.
特に、一般式C、F !A−I COOR(但し、式中
nは6〜10の整数を表し、Rは炭素数1〜25の炭化
水素基を表す。)で示されるパーフルオロアルキルカル
ボン酸エステルも低温特性が良好であることから、上記
カルボン酸パーフルオロアルキルエステルと併用するの
に好適である。In particular, general formulas C, F! Perfluoroalkylcarboxylic acid esters represented by A-I COOR (where n represents an integer of 6 to 10 and R represents a hydrocarbon group having 1 to 25 carbon atoms) also have good low-temperature properties. Therefore, it is suitable for use in combination with the above carboxylic acid perfluoroalkyl ester.
また、必要に応じて防錆剤を併用してもよい。Moreover, a rust preventive agent may be used in combination as necessary.
使用可能な防錆剤としては、通常この種の磁気記録媒体
の防錆剤として使用されるものであれば如何なるもので
もよく、例えば二価フェノール。As the rust preventive agent that can be used, any rust preventive agent that is normally used as a rust preventive agent for this type of magnetic recording medium may be used, such as dihydric phenol.
アルキルフェノールあるいはニトロソフェノール、等の
フェノール類、純ナフトール又はニトロ、ニトロソ、ア
ミノ、ハロゲノ置換ナフトール等のナフトール類、メチ
ルキノン、ヒドロキシキノン。Phenols such as alkylphenol or nitrosophenol, naphthols such as pure naphthol or nitro-, nitroso-, amino-, or halogeno-substituted naphthol, methylquinone, hydroxyquinone.
アミノキノン、ニトロキノン又はハロゲキノキン等のキ
ノン類、ベンゾフェノン及びその誘導体であるヒドロキ
シヘンシフエノン、アミノベンゾフェノン等のジアリー
ルケトン、アクリジン、4−キノリツール、キヌレン酸
又はリボフラビン等の窒素原子を含む複素環化合物、ト
コフェロール又はグアノシン等の酸素原子を含む複素環
化合物、スルホラン、スルホレン又はビチオン等の硫黄
原子を含む複素環化合物、チオフェノール、ジチゾン又
はチオオキシン等のメルカプト基を有する化合物、エン
タチオ酸又はルベアン酸等のチオカルボン酸またはその
塩、ジアゾスルフィド又はベンゾチアゾリン等のチアゾ
ール系化合物等が挙げられる。上記防錆剤は、潤滑剤と
混合させて用いてもよいが、例えば強磁性金属薄膜の表
面に先ず上記防錆剤を塗布し、しかる後潤滑剤を塗布す
るというように、2層以上に分けて被着すると効果が高
い。Quinones such as aminoquinone, nitroquinone or halogen quinone, diaryl ketones such as benzophenone and its derivatives hydroxyhemsiphenone and aminobenzophenone, acridine, 4-quinolitool, heterocyclic compounds containing a nitrogen atom such as kynurenic acid or riboflavin, tocopherol or Heterocyclic compounds containing an oxygen atom such as guanosine, heterocyclic compounds containing a sulfur atom such as sulfolane, sulfolene or bithione, compounds having a mercapto group such as thiophenol, dithizone or thiooxin, thiocarboxylic acids such as entathioic acid or rubeanic acid, or Salts thereof, diazosulfide, thiazole compounds such as benzothiazoline, etc. can be mentioned. The above-mentioned rust preventive agent may be used in combination with a lubricant, but for example, the above-mentioned rust preventive agent is first applied to the surface of a ferromagnetic metal thin film, and then a lubricant is applied thereto. It is more effective if applied separately.
これらカルボン酸パーフルオロアルキルエステルを含存
する潤滑剤層を強磁性金属gIM上に付着させる方法と
しては、上記潤滑剤を溶媒に溶解して得られた溶液を強
磁性金属薄膜の表面に塗布もしくは噴霧するか、あるい
は逆にこの溶液中に強磁性金171m Bを浸漬し乾燥
すればよい。A method for depositing a lubricant layer containing these carboxylic acid perfluoroalkyl esters on a ferromagnetic metal gIM is to apply or spray a solution obtained by dissolving the above lubricant in a solvent onto the surface of a ferromagnetic metal thin film. Alternatively, ferromagnetic gold 171mB may be immersed in this solution and dried.
ここで、その塗布量は、0.5■/lyl〜100■/
ITrであるのが好ましく、1■/−〜20■/dであ
るのがより好ましい、この塗布量があまり少なすぎると
、摩擦係数の低下、耐摩耗性・耐久性の向上という効果
が顕れず、一方あまり多すぎると、摺動部材と強磁性金
属薄膜との間ではりつき現象が起こり、却って走行性が
悪くなる。Here, the coating amount is 0.5■/lyl to 100■/lyl
ITr is preferable, and 1■/- to 20■/d is more preferable. If this coating amount is too small, the effects of lowering the friction coefficient and improving wear resistance and durability will not be realized. On the other hand, if the amount is too large, a sticking phenomenon will occur between the sliding member and the ferromagnetic metal thin film, which will actually worsen running performance.
本発明が適用される磁気記録媒体は、非磁性支持体上に
磁性層として強磁性金属iWaを設けたものであるが、
ここで非磁性支持体の素材としては、ポリエチレンテレ
フタレート等のポリエステル類、ポリエチレン、ポリプ
ロピレン等のポリオレフィン類、セルローストリアセテ
ート、セルロースダイアセテート、セルロースアセテー
トブチレート等のセルロース誘導体、ポリ塩化ビニル、
ポリ塩化ビニリデン等のビニル系樹脂、ポリカーボネー
ト、ポリイミド、ポリアミドイミド等のプラスチック、
アルミニウム合金、チタン合金等の軽金属、アルミナガ
ラス等のセラミックス等が挙げられる。The magnetic recording medium to which the present invention is applied is one in which a ferromagnetic metal iWa is provided as a magnetic layer on a nonmagnetic support.
Examples of materials for the nonmagnetic support include polyesters such as polyethylene terephthalate, polyolefins such as polyethylene and polypropylene, cellulose derivatives such as cellulose triacetate, cellulose diacetate, and cellulose acetate butyrate, polyvinyl chloride,
Vinyl resins such as polyvinylidene chloride, plastics such as polycarbonate, polyimide, polyamideimide,
Examples include light metals such as aluminum alloys and titanium alloys, and ceramics such as alumina glass.
この非磁性支持体の形態としては、フィルム、シート、
ディスク、カード、ドラム等のいずれでもよい。The forms of this non-magnetic support include film, sheet,
It may be a disk, card, drum, etc.
上記非磁性支持体には、その表面に山状突起やしわ状突
起1粒状突起等の突起を1種以上を形成し、表面粗さを
コントロールしてもよい。The surface roughness of the non-magnetic support may be controlled by forming one or more types of protrusions such as mountain-like protrusions or wrinkle-like protrusions on the surface of the non-magnetic support.
上記山状突起は、例えば高分子フィルム製膜時に粒径5
00〜3000人程度の無機微粒子を内添することによ
り形成され、高分子フィルム表面からの高さは100〜
1000人、密度はおよそlXl0’〜toxto’個
/鰭2とする。山状突起を形成するために使用される無
機微粒子としては、炭酸カルシウム(CaCOs)やシ
リカ、アルミナ等が好適である。For example, the above-mentioned mountain-like protrusions have a particle size of 5 when forming a polymer film.
It is formed by internally adding inorganic fine particles of about 0.00 to 3000, and the height from the polymer film surface is 100 to 3000.
1000 individuals, density approximately lXl0' to toxto' individuals/2 fins. Calcium carbonate (CaCOs), silica, alumina, etc. are suitable as the inorganic fine particles used to form the mountain-like protrusions.
上記しわ状突起は、例えば特定の混合溶媒を用いた樹脂
の希gI溶液を塗布乾燥することにより形成される起伏
であって、その高さは0.01〜108m、好ましくは
0.03〜0.5μm、突起間の最短間隔はO,1〜2
011mとする。このしわ状突起を形成するための樹脂
としては、ポリエチレンテレフタレート8ポリエチレン
ナフタレート等の飽和ポリエステル、ポリアミド、ポリ
スチロール、ポリカーボネート、ポリアクリレート、ポ
リスルホン、ポリエーテルスルホン、ポリ塩化ビニル、
ポリ塩化ビニリデン、ポリビニルブチラール、ポリフェ
ニレンオキサイド、フェノキシ樹脂等の各種樹脂の単体
、混合体または共重合体であり、可溶性溶剤を有するも
のが通している。そして、これらの樹脂をその良溶媒に
溶解せしめた樹脂濃度1〜10001)l)Ifの溶液
に、その樹脂の貧溶媒であって前記良溶媒より高い沸点
を有する溶媒を樹脂に対して1G−100倍量添加した
溶液を、高分子フィルムの表面に塗布・乾燥することに
より、非常に微細なしわ状凹凸を有する薄層を得ること
ができる。The wrinkle-like protrusions are undulations formed by applying and drying a dilute gI solution of resin using a specific mixed solvent, and the height thereof is 0.01 to 108 m, preferably 0.03 to 0.0 m. .5μm, the shortest distance between protrusions is O,1~2
011m. Examples of the resin for forming the wrinkled projections include saturated polyesters such as polyethylene terephthalate 8 polyethylene naphthalate, polyamides, polystyrene, polycarbonates, polyacrylates, polysulfones, polyethersulfones, polyvinyl chloride,
It is a single substance, a mixture, or a copolymer of various resins such as polyvinylidene chloride, polyvinyl butyral, polyphenylene oxide, and phenoxy resin, and those having a soluble solvent are used. Then, to a solution of these resins dissolved in the good solvent with a resin concentration of 1 to 10001) If, a solvent that is a poor solvent for the resin and has a boiling point higher than the good solvent is added at 1 G- By applying a solution added in 100 times the amount to the surface of a polymer film and drying it, a thin layer having very fine wrinkle-like irregularities can be obtained.
粒状突起は、アクリル樹脂等の有機超微粒子またはシリ
カ、金属粉等の無機微粒子を球状あるいは半球状に付着
させることにより形成される。この粒状突起の高さは、
50〜500人、密度は1XIOh〜50X10−個/
fl富程度とする。The granular protrusions are formed by attaching organic ultrafine particles such as acrylic resin or inorganic fine particles such as silica or metal powder in a spherical or semispherical shape. The height of this granular protrusion is
50 to 500 people, density 1XIOh to 50X10-pieces/
fl wealth level.
これら突起の少なくとも一種以上を形成すれば磁性層で
ある強磁性金属薄膜の表面性が制御されるが、2種以上
を組み合わせることにより効果が増し、特に山伏突起を
設けたベースフィルム上にしわ状突起とつぶ状突起を形
成すれば、極めて耐久性、走行性が改善される。The surface properties of the ferromagnetic metal thin film that is the magnetic layer can be controlled by forming at least one type of these protrusions, but the effect is enhanced by combining two or more types. By forming protrusions and bulge-like protrusions, durability and running properties are greatly improved.
この場合、突起の全体としての高さは、100〜200
0人の範囲内であることが好ましく、その密度は1m”
当り平均でlXl0’−IXIO’個であることが好ま
しい。In this case, the overall height of the protrusion is 100 to 200
Preferably within the range of 0 people, the density is 1m”
It is preferable that the number is 1X10'-IXIO' on average.
また、上記磁性層である強磁性金属薄膜は、真空蒸着法
やイオンブレーティング法、スパッタリング法等の真空
薄膜形成技術により連続膜として形成される。Further, the ferromagnetic metal thin film that is the magnetic layer is formed as a continuous film by a vacuum thin film forming technique such as a vacuum evaporation method, an ion blating method, or a sputtering method.
上記真空蒸着法は、10−4〜10−@Torrの真空
下で強磁性金属材料を抵抗加熱、高周波加熱、電子ビー
ム加熱等により蒸発させ、ディスク基板上に蒸発金属(
強磁性金属材料)を沈着するというものであり、−aに
高い抗磁力を得るため基板に対して上記強磁性金属材料
を斜めに蒸着する斜方蒸着法が採用される。あるいは、
より高い抗磁力を得るために酸素雰囲気中で上記蒸着を
行うものも含まれる。In the vacuum evaporation method described above, a ferromagnetic metal material is evaporated under a vacuum of 10-4 to 10-Torr by resistance heating, high-frequency heating, electron beam heating, etc., and the evaporated metal (
In order to obtain a high coercive force, an oblique evaporation method is adopted in which the ferromagnetic metal material is deposited obliquely to the substrate. or,
It also includes those in which the above-mentioned vapor deposition is performed in an oxygen atmosphere in order to obtain higher coercive force.
上記イオンブレーティング法も真空蒸着法の一種であり
、1O−4〜l O−”Torrの不活性ガス雰囲気中
でDCグロー放電、RFFa−放電を起こして、放電中
で上記強磁性金属材料を蒸発させるというものである。The above-mentioned ion brating method is also a type of vacuum evaporation method, in which DC glow discharge and RFFa-discharge are caused in an inert gas atmosphere of 1 O-4 to 1 O-'' Torr, and the above-mentioned ferromagnetic metal material is deposited during the discharge. It is evaporated.
上記スパッタリング法は、10−”〜l O−’Tor
rのアルゴンガスを主成分とする雰囲気中でグロー放電
を起こし、生じたアルゴンガスイオンでターゲット表面
の原子をたたき出すというものであり、グロー放電の方
法により直流2極、3極スパツタ法や、高周波スパッタ
法、またはマグネトロン放電を利用したマグネトロンス
パッタ法等がある。The above sputtering method uses 10-" to l O-'Tor
A glow discharge is caused in an atmosphere mainly composed of argon gas, and the generated argon gas ions are used to knock out atoms on the target surface. There are sputtering methods, magnetron sputtering methods using magnetron discharge, and the like.
このスパッタリング法による場合には、CrやW。In the case of this sputtering method, Cr or W is used.
V等の下地膜を形成しておいてもよい。A base film such as V may be formed in advance.
なお、上記いずれの方法においても、基板上にあらかじ
めBi、Sb、Pb、Sn、Ga、In。In any of the above methods, Bi, Sb, Pb, Sn, Ga, and In are preliminarily deposited on the substrate.
Cd、Ge、Si、Tl1等の下地金属層を被着形成し
ておき、基板面に対して垂直方向から成膜することによ
り、磁気異方性の配向かなく面内等方法に優れた磁性層
を形成することができ、例えば磁気ディスクとする場合
には好適である。By pre-depositing a base metal layer such as Cd, Ge, Si, Tl1, etc., and forming the film from a direction perpendicular to the substrate surface, excellent magnetic properties can be achieved in the in-plane direction without magnetic anisotropy orientation. It is suitable for forming a layer, for example, into a magnetic disk.
このような真空薄膜形成技術により金属磁性薄膜を形成
する際に、使用される強磁性金属材料としては、Fe、
Co、Ni等の金属の他に、C。When forming a metal magnetic thin film using such vacuum thin film forming technology, the ferromagnetic metal materials used include Fe,
In addition to metals such as Co and Ni, C.
−Ni合金、Co−Pt合金、Co−Ni−Pt合金、
Fe−Co合金、Fa−Ni合金、Fe−Co−Ni合
金、Fe−Go−B合金、Co−N1−Fe−B合金、
Go−Cr合金あるいはこれらにCr、An等の金属が
含有されたもの等が挙げられる。特に、Co−Cr合金
を使用した場合には、垂直磁化膜が形成される。-Ni alloy, Co-Pt alloy, Co-Ni-Pt alloy,
Fe-Co alloy, Fa-Ni alloy, Fe-Co-Ni alloy, Fe-Go-B alloy, Co-N1-Fe-B alloy,
Examples include Go-Cr alloys and those containing metals such as Cr and An. In particular, when a Co--Cr alloy is used, a perpendicularly magnetized film is formed.
このような手法により形成される磁性層の膜厚は、0.
04〜1μm程度である。The thickness of the magnetic layer formed by such a method is 0.
It is about 0.04 to 1 μm.
また、非磁性支持体の磁性層が設けられる面とは反対側
に、いわゆるバックコート層を形成してもよい、バック
コート層は、塩化ビニル−酢酸ビニル、フェノール樹脂
又はボリフフ化ビニル並びにポリウレタン樹脂又はブタ
ジェン系共重合体等の結合剤樹脂とit性を付与するた
めのカーボン系微粉末又は表面粗度のコントロール及び
耐久性向上のために添加される無機顔料等の粉末成分と
をアセトン、メチルエチルケトン又はベンゼン等の有機
溶媒に混合分散させたバンクコート用塗料を非磁性支持
体面に塗布することにより形成される。In addition, a so-called back coat layer may be formed on the side of the non-magnetic support opposite to the side on which the magnetic layer is provided. Alternatively, a binder resin such as a butadiene copolymer and a powder component such as a carbon-based fine powder to impart IT properties or an inorganic pigment added to control surface roughness and improve durability are combined with acetone, methyl ethyl ketone, etc. Alternatively, it can be formed by applying a bank coating paint mixed and dispersed in an organic solvent such as benzene to the surface of a non-magnetic support.
前述のバンクコート層には潤滑剤を使用してもよい、こ
の場合、上記バックコート層中に潤滑剤を内添する方法
、あるいはバンクコート層上に潤滑剤を被着する方法が
ある。いずれにしても、上記潤滑剤としては、脂肪酸、
脂肪酸エステル、脂肪酸アミド、金属石鹸、脂肪族アル
コール、パラフィン、シリコーン等従来より周知の潤滑
剤が使用できる。A lubricant may be used in the bank coat layer. In this case, the lubricant may be internally added to the back coat layer, or the lubricant may be deposited on the bank coat layer. In any case, the above-mentioned lubricants include fatty acids,
Conventionally known lubricants such as fatty acid esters, fatty acid amides, metal soaps, fatty alcohols, paraffins, and silicones can be used.
カルボン酸パーフルオロアルキルエステル及び極圧剤を
含む潤滑剤層は、強磁性金属薄膜上にトップコート層と
して形成することにより良好な潤滑作用を発揮して摩擦
係数を低減する。特に、カルボン酸パーフルオロアルキ
ルエステルは、低温下においても良好な潤滑効果を発揮
する。A lubricant layer containing a carboxylic acid perfluoroalkyl ester and an extreme pressure agent exhibits a good lubricating effect and reduces the coefficient of friction by being formed as a top coat layer on a ferromagnetic metal thin film. In particular, carboxylic acid perfluoroalkyl esters exhibit good lubricating effects even at low temperatures.
〔実施例〕
以下、本発明の具体的な実施例について説明するが、本
発明はこれら実施例に限定されるものではない。[Examples] Specific examples of the present invention will be described below, but the present invention is not limited to these examples.
先ず、以下の合成例にしたがってカルボン酸パーフルオ
ロアルキルエステルを合成した。First, a carboxylic acid perfluoroalkyl ester was synthesized according to the following synthesis example.
合成例 市販のオレイン酸、リノール酸、リルン酸。Synthesis example Commercially available oleic acid, linoleic acid, lylunic acid.
ミリスチン酸、パルミチン酸をそれぞれ五塩化リン(P
C1%)あるいは塩化チオニル(SOCIg)で塩素化
し、相当するカルボン酸クロライドを得た。なお、プク
ン酸クロライドは市販のものを使用した。Myristic acid and palmitic acid are each converted into phosphorus pentachloride (P).
C1%) or thionyl chloride (SOCIg) to obtain the corresponding carboxylic acid chloride. Note that a commercially available pucunyl chloride was used.
一方、ペンタデカフルオロオクタン酸あるいはノナデカ
フルオロデカン酸をジメチルホルムアミド(DMF)を
触媒として塩化チオニル(SOCI□)で塩素化した後
、水素化リチウムアルミニウムで還元してペンタデカフ
ルオロ−1−オクタツール及びノナデカフルオロ−1−
デカノールを合成した。On the other hand, pentadecafluorooctanoic acid or nonadecafluorodecanoic acid is chlorinated with thionyl chloride (SOCI□) using dimethylformamide (DMF) as a catalyst, and then reduced with lithium aluminum hydride to produce pentadecafluoro-1-octatool. and nonadecafluoro-1-
Synthesized decanol.
次いで、上記ペンタデカフルオロ−1−オクタツールあ
るいはノナデカフルオロ−1−デカノールをトリエチル
アミンとともにクロロホルムに溶解させ、水冷下で先に
合成したカルボン酸クロライドのいずれか1種を30分
かけて滴下した0滴下終了後、−晩常温で攪拌した。こ
れを水、5%希塩酸、l’Ja)(C0w水溶液、水の
順で洗浄した後、真空蒸留して精製した。Next, the above pentadecafluoro-1-octatool or nonadecafluoro-1-decanol was dissolved in chloroform together with triethylamine, and one of the carboxylic acid chlorides synthesized earlier was added dropwise over 30 minutes under water cooling. After completion of the dropwise addition, the mixture was stirred at room temperature overnight. This was washed with water, 5% diluted hydrochloric acid, 1'Ja) (C0w aqueous solution, and water), and purified by vacuum distillation.
以上の合成方法に従い、カルボン酸クロライドの種類を
変えて化合物を8種類合成した。According to the above synthesis method, eight types of compounds were synthesized by changing the type of carboxylic acid chloride.
生成物の確認は、赤外分光分析(IR)及び質量分析(
MASS)によって行った1例えばオレイン酸ペンタデ
カフルオロオクチルエステルの場合には、1360〜1
100c鵬−1にかけてCF結合特有の吸収が見られる
こと、1760cm−’にエステルのC=0の吸収が見
られること、3020cs+−’及び2930c+e−
’にCIの伸縮振動による吸収が見ら九ること、等から
確認した。また質量分析によるマススペクトルで、66
4の分子イオンピークM゛が存在することも、この構造
を支持している。なお、上記質量分析は、日本電子社製
。Confirmation of the product was performed using infrared spectroscopy (IR) and mass spectrometry (
For example, in the case of oleic acid pentadecafluorooctyl ester, 1360-1
Absorption peculiar to CF bond is observed at 100c Peng-1, absorption of C=0 of ester is observed at 1760cm-', 3020cs+-' and 2930c+e-
It was confirmed from the fact that absorption due to CI stretching vibration was observed in '. In addition, the mass spectrum obtained by mass spectrometry shows that 66
The presence of the molecular ion peak M′ of 4 also supports this structure. The above mass spectrometer is manufactured by JEOL Ltd.
質量分析計DX303を用いて行い、ガスクロマトグラ
フにより単一成分であることを確認してから測定した。The measurement was performed using a mass spectrometer DX303, and the measurement was performed after confirming that it was a single component using a gas chromatograph.
実施例
14μm厚のポリエチレンテレフタレートフィルムに斜
め蒸着法によりCoを被着さ廿、膜厚1000人の強磁
性金属薄膜を形成した。Example 1 Co was deposited on a polyethylene terephthalate film having a thickness of 4 μm by oblique vapor deposition to form a ferromagnetic metal thin film having a thickness of 1000 μm.
次に、この強磁性金属薄膜表面上に、先の合成例で合成
したカルボン酸パーフルオロアルキルエステル0.48
gを800gのフレオンに溶解し、それに極圧剤を1
;1の割合で添加した溶液を塗布し、8m−幅に裁断し
てサンプルテープを作成した。各実施例で使用したカル
ボン酸パーフルオロアルキルエステルの種類及び掻圧剤
名を第1表(11及び第1表(2)に示す。Next, 0.48% of the carboxylic acid perfluoroalkyl ester synthesized in the previous synthesis example was placed on the surface of this ferromagnetic metal thin film.
Dissolve g in 800 g of freon and add 1 lb of extreme pressure agent to it.
A sample tape was prepared by applying a solution added at a ratio of 1:1 and cutting it into a width of 8 m. The type of carboxylic acid perfluoroalkyl ester and the name of the scratching agent used in each example are shown in Table 1 (11) and Table 1 (2).
(以下余白)
第1表(1)
第1表(2)
作成された各サンプルテープについて、温度25℃、相
対湿度(RH)50%、および−5℃の各条件下での動
g擦係数及びシャトル耐久性を測定した。この動摩擦係
数は、材質がステンレス(SUS304)のガイリピン
を用い、一定のテンションをかけ5 as/secの速
度で送り、試験したものである。また、シャトル耐久性
は、1回につき2分間のシャトル走行を行い、出力が一
3dB低下までのシャトル回数で評価した。メチル耐久
性はポーズ状態での出力の一3dBまでの減衰時間を評
価した。結果を第2表+11及び第2表(2)に示す。(Leaving space below) Table 1 (1) Table 1 (2) Dynamic g-friction coefficient for each sample tape created under the conditions of 25°C, 50% relative humidity (RH), and -5°C and shuttle durability was measured. This dynamic friction coefficient was tested by using a gyrip pin made of stainless steel (SUS304) and feeding it at a speed of 5 as/sec under a constant tension. In addition, the shuttle durability was evaluated by running the shuttle for 2 minutes each time, and determining the number of shuttle runs until the output decreased by 13 dB. Methyl durability was evaluated by evaluating the decay time for the output to -3 dB in a pause state. The results are shown in Table 2 +11 and Table 2 (2).
第2表(1)
第2表(2)
この表からも明らかなように、本発明の各実施例は、常
温、低温の各条件下で動摩擦係数が小さく、走行が極め
て安定しており、また100回往復走行後もテープ表面
の損傷は全く見られなかった。また、耐久性も極めて良
く、150回シャトル走行を行っても出力の一3dB低
下は見られなかった。これに対して、潤滑剤層のない比
較例のテープでは、摩擦係数が往復走行回数が多くなる
につれて大となり、走行も不安定でテープの摩耗が見ら
れ、耐久性も悪いものであった。Table 2 (1) Table 2 (2) As is clear from this table, each example of the present invention has a small dynamic friction coefficient under both normal temperature and low temperature conditions, and the running is extremely stable. Further, even after running back and forth 100 times, no damage was observed on the tape surface. Furthermore, the durability was extremely good, and even after 150 shuttle runs, no decrease in output by 13 dB was observed. On the other hand, in the tape of the comparative example without a lubricant layer, the friction coefficient increased as the number of reciprocating runs increased, running was unstable, tape wear was observed, and durability was poor.
以上の説明からも明らかなように、本発明においては、
強磁性金属F4膜型の磁気記録媒体上にカルボン酸パー
フルオロアルキルエステル及び掻圧剤を含むトップコー
ト層を形成しているので、如何なる温度条件下において
も動摩擦係数を小さくすることができ、走行安定性や耐
摩耗性に優れた磁気記録媒体とすることができる。As is clear from the above description, in the present invention,
Since a top coat layer containing carboxylic acid perfluoroalkyl ester and a scratching agent is formed on the ferromagnetic metal F4 film type magnetic recording medium, the coefficient of dynamic friction can be reduced under any temperature conditions, making it possible to A magnetic recording medium with excellent stability and wear resistance can be obtained.
特に、カルボン酸パーフルオロアルキルエステルの凝固
点温度が低いことから、低温下での使用時に効果が大き
い。In particular, since the freezing point temperature of carboxylic acid perfluoroalkyl ester is low, it is highly effective when used at low temperatures.
Claims (1)
金属薄膜上にカルボン酸パーフルオロアルキルエステル
及び極圧剤を含むトップコート層を形成したことを特徴
とする磁気記録媒体。A magnetic recording medium comprising: a ferromagnetic metal thin film formed on a non-magnetic support; and a top coat layer containing a carboxylic acid perfluoroalkyl ester and an extreme pressure agent formed on the ferromagnetic metal thin film.
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP61079516A JPS62236120A (en) | 1986-04-07 | 1986-04-07 | Magnetic recording medium |
CA 524293 CA1297738C (en) | 1986-01-09 | 1986-12-02 | Magnetic recording medium |
AU66047/86A AU585102B2 (en) | 1986-01-09 | 1986-12-03 | Magnetic recording medium |
AT87100060T ATE87389T1 (en) | 1986-01-09 | 1987-01-05 | MAGNETIC RECORDING CARRIER. |
DE87100060T DE3784948T2 (en) | 1986-01-09 | 1987-01-05 | Magnetic record carrier. |
EP87100060A EP0229014B1 (en) | 1986-01-09 | 1987-01-05 | Magnetic recording medium |
US07/001,044 US4735848A (en) | 1986-01-09 | 1987-01-07 | Magnetic recording medium |
KR1019870000073A KR0134786B1 (en) | 1986-01-09 | 1987-01-08 | Magnetic recording medium |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP61079516A JPS62236120A (en) | 1986-04-07 | 1986-04-07 | Magnetic recording medium |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS62236120A true JPS62236120A (en) | 1987-10-16 |
Family
ID=13692136
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP61079516A Pending JPS62236120A (en) | 1986-01-09 | 1986-04-07 | Magnetic recording medium |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS62236120A (en) |
-
1986
- 1986-04-07 JP JP61079516A patent/JPS62236120A/en active Pending
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