WO2023181959A1 - 磁気ディスクの製造方法および潤滑剤溶液 - Google Patents

磁気ディスクの製造方法および潤滑剤溶液 Download PDF

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Publication number
WO2023181959A1
WO2023181959A1 PCT/JP2023/009015 JP2023009015W WO2023181959A1 WO 2023181959 A1 WO2023181959 A1 WO 2023181959A1 JP 2023009015 W JP2023009015 W JP 2023009015W WO 2023181959 A1 WO2023181959 A1 WO 2023181959A1
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Prior art keywords
lubricant
perfluoropolyether
magnetic disk
group
solvent
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English (en)
French (fr)
Japanese (ja)
Inventor
豪 清水
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Moresco Corp
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Moresco Corp
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Priority to US18/848,680 priority Critical patent/US20250226005A1/en
Priority to CN202380028473.XA priority patent/CN118891676A/zh
Priority to JP2024509980A priority patent/JP7714120B2/ja
Publication of WO2023181959A1 publication Critical patent/WO2023181959A1/ja
Anticipated expiration legal-status Critical
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    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/62—Record carriers characterised by the selection of the material
    • G11B5/72—Protective coatings, e.g. anti-static or antifriction
    • G11B5/725—Protective coatings, e.g. anti-static or antifriction containing a lubricant, e.g. organic compounds
    • G11B5/7253—Fluorocarbon lubricant
    • G11B5/7257—Perfluoropolyether lubricant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/32—Polymers modified by chemical after-treatment
    • C08G65/329—Polymers modified by chemical after-treatment with organic compounds
    • C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/50—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing halogen
    • C10M105/54—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing halogen containing carbon, hydrogen, halogen and oxygen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/38—Lubricating compositions characterised by the base-material being a macromolecular compound containing halogen
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/62—Record carriers characterised by the selection of the material
    • G11B5/72—Protective coatings, e.g. anti-static or antifriction
    • G11B5/725—Protective coatings, e.g. anti-static or antifriction containing a lubricant, e.g. organic compounds
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/04—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen
    • C10M2213/043—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C10M2213/0606—Perfluoro polymers used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/64—Environmental friendly compositions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/74—Noack Volatility
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/14—Electric or magnetic purposes
    • C10N2040/18—Electric or magnetic purposes in connection with recordings on magnetic tape or disc
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/015—Dispersions of solid lubricants
    • C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating

Definitions

  • the present invention relates to a method for manufacturing a magnetic disk and a lubricant solution.
  • a magnetic disk in a magnetic recording/reproducing device generally has an underlayer, a magnetic layer, a protective layer, and a lubricant layer formed in this order on a nonmagnetic substrate.
  • the mainstream method for forming a lubricant layer is to apply it by dipping using a solution prepared by diluting a lubricant with a fluorine-based solvent.
  • highly polar perfluoropolyether compounds having a functional group such as a hydroxyl group, an aromatic ring, or a phosphazene at the end of a perfluoropolyether skeleton as a lubricant.
  • the solvent for diluting the lubricant must have sufficient dissolving power to dissolve the lubricant, be liquid at room temperature, and have high volatility in order to form a uniform film.
  • the material be nonflammable.
  • fluorine-based solvents for diluting magnetic disk lubricants include HFC (hydrofluorocarbon) Vertrel (Mitsui Chemours Fluoro Products Co., Ltd., registered trademark) XF and HFE (hydrofluoroether) Novec (3M Co., Ltd.). (registered trademark) 7100 etc. are used.
  • a lubricant coating liquid is prepared by dissolving a perfluoropolyether compound having a perfluorotrimethyleneoxy repeating unit in the main chain and a perfluoropolyether compound having a cyclic triphosphazene structure in Vertrel XF. It is disclosed that a magnetic disk substrate is prepared and immersed in a lubricant coating liquid to form a lubricant layer.
  • Patent Document 2 discloses that a lubricant layer is formed by immersing a magnetic disk in a solution in which a lubricant containing a phosphazene compound is dissolved in perfluorohexyl methyl ether (HFE-7100).
  • Patent Document 3 discloses that a perfluoropolyether lubricant having a cyclic triphosphazene end group in the molecule was diluted using HFE-7100 as a solvent and applied onto a protective layer by a dip coating method. ing.
  • One aspect of the present invention provides a method for manufacturing a magnetic disk and a lubricant solution using a fluorinated solvent that has a low global warming potential and excellent solubility of a highly polar perfluoropolyether lubricant.
  • the purpose is to
  • one embodiment of the present invention includes the following configuration.
  • a method for manufacturing a magnetic disk according to an embodiment of the present invention includes a lubricant application step of applying a lubricant solution containing a perfluoropolyether lubricant to the surface of the magnetic disk.
  • the solvent used in the lubricant solution contains hydrofluoroether (HFE) having a structure represented by the following formula (A) and having a 100-year global warming potential (GWP) of less than 1000.
  • HFE hydrofluoroether
  • Ra represents either F, CF 2 -Re or CF 3.
  • Rb represents either O-Rd or C(-Rf) 3.
  • Rc represents H, F and CF3 .
  • Re and Rd each independently represent a hydrocarbon group that may be partially substituted with a fluorine atom, and at least one carbon atom in the main chain is an oxygen atom.
  • Rf each independently represents any one of a hydrocarbon group, H, and F that may be partially substituted with a fluorine atom; At least one carbon atom in the main chain of the optionally substituted hydrocarbon group may be substituted with an oxygen atom.
  • a lubricant solution according to an embodiment of the present invention is a lubricant solution containing a perfluoropolyether-based lubricant, and the solvent used in the lubricant solution has a structure of the following formula (A). and contains hydrofluoroethers with a 100-year global warming potential of less than 1000.
  • Ra represents either F, CF 2 -Re or CF 3.
  • Rb represents either O-Rd or C(-Rf) 3.
  • Rc represents H, F and CF3 .
  • Re and Rd each independently represent a hydrocarbon group that may be partially substituted with a fluorine atom, and at least one carbon atom in the main chain is an oxygen atom.
  • Rf each independently represents any one of a hydrocarbon group, H, and F that may be partially substituted with a fluorine atom; At least one carbon atom in the main chain of the optionally substituted hydrocarbon group may be substituted with an oxygen atom.
  • a method for manufacturing and lubricating a magnetic disk using a fluorinated solvent that has a low global warming potential and has excellent solubility in a highly polar perfluoropolyether lubricant solvent can be provided.
  • FIG. 1 is a cross-sectional view showing the configuration of a magnetic disk in an embodiment of the present invention.
  • FIG. 1 is a cross-sectional view showing the configuration of a magnetic disk in an embodiment of the present invention.
  • Vertrel registered trademark
  • HFC hydrofluorocarbon
  • a method for manufacturing a magnetic disk according to an embodiment of the present invention includes a lubricant application step of applying a lubricant solution containing a perfluoropolyether lubricant to the surface of the magnetic disk.
  • the solvent used in the lubricant solution contains HFE having the structure of the following formula (A) and having a GWP 100 year value of less than 1000.
  • Ra represents either F, CF 2 -Re or CF 3.
  • Rb represents either O-Rd or C(-Rf) 3.
  • Rc represents H, F and CF3 .
  • Re and Rd each independently represent a hydrocarbon group that may be partially substituted with a fluorine atom, and at least one carbon atom in the main chain is an oxygen atom.
  • Rf each independently represents any one of a hydrocarbon group, H, and F that may be partially substituted with a fluorine atom; At least one carbon atom in the main chain of the optionally substituted hydrocarbon group may be substituted with an oxygen atom.
  • the solvent used in the lubricant solution has the structure of the above formula (A) and has a GWP 100 year value of less than 1000. Contains HFE. According to this configuration, a method for manufacturing a magnetic disk using a fluorine-based solvent having a low GWP and excellent solubility in the solvent of a highly polar perfluoropolyether lubricant, and a method for lubricating the magnetic disk. A drug solution can be provided. Furthermore, the solvent has excellent evaporability comparable to Vertrel XF, which is currently mainly used, and can form a uniform lubricating layer.
  • the solvent having the above structure provides an additional effect of improving the adsorption of the lubricant layer to the magnetic disk.
  • the solvent having the above structure has a high contact angle with water, n-hexadecane, etc. on the lubricating layer, and has a small surface energy of the lubricating layer.
  • a lubricating layer such as water or n-hexadecane having a high contact angle and a low surface energy has the advantage of being able to prevent contamination of the magnetic disk surface.
  • HFE refers to a compound containing an ether structure having hydrogen atoms partially substituted with fluorine atoms.
  • the HFE may have a structure represented by the following formula (A).
  • Ra represents either F, CF 2 -Re or CF 3.
  • Rb represents either O-Rd or C(-Rf) 3.
  • Rc represents H, F and CF3 .
  • Re and Rd each independently represent a hydrocarbon group that may be partially substituted with a fluorine atom, and at least one carbon atom in the main chain is an oxygen atom.
  • Rf each independently represents any one of a hydrocarbon group, H, and F that may be partially substituted with a fluorine atom; At least one carbon atom in the main chain of the optionally substituted hydrocarbon group may be substituted with an oxygen atom.
  • HFE has a structure represented by general formula (A) in its molecule, it can dissolve highly polar perfluoropolyether lubricants. This is because the hydrogen atoms bonded to the carbon atoms bonded to Ra, Rb, and Rc in general formula (A) are biased toward positive charges because they are surrounded by Ra, Rb, and Rc, which may contain many fluorine atoms. It's for a reason. It is presumed that this is because the hydrogen atoms form hydrogen bonds with the polar groups of the highly polar perfluoropolyether lubricant, improving the affinity between the lubricant and HFE.
  • the HFE is not particularly limited as long as it has the above structure, but for example, Rd-O-CH 2 F, Rd-O-CHF 2 , Rd-O-CHFCF 3 , Rd-O- CH2CF2 - Re, Rd-O- CHFCF2 -Re, Rd-O-CH( CF3 ) CF2 -Re, Rd-O - CH2CF3 , Rd-O-CH( CF3 ) 2 , C(-Rf) 3 -CH 2 F, C(-Rf) 3 -CHF 2 , C(-Rf) 3 -CHFCF 3 , C(-Rf) 3 -CH 2 CF 2 -Re, C(-Rf) 3 -CHFCF 2 -Re, C(-Rf) 3 -CH(CF 3 )CF 2 -Re, C(-Rf) 3 -CH(CF 3 )CF 2 -Re, C(-Rf) 3 -CH(CF 3
  • Re and Rd are each independently a hydrocarbon group having 1 to 10 carbon atoms, more preferably 1 to 5 carbon atoms, and still more preferably 1 to 3 carbon atoms, which may be partially substituted with a fluorine atom. be. At least one carbon atom in the main chain may be substituted with an oxygen atom. In addition, when at least one carbon atom in the main chain is substituted with an oxygen atom, the substituted oxygen atom is also considered to be a carbon atom and is counted as the number of carbon atoms in the hydrocarbon group (in Rf below). is the same).
  • Rf each independently represents any one of a hydrocarbon group optionally substituted with a fluorine atom, H, and F; may have at least one carbon atom in the main chain substituted with an oxygen atom.
  • at least one of Rf is a hydrocarbon group that may be partially substituted with the fluorine atom, and at least one of the carbon atoms in the main chain may be substituted with an oxygen atom.
  • Rf each independently represents a hydrocarbon group having 1 to 10 carbon atoms, more preferably 1 to 5 carbon atoms, and even more preferably 1 to 3 carbon atoms, which may be partially substituted with a fluorine atom, H, and F.
  • the hydrocarbon group which represents any of the above and may be partially substituted with a fluorine atom at least one carbon atom in the main chain may be substituted with an oxygen atom.
  • at least one of Rf is a hydrocarbon group having 1 to 10 carbon atoms, more preferably 1 to 5 carbon atoms, and still more preferably 1 to 3 carbon atoms, which may be partially substituted with the fluorine atom.
  • At least one carbon atom in the main chain may be substituted with an oxygen atom.
  • one of Rf is a hydrocarbon group that may be partially substituted with the fluorine atom, and at least one of the carbon atoms in the main chain is optionally substituted with an oxygen atom, and Rf It is more preferable that the other two are each independently either H or F.
  • the above-mentioned HFEs can be used alone or in combination of two or more types.
  • HFE HFE
  • 1,1,2,2-tetrafluoroethyl 2,2,2-trifluoroethyl ether 1,1,2,3,3,3-hexafluoropropyl Methyl ether, 1,1,1,3,3,3-hexafluoro-2-methoxypropane (hexafluoroisopropyl methyl ether), methyl 2,2,3,3,3-pentafluoropropyl ether, ethyl 1,1 , 2,2-tetrafluoroethyl ether, ethyl 1,1,2,3,3,3-hexafluoropropyl ether and the like.
  • the HFE is a compound whose GWP 100-year value is less than 1000.
  • GWP refers to the GWP according to the IPCC Fifth Assessment Report, which means that when a unit mass (e.g., 1 kg) of greenhouse gas is released into the atmosphere, within a certain period of time (e.g., This is the estimated value of the integrated value of radiant energy given to the earth over the next 100 years as a ratio to carbon dioxide. Therefore, the larger the value of GWP, the greater the negative impact on global warming, and the smaller the value of GWP, the smaller the negative impact on global warming.
  • GWP values are published based on different time scales such as 20 years, 100 years, and 500 years, the 100-year GWP value is generally used.
  • the GWP 100-year value of the HFE is preferably less than 1000, more preferably less than 900, even more preferably less than 800, even more preferably less than 700, and most preferably less than 600. be.
  • the boiling point of the HFE is preferably 30°C to 100°C, more preferably 35°C to 90°C, even more preferably 40°C to 80°C. It is preferable that the boiling point of the HFE is 100° C. or lower, since the drying properties of the solvent after coating on the disk are excellent. Further, it is preferable that the boiling point of the HFE is 30° C. or higher, since there is less significant concentration change in the solution containing the lubricant due to evaporation of the solvent.
  • the HFE is preferably nonflammable from the viewpoint of safety in the manufacturing process.
  • nonflammability refers to a standard based on JIS method K2265.
  • the HFE has three or more carbon-hydrogen bonds. As a result, since it is a liquid at room temperature, it is suitable for the dipping method, and furthermore, the 100-year global warming potential value tends to be low.
  • the solvent used in the lubricant solution may contain the above-mentioned HFE, but may contain other solvents as long as the effects of the present invention are not adversely affected.
  • an organic solvent not containing a fluorine atom can be used as the other solvent.
  • the organic solvent not containing a fluorine atom include alcohols such as methanol, ethanol, n-propyl alcohol, isopropyl alcohol, t-butanol, and n-butanol; ketones; ethers; dimethyl sulfoxide; dimethyl formamide, etc. .
  • the overall GWP can be reduced according to an embodiment of the present invention.
  • the content of the other solvent is not limited to this, but based on the total amount of the solvent, preferably 30% by weight or less, more preferably 20% by weight or less, still more preferably 10% by weight or less, especially Preferably it is 5% by weight or less.
  • the perfluoropolyether lubricant used as a lubricant is a perfluoropolyether compound having the structure of the following formula (1). It is preferable that it contains.
  • x is a real number from 0 to 3
  • y is a real number from 0 to 1
  • z, l, m, n, and o are each a real number from 0 to 15, provided that x, Either one of y is a real number of 1 or more, and at least one of z, l, m, n, or o is a real number of 1 or more.
  • the above formula (1) includes, for example, Demnam skeleton: -CF 2 CF 2 O- (CF 2 CF 2 CF 2 O) m CF 2 CF 2 -, Fomblin skeleton: -CF 2 O- (CF 2 O) z (CF 2 CF 2 O) l CF 2 -, C2 skeleton: -CF 2 O- (CF 2 CF 2 O) l CF 2 -, C4 skeleton: -CF 2 CF 2 CF 2 O- (CF 2 CF 2 CF 2 CF 2 O) n CF 2 CF 2 CF 2 -, Krytox skeleton: CF(CF 3 )O-(CF(CF 3 )CF 2 O) o CF(CF 3 )-, and the like.
  • z, l, m, n, and o are real numbers from 1 to 15. Note that in the Fomblin skeleton, CF 2 O and CF 2 CF 2 O may be randomly repeated.
  • the perfluoropolyether compound preferably has at least one structure represented by formula (1) in the molecule. That is, the perfluoropolyether compound may have two or more structures represented by formula (1) in the molecule. In that case, two or more of the structures represented by formula (1) may be bonded via any organic group. Examples of the organic group include an aliphatic hydrocarbon group and an aromatic hydrocarbon group. The aliphatic hydrocarbon group and aromatic hydrocarbon group may have an ether bond and/or a hydroxyl group.
  • R 2 is an organic group having a perfluoropolyether skeleton.
  • R 2 is, for example, a perfluoropolyether skeleton represented by the above formula (1), and as described above, two or more of the structures represented by the formula (1) are bonded via an arbitrary organic group. You can leave it there.
  • R 1 and R 3 are each independently an organic group having a fluorine atom, hydroxyl group, halogenated alkyl group, alkoxy group, carboxyl group, amino group, ester group, amide group, aryl group, or phosphazene at the end.
  • R 1 and R 3 are each independently -F, -CH 2 OH, -CH 2 OCH 2 CH(OH)CH 2 OH, -CH 2 OCH 2 CH(OH)CH 2 OCH 2 CH(OH )CH 2 OH, -CH 2 O(CH 2 ) g OH, -CH 2 OCH 2 CH(OH)CH 2 OC 12 H 9 O, -CH 2 OCH 2 CH(OH)CH 2 OC 10 H 7 , or CH2OCH2CH ( OH ) CH2OC6H4 - R4 .
  • g is a real number from 1 to 10
  • examples of R 4 include a hydrogen atom, a hydroxyl group, an alkoxy group having 1 to 4 carbon atoms, an amino group, and an amide residue.
  • R 4 is preferably a hydroxyl group or an alkoxy group.
  • examples of perfluoropolyether compounds in which two or more perfluoropolyether skeletons are bonded via an arbitrary organic group include a compound represented by the following formula (4).
  • R 1 -R 5 -R 6 -R 7 -R 3 ...(4) R 5 and R 7 are organic groups having a perfluoropolyether skeleton, for example, the perfluoropolyether skeleton represented by the above formula (1).
  • R 6 is any organic group, such as an aliphatic hydrocarbon group or an aromatic hydrocarbon group.
  • the aliphatic hydrocarbon group and aromatic hydrocarbon group may have an ether bond and/or a hydroxyl group.
  • R 1 and R 3 are the same organic groups as in formula (2).
  • the number average molecular weight of the perfluoropolyether compound is not particularly limited, but is preferably from 500 to 6,000, more preferably from 700 to 4,000.
  • the number of hydroxyl groups in one molecule of the perfluoropolyether compound is also not limited, but is preferably 1 to 10, more preferably 2 to 8, and even more preferably 4 to 8.
  • the number average molecular weight of the perfluoropolyether compound is a value measured by 19 F-NMR using JNM-ECX400 manufactured by JEOL. In NMR measurements, the sample itself is used for measurement without diluting the sample with a solvent. A known peak that is part of the skeletal structure of the perfluoropolyether compound is used as a standard for chemical shift.
  • the perfluoropolyether compound may be a perfluoropolyether compound satisfying the following formula (3). NOH /(Mn/1500) ⁇ 2...(3)
  • N OH represents the number of hydroxyl groups in one molecule of the perfluoropolyether compound
  • Mn represents the number average molecular weight of the perfluoropolyether compound.
  • the solvent described in [1.1] above can be suitably used for any perfluoropolyether lubricant, but is particularly suitable for highly polar perfluoropolyether compounds that satisfy formula (3). It can be suitably used.
  • a highly polar perfluoropolyether compound that satisfies formula (3) has low solubility in HFE, but is well soluble in the solvent described in [1.1] above.
  • the solvents described in .1] are very effective.
  • the perfluoropolyether compound may be used alone, or two or more types may be used in combination.
  • Lubricant application step A method for manufacturing a magnetic disk according to an embodiment of the present invention includes applying a lubricant solution containing the above-mentioned perfluoropolyether lubricant and using the above-mentioned solvent as a solvent to the magnetic disk.
  • the lubricant is applied to the surface of the lubricant.
  • the lubricant solution may be any solution in which the above-mentioned perfluoropolyether lubricant is dissolved in the above-mentioned solvent.
  • the lubricant solution can be used as a recording medium lubricant for improving the sliding characteristics of a magnetic disk.
  • the concentration of the perfluoropolyether lubricant in the lubricant solution is preferably 0.001% to 1.0% by weight, more preferably 0.003% to 0.5% by weight, and 0.005% by weight. More preferably % by weight to 0.3% by weight. It is preferable that the concentration of the perfluoropolyether lubricant is 0.001% by weight or more, since by coating the disk with perfluoropolyether, the surface can be inactivated and sliding properties can be ensured. Further, if it is 1.0% by weight or less, the coating film becomes thinner, so it is preferable.
  • the lubricant solution only needs to contain the perfluoropolyether lubricant and the solvent, and more preferably consists of the perfluoropolyether lubricant and the solvent, but may also contain other components.
  • the other components include lubricants other than the perfluoropolyether lubricant, hydrocarbon lubricants, fatty acid ester lubricants, and the like.
  • the content of the other components is, for example, 10% by weight or less based on the total weight of the lubricant solution.
  • the lubricant solution is applied to the surface of the magnetic disk.
  • the magnetic disk includes, for example, a magnetic disk 1 shown in FIG. 1, a recording layer 4, a protective layer 3, and a lubricant layer 2 disposed on a nonmagnetic substrate 8.
  • the lubricant layer 2 contains the aforementioned lubricant.
  • the magnetic disk may include a lower layer 5 disposed under the recording layer 4, one or more soft magnetic lower layers 6 disposed under the lower layer 5, and one An adhesive layer 7 disposed under the above soft magnetic lower layer 6 may be included.
  • the lubricant solution is applied to the surface of the protective layer of a magnetic disk on which at least a recording layer and a protective layer are formed on a non-magnetic substrate to form a lubricant layer.
  • the method of applying the lubricant solution to the surface of the magnetic disk is not limited to this, but examples include a dipping method, a spin coating method, a spray method, a paper coating method, etc. can. Among these, the dipping method is more preferred.
  • the temperature of the lubricant solution when applying the lubricant solution to the surface of the magnetic disk is not particularly limited; From the viewpoint of minimizing the temperature of the lubricant solution during application, it is preferable that the temperature of the lubricant solution is 10°C to 40°C.
  • ultraviolet irradiation or heat treatment may be performed after applying the lubricant solution to the surface of the protective layer.
  • ultraviolet irradiation or heat treatment By performing ultraviolet irradiation or heat treatment, a stronger bond can be formed between the lubricant layer and the protective layer, and evaporation of the lubricant due to heating can be prevented.
  • ultraviolet irradiation it is recommended to use ultraviolet rays with a main wavelength of 185 nm or 254 nm in order to activate the interface between the lubricant and the protective layer without affecting the deep parts of the lubricant layer and the protective layer.
  • the temperature when performing the heat treatment is preferably 60 to 170°C, more preferably 80 to 170°C, and even more preferably 80 to 150°C.
  • the lubricant solution can be applied to the surface of the magnetic disk by immersing the magnetic disk in the lubricant solution and pulling it up.
  • the time for immersing the magnetic disk is not particularly limited, but is, for example, 1 minute to 10 minutes.
  • the speed at which the magnetic disk is pulled up after being immersed is not particularly limited, but is, for example, 0.5 mm/sec to 5 mm/sec.
  • the method for manufacturing a magnetic disk according to an embodiment of the present invention further includes a step of manufacturing a perfluoropolyether lubricant, a step of preparing the lubricant solution, and a step of preparing a lubricant solution on a non-magnetic substrate.
  • the method may include a step of forming a recording layer, a step of forming a protective layer on the recording layer, and the like.
  • Each layer of the magnetic disk other than the lubricating layer may include materials known in the art to be suitable for individual layers of a magnetic disk.
  • examples of the material for the recording layer include alloys in which chromium, platinum, tantalum, etc. are added to elements capable of forming ferromagnetic materials, such as iron, cobalt, and nickel, or oxides thereof.
  • examples of the material for the protective layer include carbon, Si 3 N 4 , SiC, SiO 2 and the like.
  • Examples of the material for the nonmagnetic substrate include aluminum alloy, glass, and polycarbonate.
  • the method for preparing the lubricant solution is also not particularly limited.
  • it can be prepared by dissolving the perfluoropolyether lubricant described above in the solvent.
  • the HFE used in the solvent may be one manufactured by a conventionally known method or a commercially available product.
  • the method for producing the perfluoropolyether lubricant is not particularly limited either, and any conventionally known method can be appropriately selected to produce the perfluoropolyether lubricant.
  • Lubricant solution One aspect of the present invention is a lubricant solution containing a perfluoropolyether lubricant, wherein the solvent used in the lubricant solution has a structure of the following formula (A). Also included are lubricant solutions containing HFE, and having a GWP 100 year value of less than 1000.
  • Ra represents either F, CF 2 -Re or CF 3.
  • Rb represents either O-Rd or C(-Rf) 3.
  • Rc represents H, F and CF3 .
  • Re and Rd each independently represent a hydrocarbon group that may be partially substituted with a fluorine atom, and at least one carbon atom in the main chain is an oxygen atom.
  • Rf is a hydrocarbon group that may be partially substituted with H, F, and fluorine atoms, and at least one carbon atom in the main chain is an oxygen atom. (May be replaced.)
  • perfluoropolyether lubricant solvent, and lubricant solution are as described in [1] above.
  • the lubricant solution can be used as a recording medium lubricant to improve the sliding characteristics of a magnetic disk.
  • it can also be used as a lubricant for recording media in other recording devices that involve sliding between a head and a recording medium such as a magnetic tape.
  • it can be used not only for recording devices but also as a lubricant for devices that have sliding parts.
  • a method for manufacturing a magnetic disk comprising a lubricant coating step of applying a lubricant solution containing a perfluoropolyether lubricant to the surface of the magnetic disk, wherein the solvent used in the lubricant solution is
  • a method for manufacturing a magnetic disk comprising a hydrofluoroether having a structure represented by the following formula (A) and a 100-year global warming potential of less than 1000.
  • Ra represents either F, CF 2 -Re or CF 3.
  • Rb represents either O-Rd or C(-Rf) 3.
  • Rc represents H, F and CF3 .
  • Re and Rd each independently represent a hydrocarbon group that may be partially substituted with a fluorine atom, and at least one carbon atom in the main chain is an oxygen atom.
  • Rf each independently represents any one of a hydrocarbon group, H, and F that may be partially substituted with a fluorine atom; At least one carbon atom in the main chain of the optionally substituted hydrocarbon group may be substituted with an oxygen atom.
  • R 1 -R 2 -R 3 ...(2)
  • R 2 is an organic group having a perfluoropolyether skeleton, and R 1 and R 3 each independently have a fluorine atom, a hydroxyl group, a halogenated alkyl group, an alkoxy group, or a carboxyl group at the end. , an organic group having an amino group, an ester group, an amide group, a phosphazene, or an aryl group.
  • [6] The production method according to [4] or [5], wherein the perfluoropolyether compound is a perfluoropolyether compound satisfying the following formula (3).
  • Ra represents either F, CF 2 -Re or CF 3.
  • Rb represents either O-Rd or C(-Rf) 3.
  • Rc represents H, F and CF3 .
  • Re and Rd each independently represent a hydrocarbon group that may be partially substituted with a fluorine atom, and at least one carbon atom in the main chain is an oxygen atom.
  • Rf each independently represents any one of a hydrocarbon group, H, and F that may be partially substituted with a fluorine atom; At least one carbon atom in the main chain of the optionally substituted hydrocarbon group may be substituted with an oxygen atom.
  • solvents used in the lubricant solutions in Examples and Comparative Examples are shown below.
  • Ra, Rb, and Rc represent Ra, Rb, and Rc in formula (A), and Rb is "O" when Rb is O-Rd, and Rb is C(-Rf ) If it is 3 , write “C”.
  • Solvent 1 1,1,2,2-tetrafluoroethyl 2,2,2-trifluoroethyl ether (CAS No. 406-78-0, manufactured by Tokyo Chemical Industry Co., Ltd.)
  • Solvent 2 1,1,2,3,3,3-hexafluoropropyl methyl ether (CAS No.
  • Solvent 3 1,1,1,3,3,3-hexafluoro-2-methoxypropane (hexafluoroisopropyl methyl ether) (CAS No. 13171-18-1, manufactured by Halocarbon)
  • Solvent 4 Methyl 2,2,3,3,3-pentafluoropropyl ether (CAS No. 378-16-5, manufactured by Tokyo Chemical Industry Co., Ltd.)
  • Solvent 5 Ethyl 1,1,2,2-tetrafluoroethyl ether (CAS No. 512-51-6, manufactured by Tokyo Chemical Industry Co., Ltd.)
  • Solvent 6 Ethyl 1,1,2,3,3,3-hexafluoropropyl ether (CAS No.
  • Solvent 7 1,1,1,2,3,4,4,5,5,5-decafluoropentane (Mitsui Chemours Fluoro Products Co., Ltd., Vertrel-XF)
  • Solvent 8 Methyl nonafluorobutyl ether, methyl nonafluoroisobutyl ether mixture (manufactured by 3M, Novec 7100)
  • Solvent 9 Ethyl nonafluorobutyl ether, ethyl nonafluoroisobutyl ether mixture (manufactured by 3M, Novec 7200)
  • Solvent 10 2,2,2-tolylfluoroethanol (manufactured by Tosoh F-Tech Co., Ltd.).
  • the evaluation of evaporability was performed using the following steps (1) to (4): (1) Place a Petri dish with a diameter of 28 mm and a depth of 15 mm on an electronic balance with a windshield, pour 2 ml of solvent into the Petri dish, and leave it at room temperature. (20°C to 25°C, the same applies hereinafter); (2) When 5 minutes, 10 minutes, 15 minutes, 20 minutes, 25 minutes, and 30 minutes have elapsed since the addition of the solvent, (3) The amount of weight loss per hour was calculated, and the average volume reduction rate (ml/min) was calculated from the calculated amount of weight loss and the density of the solvent; (4) Vertrel-XF was used as the solvent. The average volume reduction rate of Comparative Example 1 using was set as 1.0, and the relative volume reduction rate was calculated from the average volume reduction rate calculated in (3). The average volume reduction rate for Vertrel-XF was 0.028 ml/min.
  • the film thickness of the lubricant layer coating film formed by applying the lubricant solution was measured using the following steps (1) to (3): (1) A 2.5-inch magnetic film was placed in the lubricant solution.
  • the disk was immersed for 3 minutes, and the magnetic disk was lifted vertically upward from the solution at a pulling speed of 1 mm/sec so that the pulling direction was parallel to the magnetic disk surface to form a lubricating layer coating;
  • FT - Using IR manufactured by Bruker, VERTEX70
  • the distance from the center of the magnetic disk is 15 mm (indicated as "ID” in Table 1) and 20 mm (indicated as “MD” in Table 1) ), and 25 mm (indicated as "OD” in Table 1)
  • the IR intensity was measured at three points, and the film thickness at the three points was calculated from a calibration curve of the film thickness measured with an ellipsometer and the IR intensity.
  • the contact angle of the lubricant coating film was measured using the following steps (1) to (3): (1) A 2.5-inch magnetic disk was immersed in the lubricant solution for 3 minutes, and the pulling speed was adjusted. The disk was lifted vertically upward from the solution at a rate of 1 mm/sec so that the pulling direction was parallel to the surface of the magnetic disk to form a lubricant coating film with a thickness of about 13 ⁇ . The film thickness was measured using the same method as for measuring the film thickness of the lubricant coating film, and the average value of the measured film thicknesses was taken as the film thickness; (2) The magnetic disk on which the lubricant coating film was formed was placed at room temperature.
  • a magnetic disk on which a lubricant coating film was prepared in the same manner as for measuring the contact angle was immersed in Vertrel-XF for 5 minutes, and then lifted vertically upward at 1 mm/sec so that the pulling direction was parallel to the magnetic disk surface.
  • the thickness of the lubricant coating film remaining on the magnetic disk was measured.
  • the film thickness of the lubricant coating film was measured using FT-IR (manufactured by Bruker, VERTEX70).
  • Example 1 The perfluoropolyether compound was dissolved in Solvent 1 at room temperature to a concentration of 1000 ppm on a mass basis to prepare a lubricant solution. The lubricant solubility of the obtained lubricant solution was evaluated. Evaporability was evaluated using Solvent 1 as it was.
  • Example 2 and 3 The lubricant solutions of Examples 2 and 3 were prepared in the same manner as in Example 1, except that Solvent 1 was changed to Solvent 2 and Solvent 3, respectively, and the solubility of the lubricants was evaluated. Regarding Solvent 3, the film thickness was also evaluated. Evaporability was evaluated using Solvents 2 and 3 as they were.
  • a lubricant solution was prepared in the same manner as in Example 1, except that the perfluoropolyether compound was separately dissolved in Solvent 3 to a concentration of 500 ppm on a mass basis.
  • a lubricant layer coating film was formed using this separately prepared lubricant solution, and the obtained lubricant coating film was subjected to adsorption evaluation, contact angle measurement, and surface energy calculation as Example 3.
  • Example 4 to 6 The lubricant solutions of Examples 4 to 6 were prepared in the same manner as in Example 1, except that Solvent 1 was changed to Solvents 4 to 6, respectively, and the solubility of the lubricants was evaluated. Evaporability was evaluated using each of Solvents 4 to 6 as is.
  • Comparative example 1 A lubricant solution of Comparative Example 1 was prepared in the same manner as in Example 1 except that Solvent 1 was changed to Solvent 7, and the solubility of the lubricant was evaluated and the film thickness was measured. Evaporability was evaluated using Solvent 7 as it was.
  • a lubricant solution was prepared in the same manner as in Example 1, except that the perfluoropolyether compound was separately dissolved in Solvent 7 to a concentration of 500 ppm on a mass basis.
  • a lubricant layer coating film was formed using this separately prepared lubricant solution, and the contact angle was measured, surface energy was calculated, and adsorption properties were evaluated for the obtained lubricant coating film.
  • Lubricant solutions of Comparative Examples 2 to 4 were prepared in the same manner as in Example 1, except that Solvent 1 was changed to Solvents 8 to 10, respectively, and the solubility and evaporability of the lubricants were evaluated.
  • Solvent 10 Comparative Example 4
  • the film thickness was measured, the contact angle was measured, the surface energy was calculated, and the adsorption property was evaluated. Evaporability was evaluated using Solvents 8 to 10 as they were.
  • the solvents used in Examples 1 to 6 have a low GWP of less than 1000, and have a small impact on global warming. Furthermore, the solvent used in Examples 1 to 6 was HFE, similar to the solvent used in Comparative Examples 2 to 3, but surprisingly it was not able to dissolve the highly polar perfluoropolyether lubricant. It has been shown. Thus, it can be seen that the solvents used in Examples 1 to 6 have low GWP and are excellent in solubility of highly polar perfluoropolyether lubricants.
  • Vertrel XF of Comparative Example 1 which is currently mainly used, has excellent solubility for highly polar perfluoropolyether lubricants, but has a large GWP.
  • the solvents used in Examples 1 to 6 had evaporabilities within the range of 1.0 ⁇ 0.5, based on Vertrel XF of Comparative Example 1, which is currently mainly used. Since these solvents evaporate very quickly, they can be used as solvents for lubricant solutions without any problems as long as they are within the above range.
  • the solvent of Comparative Example 4 which was not HFE, had an evaporability of 0.2, and was found to have a slower evaporation rate than Examples 1 to 6 and Comparative Example 1.
  • Example 3 the variation in film thickness of the formed lubricant layer coating film at three points outward from the center of the magnetic disk was small, and was comparable to the variation when Vertrel XF was used in Comparative Example 1. It has been shown.
  • Comparative Example 4 in which a solvent other than HFE was used, droplets were observed to be generated on the outside (OD) of the magnetic disk, making it impossible to measure the film thickness. For this reason, Comparative Example 4 cannot be used as a lubricant solution. Note that there is a correlation between the evaporability and the variation in film thickness.
  • Example 1 If the evaporability is high, the solution adhering to the disk pulled up from the lubricant solution will quickly evaporate, and the lubricant solution will not drip and accumulate at the bottom of the disk, resulting in a uniform film thickness.
  • Example 1 the variation in film thickness at three points from the center to the outside of the magnetic disk was not measured, but since the evaporation property was similar to that in Example 3, Example 3 It is expected that similar results will be obtained.
  • Example 3 showed a smaller change in film thickness before and after washing than Comparative Examples 1 and 4. That is, it was shown that the lubricating layer formed in Example 3 had high adsorption to the magnetic disk. Furthermore, in Example 3, compared to Comparative Examples 1 and 4, it was shown that the contact angle with water was particularly high and the surface energy was low. That is, it was found that the lubricant layer formed in Example 3 could better prevent contamination of the magnetic disk surface.
  • a fluorinated solvent having a low GWP and excellent solubility in a highly polar perfluoropolyether lubricant solvent is used.
  • a method of manufacturing a magnetic disk and a lubricant solution may be provided. Therefore, it can be advantageously used in manufacturing magnetic disks.
  • HFE used in the magnetic disk manufacturing method and lubricant solution according to an embodiment of the present invention has a low GWP and has a small burden on the earth.
  • low GWP solvents for the HDD industry as a whole the negative effects of global warming can be minimized. This will contribute to achieving Goal 13 of the Sustainable Development Goals (SDGs), ⁇ Take concrete measures to combat climate change.''
  • Magnetic disk 2 Lubricating layer 3 Protective layer 4 Recording layer 5 Lower layer 6 Soft magnetic lower layer 7 Adhesive layer 8 Nonmagnetic substrate

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JP2008075000A (ja) * 2006-09-22 2008-04-03 Asahi Glass Co Ltd 磁気記録媒体用潤滑剤溶液
JP2020132688A (ja) * 2019-02-14 2020-08-31 セントラル硝子株式会社 溶剤組成物
WO2021024585A1 (ja) * 2019-08-06 2021-02-11 株式会社Moresco 潤滑剤溶液、磁気ディスクおよびその製造方法

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Publication number Priority date Publication date Assignee Title
JP2008075000A (ja) * 2006-09-22 2008-04-03 Asahi Glass Co Ltd 磁気記録媒体用潤滑剤溶液
JP2020132688A (ja) * 2019-02-14 2020-08-31 セントラル硝子株式会社 溶剤組成物
WO2021024585A1 (ja) * 2019-08-06 2021-02-11 株式会社Moresco 潤滑剤溶液、磁気ディスクおよびその製造方法

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