WO2017183314A1 - FILM DE BxNyCzOw, PROCÉDÉ DE FORMATION DE FILM, SUPPORT D'ENREGISTREMENT MAGNÉTIQUE, ET SON PROCÉDÉ DE FABRICATION - Google Patents

FILM DE BxNyCzOw, PROCÉDÉ DE FORMATION DE FILM, SUPPORT D'ENREGISTREMENT MAGNÉTIQUE, ET SON PROCÉDÉ DE FABRICATION Download PDF

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Publication number
WO2017183314A1
WO2017183314A1 PCT/JP2017/007858 JP2017007858W WO2017183314A1 WO 2017183314 A1 WO2017183314 A1 WO 2017183314A1 JP 2017007858 W JP2017007858 W JP 2017007858W WO 2017183314 A1 WO2017183314 A1 WO 2017183314A1
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Prior art keywords
film
recording medium
magnetic recording
forming
gas
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PCT/JP2017/007858
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English (en)
Japanese (ja)
Inventor
阿部　浩二
利行 渡邊
裕康 関野
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株式会社ユーテック
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Priority to JP2018513045A priority Critical patent/JP7129083B2/ja
Publication of WO2017183314A1 publication Critical patent/WO2017183314A1/fr

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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
    • 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
    • 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
    • G11B5/726—Two or more protective coatings
    • G11B5/7262—Inorganic protective coating
    • G11B5/7264—Inorganic carbon protective coating, e.g. graphite, diamond like carbon or doped carbon
    • G11B5/7266—Inorganic carbon protective coating, e.g. graphite, diamond like carbon or doped carbon comprising a lubricant over the inorganic carbon coating
    • 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

Definitions

  • FIG. 6 is a cross-sectional view for explaining a conventional method of manufacturing a magnetic recording medium.
  • a film formation substrate 100 in which at least a magnetic layer 102 is formed on a nonmagnetic substrate 101 is prepared, and a DLC (Diamond Like Carbon) film 103 having a thickness of 3 nm is formed on the film formation substrate 100 by plasma CVD ( Chemical vapor deposition) is used to form a film.
  • a CN film 104 having a thickness of 1 nm is formed on the DLC film 103 by sputtering.
  • the fomblin oil is applied on the CN film 104 by dipping the CN film 104 into the fluorine-based fomblin oil.
  • the film formation substrate 100 is annealed at a temperature of 150 ° C. for 1 hour, whereby a 4 nm-thick fluorinated organic film 105 that functions as a solid lubricant is formed on the CN film 104.
  • a vapor deposition method may be used as a method for forming the fluorinated organic film 105, and the vapor deposition temperature in that case is 110 ° C.
  • the reason why the DLC film 103 is formed by the plasma CVD method in the above magnetic recording medium is as follows.
  • impurities such as Co are dissolved from the magnetic layer 102 and reach the fluorinated organic film 105 (so-called corrosion). Therefore, by forming the DLC film by the plasma CVD method, it is possible to form a DLC film having a higher density than that of sputtering. Therefore, even when the film thickness is 3 nm, sufficient barrier properties to prevent corrosion are ensured. Can do.
  • the reason why the CN film 104 is formed in the magnetic recording medium is as follows. Since the contact angle of water with the DLC film 103 is about 80 °, the adhesion between the DLC film 103 and the fluorinated organic film 105 is poor when the fluorinated organic film 105 is applied on the DLC film 103. For this reason, the fluorinated organic film 105 cannot be applied on the DLC film 103. Therefore, by forming a CN film 104 having a water contact angle of about 30 ° between the DLC film 103 and the fluorinated organic film 105, the adhesion between the DLC film 103 and the fluorinated organic film 105 is improved. be able to. However, the CN film 104 does not have a barrier function for preventing corrosion.
  • the water contact angle on the surface of the B x N y C z O w film is 50 ° or less (preferably, by satisfying the formulas (1) to (5)) 30 ° or less, more preferably 15 ° or less, and more preferably 5 ° or less.
  • the B x N y C z O w film has a surface with a water contact angle of 50 ° or less (preferably 30 ° or less, more preferably 15 ° or less, more preferably 5 ° or less). B x N y C z O w film.
  • a magnetic recording medium comprising:
  • a magnetic recording medium further comprising a DLC film formed between the B x N y C z O w film and the magnetic layer.
  • the fluorinated organic film includes a C a F b film, a C a F b N c film, a C a F b H d film, a C a F b O e film, a C a F b O e H d film, and a C a F b N c O e film and C a F b N c O e H d magnetic recording medium, which is a one of the membrane of the membrane.
  • a, b, c, d, and e are natural numbers.
  • any one of the films is 3 nm or less.
  • the fluorinated organic film includes a C a F b film, a C a F b N c film, a C a F b H d film, a C a F b O e film, a C a formed by a CVD method using a source gas.
  • F b O e H d membrane is any membrane C a F b N c O e film and C a F b N c O e H d film,
  • the method of manufacturing a magnetic recording medium, wherein the source gas includes an organic source gas containing carbon and fluorine.
  • a, b, c, d, and e are natural numbers.
  • the organic material gas is C 3 F 6 , C 4 F 6 , C 6 F 6 , C 6 F 12 , C 6 F 14 , C 7 F 8 , C 7 F 14 , C 7 F 16 , C 8 F 16 , C 8 F 18 , C 9 F 18 , C 9 F 20 , C 10 F 8 , C 10 F 18 , C 11 F 20 , C 12 F 10 , C 13 F 28 , C 15 F 32 , C 20 F 42 , and C 24 F 50 ,
  • the organic material gas is C 3 F 3 N 3 , C 3 F 9 N, C 5 F 5 N, C 6 F 4 N 2 , C 6 F 9 N 3, C 6 F 12 N 2, C 6 F 15 N, C 7 F 5 N, C 8 F 4 N 2, C 9 F 21 N, C 12 F 4 N 4, C 12 F 27 N,
  • FIG. 1 is a cross-sectional view for explaining a method of manufacturing a magnetic recording medium according to one embodiment of the present invention.
  • Figure 2 is a sectional view showing a plasma CVD apparatus for forming the B x N y C z O w film 14 shown in FIG. 1 schematically.
  • a film formation substrate 2 in which at least a magnetic layer 12 is formed on a nonmagnetic substrate 11 is prepared.
  • the deposition target substrate 2 is, for example, a bird disk substrate or a media head.
  • a B x N y C z O w film 14 having a thickness of 2 nm or less (preferably 1.5 nm or less, more preferably 1 nm or less, and even more preferably 0.5 nm) on the magnetic layer 12 is shown in FIG. Film formation is performed using a plasma CVD apparatus.
  • the contact angle of water on the surface of the B x N y C z O w film 14 is 50 ° or less (preferably 30 ° or less, more preferably 15 ° or less, more preferably 5 ° or less).
  • x, y, z, and w satisfy the following formulas (1) to (5), and preferably satisfy the following formulas (1 ′) to (2 ′) and (3) to (5).
  • the B x N y C z O w film 14 is dipped into the fluorine-based fomblin oil, so that the fomblin oil is applied on the B x N y C z O w film 14.
  • a 4 nm-thick fluorinated organic film 15 functioning as a solid lubricant is formed on the B x N y C z O w film 14. It is formed.
  • the water on the surface of the B x N y C z O w film 14 is formed by forming the B x N y C z O w film 14 satisfying the above formulas (1) to (5).
  • the contact angle can be set to 50 ° or less (preferably 30 ° or less, more preferably 15 ° or less, more preferably 5 ° or less). For this reason, sufficient adhesion between the fluorinated organic film 15 and the B x N y C z O w film 14 can be secured, and the fluorinated organic film 15 is peeled off from the B x N y C z O w film 14. Can be suppressed.
  • the B x N y C z O w film 14 contains almost no hydrogen, the B x N y C z O w film 14 becomes a dense film to prevent impurities from dissolving out of the magnetic layer 12 and reaching the fluorinated organic film 15 (so-called corrosion). It can have a barrier property. Therefore, by arranging the B x N y C z O w film 14 between the magnetic layer 12 and the fluorinated organic film 15, the thickness of the film between the magnetic layer 12 and the fluorinated organic film 15 prior Can be thinner than the ones.
  • the heat resistance can be improved.
  • the plasma CVD apparatus shown in FIG. 2 will be described.
  • the plasma CVD apparatus shown in FIG. 2 has a symmetrical structure with respect to the film formation substrate (for example, a disk substrate) 1 and can form films on both surfaces of the film formation substrate 1 simultaneously.
  • the plasma CVD apparatus includes a chamber 102, and filament-shaped first and second cathode electrodes (first and second cathode filaments) 103a and 103b made of, for example, tantalum are formed in the chamber 102. ing. Both ends of each of the first and second cathode filaments 103a and 103b are electrically connected to first and second cathode power sources (first and second AC power sources) 105a and 105b located outside the chamber 102. The first and second cathode power supplies 105 a and 105 b are arranged in an insulated state with respect to the chamber 102.
  • first and second cathode power supplies 105a and 105b for example, power supplies of 0 to 50 V and 10 to 50 A (ampere) can be used.
  • One ends of the first and second cathode power supplies 105 a and 105 b are electrically connected to the ground 106.
  • first and second anode electrodes (first and second anode cones) 104a having funnel-like shapes so as to surround the first and second cathode filaments 103a and 103b, respectively.
  • 104b is disposed, and each of the first and second anode cones 104a and 104b is shaped like a speaker.
  • the first anode cone 104 a is electrically connected to the positive potential side of the first anode power source (first DC (direct current) power source) 107 a, and the first DC power source 107 a is insulated from the chamber 102. It is arranged in the state. The negative potential side of the first DC power source 107 a is electrically connected to the ground 106.
  • the second anode cone 104 b is electrically connected to the positive potential side of the second anode power source (second DC (direct current) power source) 107 b, and the second DC power source 107 b is insulated from the chamber 102. It is arranged in the state.
  • the negative potential side of the second DC power source 107 b is electrically connected to the ground 106.
  • first and second DC power sources 107a and 107b for example, power sources of 0 to 500 V and 0 to 7.5 A (ampere) can be used.
  • a deposition target substrate 1 is disposed in the chamber 102, and this deposition target substrate 1 is opposed to the first and second cathode filaments 103a and 103b and the first and second anode cones 104a and 104b. Is arranged. Specifically, the first and second cathode filaments 103a and 103b are surrounded near the center of the inner peripheral surface of the first and second anode cones 104a and 104b, and the first and second anode cones 104a are surrounded. , 104b are arranged with the maximum inner diameter side facing the film formation substrate 1.
  • the deposition target substrate 1 is sequentially supplied to the positions shown by a holder (holding unit) not shown and a transfer device (handling robot or rotary index table) not shown.
  • a first plasma wall 108 a is disposed in the chamber 102 so as to cover the space between the first cathode filament 103 a and the first anode cone 104 a and the deposition target substrate 1, and the second cathode A second plasma wall 108b is disposed so as to cover the space between each of the filament 103b and the second anode cone 104b and the deposition target substrate 1.
  • Each of the first and second plasma walls 108 a and 108 b is electrically connected to a float potential (not shown), and is disposed in an insulated state with respect to the chamber 102.
  • the first and second plasma walls 108a and 108b have a cylindrical shape or a polygonal shape.
  • Film thickness correction plates 118a and 118b are provided at the ends of the first and second plasma walls 108a and 108b on the film formation substrate 1 side, and the film thickness correction plates 118a and 118b are electrically connected to the float potential. Connected. The thickness of the film formed on the outer peripheral portion of the deposition target substrate 1 can be controlled by the film thickness correction plates 118a and 118b.
  • First and second neodymium magnets 109a and 109b are disposed outside the chamber 102.
  • the first and second neodymium magnets 109a and 109b have, for example, a cylindrical shape or a polygonal shape, and the center of the cylindrical or polygonal inner diameter is the magnet center, and the magnet center is the first and second cathode filaments. They are positioned so as to face the approximate centers of 103a and 103b and the approximate center of the deposition target substrate 1, respectively.
  • Each of the first and second neodymium magnets 109a and 109b preferably has a magnetic force of 50G (Gauss) or more and 200G or less, more preferably 50G or more and 150G or less.
  • the plasma CVD apparatus has an evacuation mechanism (not shown) for evacuating the chamber 102.
  • the plasma CVD apparatus has a gas supply mechanism (not shown) for supplying a film forming material gas into the chamber 102.
  • This gas supply mechanism has a borazine supply source and a nitriding agent supply source for supplying a gas obtained by vaporizing borazine.
  • the gas supplied from the borazine supply source is adjusted in flow rate by the mass flow controller and supplied into the chamber 102.
  • the flow rate of the nitriding agent gas supplied from the nitriding agent supply source is adjusted by a mass flow controller and supplied into the chamber 102.
  • As the nitriding agent it is preferable to use ammonia or nitrogen.
  • the deposition target substrate 1 is held by a holding unit.
  • the evacuation mechanism is activated, the inside of the chamber 102 is brought into a predetermined vacuum state, and a gas obtained by vaporizing borazine (B 3 H 6 N 3 ) by the gas supply mechanism inside the chamber 102 and nitrogen gas as a nitriding agent are supplied.
  • the first and second cathode power sources 105a and 105b supply alternating currents to the first and second cathode filaments 103a and 103b, respectively.
  • the cathode filaments 103a and 103b are heated.
  • a direct current is supplied to the film formation substrate 1 by a DC power source 112. Further, a direct current is supplied from the first and second DC power sources 107a and 107b to the first and second anode cones 104a and 104b, respectively.
  • first and second cathode filaments 103a and 103b By heating the first and second cathode filaments 103a and 103b, a large amount of electrons are emitted from the first and second cathode filaments 103a and 103b toward the first and second anode cones 104a and 104b, respectively. Glow discharge is started between each of the first and second cathode filaments 103a and 103b and each of the first and second anode cones 104a and 104b.
  • the borazine gas and nitrogen gas inside the chamber 102 are ionized by a large amount of electrons to be in a plasma state.
  • a magnetic field is generated by the first and second neodymium magnets 109a and 109b in the regions where the borazine gas and the nitrogen gas are converted into plasma in the vicinity of the first and second cathode filaments 103a and 103b, respectively.
  • the plasma can be densified by this magnetic field, and ionization efficiency can be improved.
  • the deposition raw material molecules in the plasma state are directly accelerated by the negative potential of the deposition target substrate 1, fly toward the deposition target substrate 1, and adhere to the surface of the deposition target substrate 1. Is done. Thereby, the B x N y C z O w film 14 is formed on the deposition target substrate 1.
  • a film formation substrate 1 having at least a magnetic layer 12 formed on a nonmagnetic substrate 11 is prepared, and B x N y C z O w formed on the film formation substrate 1 is prepared. While forming a film 14 is not limited thereto and may be formed B x N y C z O w film 14 on another substrate. Various substrates can be used as the other substrate in this case, and for example, an electronic device may be used.
  • the B x N y C z O w film 14 is formed using the plasma CVD apparatus shown in FIG. 2, but other CVD apparatuses may be used.
  • FIG. 3 is a cross-sectional view for explaining a method of manufacturing a magnetic recording medium according to an aspect of the present invention.
  • the same reference numerals are given to the same parts as those in FIG. 1, and only different parts will be described.
  • the second embodiment is the same as the first embodiment except that a DLC film is formed between the magnetic layer 12 and the B x N y C z O w film 14. Specifically, a DLC film 13 having a thickness of 1 nm (preferably 0.5 nm) is formed on the deposition target substrate 1 by a CVD method. Next, the steps after forming the B x N y C z O w film 14 on the DLC film 13 are the same as those in the first embodiment.
  • the same effect as that of the first embodiment can be obtained.
  • impurities such as Cr are dissolved from the magnetic layer 12 into the high-density B x N y C z O w film 14 that does not contain hydrogen and reach the fluorinated organic film 15 (so-called corrosion). Therefore, the B x N y C z O w film 14 also has the barrier property that was conventionally given only to the DLC film 13, so that the DLC film 13 Corrosion can be prevented even if the thickness is reduced. As a result, the thickness of the film between the magnetic layer 12 and the fluorinated organic film 15 can be made thinner than the conventional one.
  • the film thickness of the B x N y C z O w film 14 may be 1 nm (preferably 0.5 nm).
  • the steps until the B x N y C z O w film 14 is formed on the magnetic layer 12 shown in FIG. 1 are the same as those in the first embodiment. omitted, illustrating the step of forming a fluorinated organic film 15 on the B x N y C z O w film 14 by using the plasma CVD apparatus shown in FIG.
  • This embodiment is the same as the first embodiment except for the step of forming the fluorinated organic film 15.
  • FIG. 4 is a cross-sectional view schematically illustrating a plasma CVD apparatus for forming a fluorinated organic film according to one embodiment of the present invention.
  • the plasma CVD apparatus has a chamber 2, and a holding electrode 4 that holds the deposition target substrate 1 is disposed below the chamber 2.
  • a gas introduction path (not shown) is provided inside the gas shower electrode 7.
  • One side of the gas introduction path is connected to the supply port, and the other side of the gas introduction path is connected to the source gas supply mechanism 3.
  • the chamber 2 is provided with an exhaust port for evacuating the inside of the chamber 2. This exhaust port is connected to an exhaust pump (not shown).
  • the plasma CVD apparatus has a control unit (not shown) for controlling the high-frequency power source 6, the source gas supply mechanism 3, the exhaust pump, and the like, and this control unit performs a CVD film forming process to be described later. It controls the plasma CVD apparatus.
  • any one of a C a F b film, a C a F b N c film, a C a F b O d film, and a C a F b N c O d film is used as the fluorinated organic film 15.
  • a, b, c, and d are natural numbers.
  • the deposition target substrate 1 is inserted into the chamber 2 shown in FIG. 4, and the deposition target substrate 1 is held on the holding electrode 4 in the chamber 2.
  • the inside of the chamber 2 is evacuated by an exhaust pump.
  • a shower-like source gas is introduced into the chamber 2 from the supply port of the gas shower electrode 7 and supplied to the surface of the deposition target substrate 1.
  • the supplied source gas passes between the holding electrode 4 and the earth shield 5 and is exhausted to the outside of the chamber 2 by an exhaust pump.
  • the inside of the chamber 2 is made a source gas atmosphere, and a high frequency (RF) of 13.56 MHz, for example, is applied by the high frequency power source 6.
  • RF high frequency
  • high-frequency power is supplied to the holding electrode 4 and ground is supplied to the gas shower electrode 7.
  • high-frequency power is supplied to the gas shower electrode 7 and ground is supplied to the holding electrode 4. Also good.
  • triheptafluoropropylamine (tertiary amine) of perfluoroamines may be used as the organic material gas in forming a C a F b film as the film 15.
  • the organic raw material gas when forming a C a F b O d film as the film 15 is C 3 F 6 O, C 4 F 6 O 3 , C 4 F 8 O, C 5 F 6 O 3 , C 6 F 4 O 2 , C 6 F 10 O 3 , C 8 F 4 O 3 , C 8 F 8 O, C 8 F 8 O 2 , C 8 F 14 O 3 , C 13 F 10 O, C 13 F 10 O 3 , And C 2 F 6 O (C 3 F 6 O) n (CF 2 O) m.
  • a F b O e film, C a F b O e H d film, C a F b N c O e film and C a F b N c O e H d either film 15 of the film is the film thickness It is 3 nm or less (more preferably 1 nm or less), has a large water contact angle and water repellency, and functions as a solid lubricant.
  • This film 15 is preferably an amorphous film.
  • the Young's modulus of the film 15 is preferably 0.1 to 30 GPa.
  • Substrate Magnetic layer / glass disk (substrate with magnetic layer sputtered on glass disk surface)
  • Substrate temperature 400 ° C
  • Film forming apparatus Plasma CVD apparatus shown in FIG.
  • the B x N y C z O w film of this example contains 42.3% B, 42.7% N, 5.2% C, and 9.8% O. It was.
  • B x N y C z O w film of this embodiment B x N y C z O w film of x of the first embodiment, y, z, it is in the range of w.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Chemical Vapour Deposition (AREA)
  • Magnetic Record Carriers (AREA)

Abstract

Le problème décrit par la présente invention vise à fournir un film de BxNyCzOw ayant une surface ayant un angle de contact d'eau de 50° ou moins. La solution décrite par la présente invention concerne un film de BxNyCzOw formé sur un substrat, où x, y, z et w dans le film de BxNyCzOw satisfont les équations (1)-(5) ci-dessous. (1) 0,4 < x < 0,6; (2) 0,4 < y < 0,6; (3) 0 ≤ z < 0,1; (4) 0 ≤ w < 0,1; (5) x + y + z + w = 1
PCT/JP2017/007858 2016-04-20 2017-02-28 FILM DE BxNyCzOw, PROCÉDÉ DE FORMATION DE FILM, SUPPORT D'ENREGISTREMENT MAGNÉTIQUE, ET SON PROCÉDÉ DE FABRICATION WO2017183314A1 (fr)

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JP2018513045A JP7129083B2 (ja) 2016-04-20 2017-02-28 ＢｘＮｙＣｚＯｗ膜の成膜方法、磁気記録媒体およびその製造方法

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JP2016084510 2016-04-20
JP2016-084510 2016-04-20

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WO2017183314A1 true WO2017183314A1 (fr) 2017-10-26

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0562169A (ja) * 1991-09-06 1993-03-12 Hitachi Metals Ltd 非晶質窒化ほう素膜
JPH10198944A (ja) * 1997-01-09 1998-07-31 Fuji Photo Film Co Ltd 磁気記録ディスク
JP2015004085A (ja) * 2013-06-19 2015-01-08 富士電機株式会社 積層体の製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0562169A (ja) * 1991-09-06 1993-03-12 Hitachi Metals Ltd 非晶質窒化ほう素膜
JPH10198944A (ja) * 1997-01-09 1998-07-31 Fuji Photo Film Co Ltd 磁気記録ディスク
JP2015004085A (ja) * 2013-06-19 2015-01-08 富士電機株式会社 積層体の製造方法

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