WO2013061398A1 - CxNyHz膜、成膜方法、磁気記録媒体およびその製造方法 - Google Patents
CxNyHz膜、成膜方法、磁気記録媒体およびその製造方法 Download PDFInfo
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- WO2013061398A1 WO2013061398A1 PCT/JP2011/074457 JP2011074457W WO2013061398A1 WO 2013061398 A1 WO2013061398 A1 WO 2013061398A1 JP 2011074457 W JP2011074457 W JP 2011074457W WO 2013061398 A1 WO2013061398 A1 WO 2013061398A1
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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
- G11B5/722—Protective coatings, e.g. anti-static or antifriction containing an anticorrosive material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/347—Carbon nitride
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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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
-
- 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
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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
- G11B5/727—Inorganic carbon protective coating, e.g. graphite, diamond like carbon or doped carbon
-
- 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
- G11B5/8408—Processes or apparatus specially adapted for manufacturing record carriers protecting the magnetic layer
Definitions
- the present invention relates to a C x N y H z film, a film forming method, a magnetic recording medium, and a manufacturing method thereof.
- FIG. 18 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.
- An object of one embodiment of the present invention is to provide a high-density C x N y H z film and a film formation method.
- An object of one embodiment of the present invention is to provide a magnetic recording medium in which the thickness of a film between a magnetic layer and a fluorinated organic film is reduced, or a manufacturing method thereof.
- the C x N y H z film preferably has a surface with a water contact angle of 50 ° or less (more preferably 30 ° or less).
- One embodiment of the present invention includes a magnetic layer formed over a nonmagnetic substrate; The above-mentioned C x N y H z film formed on the magnetic layer; A fluorinated organic film formed on the C x N y H z film; A magnetic recording medium comprising:
- a DLC film formed between the C x N y H z film and the magnetic layer may be further provided.
- 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 may be either a film of H d membrane.
- a, b, c, d, and e are natural numbers.
- Each of the C a F b N c O e H d films may be an amorphous film.
- a, b, c, d, and e are natural numbers.
- the thickness of any one of the films is preferably 3 nm or less.
- One embodiment of the present invention is a film forming method for forming a C x N y H z film according to claim 1 or 2 on a deposition target substrate by a CVD method using a gas obtained by vaporizing a starting material.
- the film forming method wherein the starting material is made of C X H Y N Z and is liquid or solid at normal temperature and satisfies the following formulas (1) to (4).
- X, Y, and Z are natural numbers. (1) 4 ⁇ X ⁇ 12 (2) 0 ⁇ Y ⁇ 4 (3) 2 ⁇ Z ⁇ 12 (4) Y / X ⁇ 1
- the starting material is a compound containing the constituent elements of the thin film.
- the starting materials are C 4 H 2 N 2 , C 5 H 3 N 3 , C 7 H 3 N 3 , C 6 H 2 N 4 , C 5 H 2 N 4 , C 10 H 2 N 4 , C 12 H It may be a raw material of any one of 4 N 4 and C 6 N 4 .
- One aspect of the present invention is a method of manufacturing a magnetic recording medium in which a fluorinated organic film is formed on the C x N y H z film formed by the film forming method described above.
- the film formation substrate is a nonmagnetic substrate formed with a magnetic layer
- the C x N y H z film has a surface with a water contact angle of 50 ° or less, and is a method of manufacturing a magnetic recording medium.
- a DLC film may be formed between the C x N y H z 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 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 source gas may include an organic source gas containing carbon and fluorine.
- a, b, c, d, and e are natural numbers.
- the organic material gas may contain 3 or more carbons.
- 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 , C 14 F 8 N 2 , C 15 F 33 N, C 24
- Perfluoroamines may be used as the organic material gas.
- the C x N y H z film is held on a holding electrode, a counter electrode facing the C x N y H z film held on the holding electrode is disposed, It may be a plasma CVD method in which the DC voltage when forming DC plasma by supplying electric power to one of the holding electrode and the counter electrode or DC voltage component when forming high frequency plasma is + 150V to ⁇ 150V. .
- a high-density C x N y H z film and a film formation method can be provided.
- the CVD apparatus for forming a C x N y H z film 13 shown in FIG. 1 is a cross-sectional view schematically showing. It is sectional drawing which shows the CVD apparatus by the modification 1 typically. It is sectional drawing which shows the CVD apparatus by the modification 2 typically. It is sectional drawing which shows the CVD apparatus by the modification 3 typically. It is sectional drawing which shows the CVD apparatus by the modification 4 typically. It is sectional drawing which shows the CVD apparatus by the modification 5 typically. It is sectional drawing which shows the CVD apparatus by the modification 6 typically. It is sectional drawing which shows the CVD apparatus by the modification 7 typically.
- FIG. 11 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.
- (A) is a diagram showing a result of analyzing the C x N y H z film by FT-IR
- (B) is the result of the analysis of the DLC film by FT-IR.
- the plasma CVD apparatus for forming a C x N y H z film and DLC film according to a comparative example, according to Example 2 is a cross-sectional view schematically showing.
- the C x N y H z film of Example 2 is a diagram showing the results of surface analysis by XPS.
- A is a diagram showing an O analysis of the C x N y H z film
- B is a schematic drawing illustrating the analytic results of C x N y H z films N
- C is C x is a diagram showing the results of analysis of N y H z films C
- D is a schematic drawing illustrating the analytic results of C x N y H z films Si. It is a figure which shows the result of having surface-analyzed the DLC film of the comparative example by XPS.
- (A) is a figure which shows the analysis result of O of a DLC film
- (B) is a figure which shows the analysis result of N of a DLC film
- (C) is a figure which shows the analysis result of C of a DLC film
- (D) is a figure which shows the analysis result of Si of a DLC film. It is sectional drawing for demonstrating the manufacturing method of the conventional magnetic recording medium.
- 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.
- FIG. 2 is a cross-sectional view schematically showing a CVD apparatus for forming the C x N y H z film 14 shown in FIG.
- a film formation substrate 2 having at least a magnetic layer 12 formed on a nonmagnetic substrate 11 is prepared, and a film thickness of 1 nm (preferably 0.5 nm) is formed on the film formation substrate 2.
- DLC film 13 is formed by CVD.
- the deposition target substrate 2 is, for example, a bird disk substrate or a media head.
- a C x N y H z film 14 having a thickness of 1 nm (preferably 0.5 nm) is formed on the DLC film 13 by using the CVD apparatus shown in FIG.
- the contact angle of water on the surface of the C x N y H z film 14 is 50 ° or less (more preferably 30 ° or less).
- x, y and z satisfy the following formulas (1) to (4), and preferably satisfy the following formulas (1 ′) to (4 ′).
- the C x N y H z film 14 is dipped into the fluorine-based fomblin oil, so that the fomblin oil is applied onto the C x N y H z film 14.
- a 4 nm-thick fluorinated organic film 15 that functions as a solid lubricant is formed on the C x N y H z film 14.
- the CVD apparatus has a chamber 1, and the chamber 1 is provided with an exhaust port for evacuating the inside of the chamber 1. This exhaust port is connected to an exhaust pump (not shown).
- a holding electrode 4 for holding the deposition target substrate 2 is disposed below the chamber 1.
- the holding electrode 4 is electrically connected to a high frequency power source 6 having a frequency of 13.56 MHz, for example, and the holding electrode 4 also functions as an RF application electrode (RF cathode).
- the high frequency output density of the holding electrode 4 to which a high frequency is applied by the high frequency power source 6 is, for example, 1 ⁇ 10 ⁇ 2 W / cm 2 or less.
- the periphery and the lower part of the holding electrode 4 are shielded by an earth shield 5.
- the high frequency power source 6 is used, but another power source, for example, a DC power source or a microwave power source may be used.
- a gas shower electrode (counter electrode) 7 is arranged in a parallel position facing the holding electrode 4. These are a pair of parallel plate electrodes.
- the gas shower electrode 7 is connected to a ground potential (not shown).
- a plurality of supply ports for supplying a shower-like source gas to the side of the substrate 2 to be processed on which the DLC film 13 is formed (a space between the gas shower electrode 7 and the holding electrode 4). (Not shown) is formed.
- 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 one end of a source gas supply pipe 28.
- the periphery of the supply pipe 28 is covered with the heater 21, and the supply pipe 28 is branched into two hands.
- One end of the supply pipe 28 is connected to a valve 29, and the valve 29 is connected to a mass flow controller 31 through the pipe.
- the mass flow controller 31 is connected to the valve 30 via piping, and the valve 30 is connected to the N 2 supply source via piping.
- the other end of the supply pipe 28 is connected to the valve 19.
- the valve 19 is connected to the mass flow controller 20 via piping, and the mass flow controller 20 is connected to the valve 18 via piping.
- the valve 18 is connected to a raw material container for containing the starting raw material 16 through a pipe.
- the raw material container, the valves 18 and 19 and the mass flow controller 20 are arranged in the thermostatic chamber 17.
- the starting material 16 is made of C X H Y N Z and is liquid or solid at room temperature, satisfying the following formulas (1) to (4), preferably satisfying the following formulas (1 ′) to (4 ′) It is.
- X, Y, and Z are natural numbers.
- the reason for the above formula (1) is that if X is less than 4, the starting material becomes a gas at room temperature, and if X is larger than 12, it is difficult to evaporate the starting material. .
- the starting material 16 include C 4 H 2 N 2 (fumaronitrile), C 5 H 3 N 3 (cyanopyrazine, cyanopyrimidine) and C 7 H 3 N 3 (pyridinedicarbonitrile).
- the deposition target substrate 2 is inserted into the chamber 1, and the deposition target substrate 2 is held on the holding electrode 4 in the chamber 1. Next, the inside of the chamber 1 is evacuated by an exhaust pump.
- the starting raw material 16 is vaporized by heating in the thermostatic chamber 17, the naturalized raw material gas is controlled in flow rate by the mass flow controller 20, and the flow-controlled raw material gas is maintained by the heater 21 so as not to decrease in temperature.
- a shower-like source gas is introduced into the chamber 1 from the supply port of the gas shower electrode 7 and supplied to the surface of the deposition target substrate 2.
- the supplied source gas passes between the holding electrode 4 and the earth shield 5 and is exhausted to the outside of the chamber 1 by an exhaust pump.
- the inside of the chamber 1 is made a source gas atmosphere by controlling the supply pressure of the source gas and the exhaust gas to a predetermined pressure and a source gas flow rate, and a high frequency (RF) of 13.56 MHz, for example, is applied by the high frequency power source 6.
- RF high frequency
- a C x N y H z film 14 is formed on the DLC film 13 of the deposition target substrate 2 by generating plasma.
- N 2 gas into the raw material gas may be added to the above raw material gas flow rate was controlled by a mass flow controller 31 and N 2 gas from the N 2 supply source. Thereby, the N content in the C x N y H z film 14 can be increased.
- the C x N y H z film 14 can be provided with a barrier property for preventing impurities such as Cr from dissolving out of the magnetic layer 12 and reaching the fluorinated organic film 15 (so-called corrosion). . Corrosion can be prevented even if the DLC film 13 is made thin by providing the C x N y H z film 14 with the barrier property that was conventionally given only to the DLC film 13. 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 contact angle of water on the surface of the C x N y H z film 14 can be 50 ° or less, sufficient adhesion between the fluorinated organic film 15 and the C x N y H z film 14 is ensured. It is possible to suppress the peeling of the fluorinated organic film 15 from the C x N y H z film 14.
- a DLC film 13 is formed on the magnetic layer 12
- a C x N y H z film 14 is formed on the DLC film 13
- a fluorination is formed on the C x N y H z film 14.
- the organic film 15 is formed, the C x N y H z film 14 may be formed on the magnetic layer 12 and the fluorinated organic film 15 may be formed on the C x N y H z film 14.
- a deposition target substrate 10 having at least the magnetic layer 12 formed on the nonmagnetic substrate 11 is prepared, and C x N is formed on the DLC film 13 formed on the deposition target substrate 10.
- forms a y H z film 14 is not limited thereto and may be formed C x N y H z 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 C x N y H z film 14 is formed using the CVD apparatus shown in FIG. 2, but the CVD apparatus shown in FIGS. 3 to 9 may be used. 3 to 9, the same parts as those in FIG. 2 are denoted by the same reference numerals, and the description of the same parts is omitted.
- the CVD apparatus shown in FIG. 3 has a valve 19 that is connected to a needle valve 22 through a pipe.
- the needle valve 22 is connected to the valve 18 through a pipe, and the valve 18 is connected to a raw material container that contains the starting raw material 16 through the pipe.
- the raw material container, the valves 18 and 19 and the needle valve 22 are disposed in the thermostatic chamber 17.
- the starting material 16 include C 6 H 2 N 4 (dicyanopyrazine), C 5 H 2 N 4 (dicyanoimidazole), C 10 H 2 N 4 (tetracyanobenzene) and C 12 H 4 N 4 (tetra). Cyanoquinodimethane) and the like. Specific examples of the starting material 16 are C 4 H 2 N 2 (fumaronitrile), C 5 H 3 N 3 (cyanopyrazine, cyanopyrimidine), C 7 H 3 N 3 (pyridinedicarbonitrile) and C 6 N 4. (Tetracyanoethylene) and the like.
- the deposition target substrate 2 is inserted into the chamber 1, and the deposition target substrate 2 is held on the holding electrode 4 in the chamber 1. Next, the inside of the chamber 1 is evacuated by an exhaust pump.
- the starting raw material 16 is vaporized by heating in the thermostatic chamber 17, the naturalized raw material gas is flow-controlled by the needle valve 22, and the flow-controlled raw material gas is maintained by the heater 21 so as not to decrease in temperature.
- a shower-like source gas is introduced into the chamber 1 from the supply port of the gas shower electrode 7 and supplied to the surface of the deposition target substrate 2.
- the supplied source gas passes between the holding electrode 4 and the earth shield 5 and is exhausted to the outside of the chamber 1 by an exhaust pump.
- the inside of the chamber 1 is made a source gas atmosphere by controlling the supply pressure of the source gas and the exhaust gas to a predetermined pressure and a source gas flow rate, and a high frequency (RF) of 13.56 MHz, for example, is applied by the high frequency power source 6.
- RF high frequency
- a C x N y H z film 14 is formed on the DLC film 13 of the deposition target substrate 2 by generating plasma.
- no added N 2 gas into the raw material gas may be added to the above raw material gas flow rate was controlled by a mass flow controller 31 and N 2 gas from the N 2 supply source. Thereby, the N content in the C x N y H z film 14 can be increased.
- the CVD apparatus shown in FIG. 4 has a valve 19, and the valve 19 is connected to the vaporizer 27 through a pipe.
- the vaporizer 27 and the valve 19 are heated by the heater 21.
- the vaporizer 27 is connected to the liquid MFM 25 via a pipe, and the liquid MFM 25 is connected to the valve 18 via a pipe.
- the valve 18 is connected to a raw material container for containing the starting raw material 16 through a pipe.
- the raw material container, the valve 18 and the liquid MFM 25 are disposed in the thermostatic chamber 17.
- the vaporizer 27 is connected to the valve 24 via piping, and the valve 24 is connected to the mass flow controller 20 via piping.
- the mass flow controller 20 is connected to a valve 23a via a pipe, and the valve 23a is connected to a carrier gas supply source (Ar, He, N 2, etc.) via the pipe.
- the carrier gas supply source is connected to the valve 23b via a pipe, and the valve 23b is connected to the inside of the raw material container via the pipe.
- the deposition target substrate 2 is inserted into the chamber 1, and the deposition target substrate 2 is held on the holding electrode 4 in the chamber 1. Next, the inside of the chamber 1 is evacuated by an exhaust pump.
- the liquid starting material 16 is pumped at a carrier gas such as N 2 in the liquid MFM25, a liquid starting material whose flow rate is controlled by the liquid MFM While being introduced into the vaporizer 27, the carrier gas from the carrier gas supply source is flow-controlled by the mass flow controller 20 and introduced into the vaporizer 27.
- the vaporizer 27 vaporizes the starting material, and the naturalized starting material and A source gas containing carrier gas is introduced into the chamber 1 from the supply port of the gas shower electrode 7 through the supply pipe 28 and the gas introduction path while maintaining the source gas containing the carrier gas so as not to lower the temperature by the heater 21.
- the film is supplied to the surface of the film formation substrate 2.
- the supplied source gas passes between the holding electrode 4 and the earth shield 5 and is exhausted to the outside of the chamber 1 by an exhaust pump. Then, the inside of the chamber 1 is made a source gas atmosphere by controlling the supply pressure of the source gas and the exhaust gas to a predetermined pressure and a source gas flow rate, and a high frequency (RF) of 13.56 MHz, for example, is applied by the high frequency power source 6. Then, a C x N y H z film 14 is formed on the DLC film 13 of the deposition target substrate 2 by generating plasma.
- RF radio frequency
- the carrier gas from the carrier gas supply source is controlled by the mass flow controller 20 to be supplied to the raw material container, and the starting raw material 16 is vaporized by heating it in the thermostatic chamber 17 while bubbling the starting raw material 16, and the naturalized raw material.
- the flow rate of the gas and the carrier gas is controlled by the mass flow controller 20, and the supply port of the gas shower electrode 7 is supplied through the supply pipe 28 and the gas introduction path while maintaining the flow rate-controlled source gas and carrier gas so as not to lower the temperature by the heater 21. Then, a shower-like source gas and a carrier gas are introduced into the chamber 1 and supplied to the surface of the deposition target substrate 2.
- the starting raw material 16 is vaporized by heating with the heater 21, and the flow rate of the naturalized raw material gas is controlled by the mass flow controller 20, and the raw material gas whose flow rate is controlled is maintained by the heater 21 so that the temperature does not decrease.
- a shower-like source gas is introduced into the chamber 1 from the supply port of the gas shower electrode 7 and supplied to the surface of the film formation substrate 2.
- the starting raw material 16 is vaporized by heating with the heater 21, the flow rate of the naturalized raw material gas is controlled by the needle valve 22, and the raw material gas whose flow rate is controlled is maintained by the heater 21 so that the temperature does not decrease.
- a shower-like source gas is introduced into the chamber 1 from the supply port of the gas shower electrode 7 and supplied to the surface of the film formation substrate 2.
- the starting material 16 is heated to a predetermined temperature by the heater 21a, the liquid starting material is pumped at a carrier gas such as N 2 in the liquid MFM25, flow controlled a liquid starting material vaporizer by the liquid MFM 27
- the carrier gas from the carrier gas supply source is flow-controlled by the mass flow controller 20 and introduced into the vaporizer 27.
- the vaporizer 27 vaporizes the starting material, and the naturalized starting material and carrier gas are supplied to the vaporizer 27.
- a source gas in the form of a shower is introduced into the chamber 1 from the supply port of the gas shower electrode 7 through the supply pipe 28 and the gas introduction path while maintaining the source gas containing the heater 21 so that the temperature does not decrease. 2 to the surface.
- the carrier gas from the carrier gas supply source is flow-controlled by the mass flow controller 20 and supplied to the raw material container so that the starting raw material 16 is heated by the heater 21 while the starting raw material 16 is bubbled, and the naturalized raw material gas is obtained.
- the flow rate of the carrier gas is controlled by the mass flow controller 20, and the supply gas 28 and the gas introduction path are passed through the supply port of the gas shower electrode 7 while maintaining the flow rate-controlled source gas and carrier gas so as not to lower the temperature by the heater 21.
- shower-like source gas and carrier gas are introduced into the chamber 1 and supplied to the surface of the deposition target substrate 2.
- FIG. 10 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 1, and a holding electrode 4 that holds a substrate 2 to be processed is disposed below the chamber 1.
- the holding electrode 4 is electrically connected to a high frequency power source 6 having a frequency of 13.56 MHz, for example, and the holding electrode 4 also functions as an RF application electrode.
- the periphery and the lower part of the holding electrode 4 are shielded by an earth shield 5.
- the high frequency power source 6 is used, but another power source, for example, a DC power source or a microwave power source may be used.
- a gas shower electrode (counter electrode) 7 is arranged in a parallel position facing the holding electrode 4. These are a pair of parallel plate electrodes.
- the gas shower electrode is connected to the ground potential.
- a power source is connected to the holding electrode 4 and a ground potential is connected to the gas shower electrode.
- a ground potential may be connected to the holding electrode 4 and a power source may be connected to the gas shower electrode.
- a shower-like source gas is supplied to the side of the substrate 2 to be processed on which the C x N y H z film 14 is formed (the space between the gas shower electrode 7 and the holding electrode 4).
- a plurality of supply ports are formed.
- the source gas one having an organic source gas containing carbon and fluorine can be used. This organic source gas preferably contains three or more carbons.
- 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 1 is provided with an exhaust port for evacuating the inside of the chamber 1. 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 2 is inserted into the chamber 1 shown in FIG. 10, and the deposition target substrate 2 is held on the holding electrode 4 in the chamber 1.
- the inside of the chamber 1 is evacuated by an exhaust pump.
- a shower-like source gas is introduced into the chamber 1 from the supply port of the gas shower electrode 7 and supplied to the surface of the deposition target substrate 2.
- the supplied source gas passes between the holding electrode 4 and the earth shield 5 and is exhausted to the outside of the chamber 1 by an exhaust pump.
- the inside of the chamber 1 is made a source gas atmosphere by controlling the supply pressure of the source gas and the exhaust gas to a predetermined pressure and a source gas flow rate, and a high frequency (RF) of 13.56 MHz, for example, is applied by the high frequency power source 6.
- RF radio frequency
- the film forming conditions are such that the pressure is 0.01 Pa to atmospheric pressure, the processing temperature is room temperature, and the DC voltage component when forming the high frequency plasma is +150 V to ⁇ 150 V (more preferably +50 V to ⁇ 50 V). It is preferable to carry out with. By suppressing the DC voltage component in this way, plasma damage to the film below the fluorinated organic film 15 can be suppressed.
- the organic raw material gas for forming a C a F b film as the film 15 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 It has at least one of 13 F 28 , C 15 F 32 , C 20 F 42 , and C 24 F 50 .
- the organic material gas used when forming a C a F b N c film as the film 15 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, C It has at least one of 14 F 8 N 2 , C 15 F 33 N, C 24 F 45 N 3 , and triheptafluoropropylamine.
- 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.
- the organic source gas in the case where a C a F b N c O d film is formed as the film 15 has C 7 F 5 NO.
- the high frequency power supply 6 is used, but a DC power supply or a microwave power supply may be used.
- the DC voltage at the time of forming DC plasma by using a DC power source is preferably +150 V to ⁇ 150 V (more preferably +50 V to ⁇ 50 V).
- 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 membrane, its thickness is 3nm or less (More preferably 1 nm or less), the water contact angle is large 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.
- FIG. 11 is a cross-sectional view schematically showing a plasma CVD apparatus for forming a fluorinated organic film according to one embodiment of the present invention. The same parts as those in FIG. Only explained.
- the holding electrode 4 is electrically connected to the high frequency power source 6a and the ground potential via the changeover switch 8a, and the high frequency power or the ground potential is applied to the holding electrode 4 by the changeover switch 8a.
- the gas shower electrode 7 is electrically connected to the high frequency power source 6b and the ground potential via the changeover switch 8b, and the high frequency power or the ground potential is applied to the gas shower electrode 7 by the changeover switch 8b. ing.
- the high frequency power supplies 6a and 6b are used. However, other power supplies such as a DC power supply or a microwave power supply may be used.
- the plasma CVD apparatus also includes a control unit (not shown) for controlling the changeover switches 8a and 8b, the high frequency power supplies 6a and 6b, the plasma forming gas supply mechanism 3, the exhaust pump, and the like. Controls the plasma CVD apparatus to perform the CVD film forming process.
- the high frequency power supplies 6a and 6b and the ground potential are connected to the holding electrode 4 and the gas shower electrode 7 according to the first connection state, and the C a F is formed on the C x N y H z film 14 of the deposition target substrate 2.
- a specific method for forming the film 15 in this state is the same as that in the first embodiment, and a description thereof will be omitted.
- the high frequency power supplies 6a and 6b and the ground potential are connected to the holding electrode 4 and the gas shower electrode 7 according to the second connection state, and the C a F is formed on the C x N y H z film 14 of the deposition target substrate 2.
- a specific method for forming the film 15 in this state is as follows.
- the chamber 1 is evacuated by an exhaust pump.
- a shower-like source gas is introduced into the chamber 1 from the supply port of the gas shower electrode 7 and supplied to the surface of the C x N y H z film 14 of the deposition target substrate 2.
- the supplied source gas passes between the holding electrode 4 and the earth shield 5 and is exhausted to the outside of the chamber 1 by an exhaust pump.
- the inside of the chamber 1 is made a source gas atmosphere, and a radio frequency (RF) of, for example, 13.56 MHz is gas showered by the high frequency power source 6b.
- RF radio frequency
- a C a F b film, a C a F b N c film, a C a F b H d film, and a C a F b are formed on the DLC film 13 of the deposition target substrate 2 by being applied to the electrode 7 and generating plasma.
- the film forming conditions are such that the pressure is 0.01 Pa to atmospheric pressure, the processing temperature is room temperature, and the DC voltage component when forming the high frequency plasma is +150 V to ⁇ 150 V (more preferably +50 V to ⁇ 50 V). It is preferable to carry out with.
- the power supply from the plasma power supply is stopped, the supply of the source gas from the supply port of the gas shower electrode 7 is stopped, and the film forming process is completed.
- Example 1 The C x N y H z film was formed on a substrate, showing the C x N y H z film in FIG. 12 (A) The results were analyzed by FT-IR.
- Substrate Si Film forming apparatus: CVD apparatus shown in FIG. 6
- Starting material Cyanopyrazine
- Gas flow rate FULL OPEN (using a mass flow for toluene of 10 sccm)
- Gas pressure 5Pa
- High frequency power supply frequency 380 kHz
- High frequency output 900W
- Deposition time 10 min
- a DLC film is formed on a substrate, and the result of analyzing this DLC film by FT-IR is shown in FIG.
- Example result 12A and 12B show the results of analysis by FT-IR, in which the horizontal axis represents the wave number (cm ⁇ 1 ) and the vertical axis represents the absorbance (au).
- FIG. 12 (A) CN bonds and NH bonds were detected in the C x N y H z film, and as shown in FIG. 12 (B), CH bonds were detected in the DLC film.
- Example 2 A C x N y H z film (CVD-CN) was formed on the substrate, and the ashing rate, water contact angle, and XPS (at%) of the C x N y H z film were measured. Shown in As shown in the XPS measurement results in Table 1, the C x N y H z film of this example is in the range of x, y, z of the C x N y H z film 14 in the first embodiment.
- a DLC film was formed on a substrate, and the results of measuring the ashing rate, water contact angle, XPS (at%), and hydrogen content of the DLC film are shown in Table 2.
- FIG. 13 is a cross-sectional view schematically showing a plasma CVD apparatus for forming a C x N y H z film according to Example 2 and a DLC film according to a comparative example.
- This plasma CVD apparatus has a symmetrical structure with respect to a film formation substrate (for example, a disk substrate), and is an apparatus capable of simultaneously forming films on both surfaces of the film formation substrate 201.
- a film formation substrate for example, a disk substrate
- FIG. The left side is shown with respect to the film-forming substrate 201, and the right side is omitted.
- the plasma CVD apparatus has a chamber 202, and a filamentary cathode electrode (hot cathode) 203 made of, for example, tantalum is formed in the chamber 202. Both ends of the hot cathode 203 are electrically connected to an AC power source 205 located outside the chamber 202, and the AC power source 205 is disposed in an insulated state with respect to the chamber 202.
- the AC power source 205 for example, a power source of 0 to 50 V, 10 to 50 A (ampere) can be used.
- One end of the AC power source 205 is electrically connected to the ground 206.
- An anode electrode (horn anode) 204 having a funnel shape is disposed in the chamber 202 so as to surround the hot cathode 203, and the horn anode 204 is shaped like a speaker.
- the horn anode 204 is electrically connected to a DC power source (DC power source) 207, and the DC power source 207 is disposed in an insulated state with respect to the chamber 202.
- the positive potential side of the DC power source 207 is electrically connected to the horn anode 204, and the negative potential side of the DC power source 207 is electrically connected to the ground 206.
- the DC power source 207 for example, a power source of 0 to 500V, 0 to 7.5A (ampere) can be used.
- a film formation substrate 201 is disposed in the chamber 202, and the film formation substrate 201 is disposed so as to face the hot cathode 203 and the horn anode 204. Specifically, the hot cathode 203 is surrounded near the central portion of the inner peripheral surface of the horn anode 204, and the horn anode 204 is disposed with the maximum inner diameter side facing the deposition target substrate 201.
- the distance l between the hot cathode 203 and the deposition target substrate 201 is preferably as long as possible, specifically 200 mm or more and 300 mm or less. This is because if the distance l is less than 200 mm, the hardness of the thin film formed on the deposition target substrate 201 becomes low, and if the distance l is more than 300 mm, the film formation rate becomes slow, which is not practical.
- the deposition target substrate 201 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.
- the deposition target substrate 201 is electrically connected to a DC power source (DC power source) 212 as an ion acceleration power source, and the DC power source 212 is disposed in an insulated state from the chamber 202.
- the negative potential side of the DC power source 212 is electrically connected to the deposition target substrate 201, and the positive potential side of the DC power source 212 is electrically connected to the ground 206.
- the DC power supply 212 for example, a power supply of 0 to 1500 V and 0 to 100 mA (milliampere) can be used.
- a plasma wall 208 is disposed so as to cover the space between each of the hot cathode 203 and the horn anode 204 and the deposition target substrate 201.
- the plasma wall 208 is electrically connected to a float potential (not shown) and is disposed in an insulated state with respect to the chamber 202.
- the plasma wall 208 has a cylindrical shape or a polygonal shape, and an inner diameter B of the cylinder or the polygon is 100 mm or more and 200 mm or less.
- the inner diameter B is less than 100 mm, the ionization of the raw material gas becomes too high in the vicinity of the horn anode 204, and free carbon (ie, soot) is likely to be generated, which is not preferable. If the inner diameter B exceeds 200 mm, ionization of the source gas becomes too low in the vicinity of the horn anode 204, making it difficult to form a dense film on the deposition target substrate 201, and using a neodymium magnet described later. This is because it is difficult to create a high magnetic field.
- a film thickness correction plate 208a is provided at the end of the plasma wall 208 on the film formation substrate 201 side, and the film thickness correction plate 208a is electrically connected to the float potential.
- the thickness of the film formed on the outer peripheral portion of the deposition target substrate 201 can be controlled by the film thickness correction plate 208a.
- a neodymium magnet 209 is disposed outside the chamber 202.
- the neodymium magnet 209 has, for example, a cylindrical shape or a polygonal shape, and the distance A between the inner diameter 211 passing through the center of the cylindrical side surface or the polygonal side surface in the cylinder direction and the hot cathode 203 is within 50 mm (more preferably within 35 mm). It is preferable that The center of the inner diameter 211 is a magnet center 210, and the magnet center 210 is positioned so as to face the approximate center of the hot cathode 203 and the approximate center of the film formation substrate 201.
- the neodymium magnet 209 preferably has a magnetic force of the magnet center 210 of 50 G or more and 200 G (Gauss) or less, more preferably 50 G or more and 150 G or less.
- the plasma CVD apparatus has an evacuation mechanism (not shown) for evacuating the chamber 202.
- the plasma CVD apparatus has a gas supply mechanism (not shown) for supplying a film forming source gas into the chamber 202.
- FIG. 14 is a diagram showing the results of surface analysis of the C x N y H z film of Example 2 by XPS.
- the vertical axis represents strength (c / s) and the horizontal axis represents binding energy (eV).
- FIGS. 15A to 15D are diagrams showing the results of analysis in the depth direction by XPS while sputtering the C x N y H z film of Example 2.
- FIG. Figure 15 (A) is a result of analysis of C x N y H z films O
- FIG. 15 (B) is a result of analysis of C x N y H z films in N
- Figure 15 (C) is C x a N y H z C analysis of the film
- FIG. 15 (D) is the analysis result of the C x N y H z films Si.
- the vertical axis indicates the atomic content and the horizontal axis indicates the sputtering time.
- FIG. 16 is a diagram showing the results of surface analysis of the DLC film of the comparative example by XPS.
- the vertical axis represents strength (c / s) and the horizontal axis represents binding energy (eV).
- FIGS. 17A to 17D are diagrams showing the results of analysis in the depth direction by XPS while sputtering the DLC film of the comparative example.
- 17A shows the analysis result of O in the DLC film
- FIG. 17B shows the analysis result of N in the DLC film
- FIG. 17C shows the analysis result of C in the DLC film.
- (D) is the analysis result of Si in the DLC film.
- the vertical axis represents the atomic content
- the horizontal axis represents the sputtering time.
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Abstract
Description
まず、非磁性基板101の上に少なくとも磁性層102を形成した被成膜基板100を用意し、この被成膜基板100の上に膜厚3nmのDLC(Diamond Like Carbon)膜103をプラズマCVD(chemical vapor deposition)法により成膜する。次いで、このDLC膜103の上に厚さ1nmのCN膜104をスパッタリングにより成膜する。
DLC膜をスパッタリングにより成膜し、その膜厚を8nm以下にすると、磁性層102からCoなどの不純物が溶け出してフッ化有機膜105に到達する(いわゆるコロージョン)という問題が発生する。そこで、DLC膜をプラズマCVD法により成膜することで、スパッタリングに比べて高密度なDLC膜を成膜できるため、その膜厚を3nmとしてもコロージョンを防ぐためのバリア性を十分に確保することができる。
DLC膜103は水の接触角が80°程度であるため、DLC膜103上にフッ化有機膜105を塗布するとDLC膜103とフッ化有機膜105との密着性が悪い。このため、DLC膜103上にフッ化有機膜105を塗布することができない。そこで、DLC膜103とフッ化有機膜105との間に、水の接触角が30°程度であるCN膜104を形成することで、DLC膜103とフッ化有機膜105との密着性を高めることができる。ただし、CN膜104はコロージョンを防ぐためのバリア性の機能を有していない。
本発明の一態様は、磁性層とフッ化有機膜との間の膜の厚さを薄くした磁気記録媒体またはその製造方法を提供することを課題とする。
x,y,zは下記式(1)~(4)を満たすことを特徴とするCxNyHz膜。
(1)0.4<x<0.7
(2)0.01<y<0.5
(3)0≦z<0.3
(4)x+y+z=1
前記CxNyHz膜は水の接触角が50°以下(より好ましくは30°以下)である表面を有することが好ましい。
前記磁性層上に形成された上述したCxNyHz膜と、
前記CxNyHz膜上に形成されたフッ化有機膜と、
を具備することを特徴とする磁気記録媒体である。
前記CxNyHz膜と前記磁性層との間に形成されたDLC膜をさらに具備するとよい。
前記フッ化有機膜は、CaFb膜、CaFbNc膜、CaFbHd膜、CaFbOe膜、CaFbOeHd膜、CaFbNcOe膜及びCaFbNcOeHd膜のいずれかの膜であるとよい。ただし、a,b,c,d,eは、自然数である。
前記CaFb膜、CaFbNc膜、CaFbHd膜、CaFbOe膜、CaFbOeHd膜、CaFbNcOe膜及びCaFbNcOeHd膜それぞれはアモルファス膜であるとよい。
ただし、a,b,c,d,eは、自然数である。
前記いずれかの膜の厚さは3nm以下であるとよい。
前記出発原料は、CXHYNZからなり、常温で液体または固体であり、下記式(1)~(4)を満たすことを特徴とする成膜方法。
ただし、X,Y,Zは自然数である。
(1)4≦X≦12
(2)0≦Y≦4
(3)2≦Z≦12
(4)Y/X<1
前記出発原料は、C4H2N2、C5H3N3、C7H3N3、C6H2N4、C5H2N4、C10H2N4、C12H4N4およびC6N4のいずれか一の原料であるとよい。
前記被成膜基板は、非磁性基板上に磁性層を形成したものであり、
前記CxNyHz膜は水の接触角が50°以下である表面を有することを特徴とする磁気記録媒体の製造方法である。
前記CxNyHz膜と前記磁性層との間にDLC膜を形成するとよい。
前記フッ化有機膜は、原料ガスを用いたCVD法により形成されたCaFb膜、CaFbNc膜、CaFbHd膜、CaFbOe膜、CaFbOeHd膜、CaFbNcOe膜及びCaFbNcOeHd膜のいずれかの膜であり、
前記原料ガスは、炭素とフッ素を含む有機物原料ガスを有するとよい。
ただし、a,b,c,d,eは、自然数である。
前記有機物原料ガスが3個以上の炭素を含むとよい。
前記膜上に前記CaFb膜を形成する場合の前記有機物原料ガスは、C3F6、C4F6、C6F6、C6F12、C6F14、C7F8、C7F14、C7F16、C8F16、C8F18、C9F18、C9F20、C10F8、C10F18、C11F20、C12F10、C13F28、C15F32、C20F42、及びC24F50の少なくとも一つを有し、
前記膜上に前記CaFbNc膜を形成する場合の前記有機物原料ガスは、C3F3N3、C3F9N、C5F5N、C6F4N2、C6F9N3、C6F12N2、C6F15N、C7F5N、C8F4N2、C9F21N、C12F4N4、C12F27N、C14F8N2、C15F33N、C24F45N3、及びトリヘプタフルオロプロピルアミンの少なくとも一つを有し、
前記膜上に前記CaFbOd膜を形成する場合の前記有機物原料ガスは、C3F6O、C4F6O3、C4F8O、C5F6O3、C6F4O2、C6F10O3、C8F4O3、C8F8O、C8F8O2、C8F14O3、C13F10O、C13F10O3、及びC2F6O(C3F6O)n(CF2O)mの少なくとも一つを有し、
前記膜上に前記CaFbNcOd膜を形成する場合の前記有機物原料ガスは、C7F5NOを有するとよい。
前記有機物原料ガスとしてパーフルオロアミン類を用いるとよい。
前記原料ガスを用いたCVD法は、前記CxNyHz膜を保持電極に保持し、前記保持電極に保持された前記CxNyHz膜に対向する対向電極を配置し、前記保持電極および前記対向電極の一方の電極に電力を供給して直流プラズマを形成する際の直流電圧または高周波プラズマを形成する際の直流電圧成分を+150V~-150VとしたプラズマCVD法であるとよい。
また、本発明の一態様によれば、磁性層とフッ化有機膜との間の膜の厚さを薄くした磁気記録媒体またはその製造方法を提供することができる。
図1は、本発明の一態様に係る磁気記録媒体の製造方法を説明するための断面図である。図2は、図1に示すCxNyHz膜14を成膜するためのCVD装置を模式的に示す断面図である。
(1)0.4<x<0.7
(2)0.01<y<0.5
(3)0≦z<0.3
(4)x+y+z=1
(1')0.5<x<0.7
(2')0.05<y<0.4
(3')0≦z<0.3
(4')x+y+z=1
CVD装置は、チャンバー1を有しており、チャンバー1には、チャンバー1の内部を真空排気する排気口が設けられている。この排気口は排気ポンプ(図示せず)に接続されている。
(1)4≦X≦12
(2)0≦Y≦4
(3)2≦Z≦12
(4)Y/X<1(より好ましくは3/7≦Y/X<1)
(1')4≦X≦7
(2')0≦Y≦4
(3')2≦Z≦4
(4')Y/X<1(より好ましくは3/7≦Y/X<1)
被成膜基板2をチャンバー1内に挿入し、このチャンバー1内の保持電極4上に被成膜基板2を保持する。次いで、排気ポンプによってチャンバー1内を真空排気する。
図3に示すCVD装置はバルブ19を有し、バルブ19は配管を介してニードルバルブ22に接続されている。ニードルバルブ22は配管を介してバルブ18に接続されており、バルブ18は配管を介して出発原料16を収容する原料容器に接続されている。原料容器、バルブ18,19およびニードルバルブ22は恒温槽17内に配置されている。
出発原料16の具体例は、C4H2N2(フマルニトリル)、C5H3N3(シアノピラジン、シアノピリミジン)、C7H3N3(ピリジンジカルボニトリル)およびC6N4(テトラシアノエチレン)などが挙げられる。
被成膜基板2をチャンバー1内に挿入し、このチャンバー1内の保持電極4上に被成膜基板2を保持する。次いで、排気ポンプによってチャンバー1内を真空排気する。
図4に示すCVD装置はバルブ19を有し、バルブ19は配管を介して気化器27に接続されている。気化器27及びバルブ19はヒータ21によって加熱されるようになっている。気化器27は配管を介して液体MFM25に接続されており、液体MFM25は配管を介してバルブ18に接続されている。バルブ18は配管を介して出発原料16を収容する原料容器に接続されている。原料容器、バルブ18および液体MFM25は恒温槽17内に配置されている。気化器27は配管を介してバルブ24に接続されており、バルブ24は配管を介してマスフローコントローラ20に接続されている。マスフローコントローラ20は配管を介してバルブ23aに接続されており、バルブ23aは配管を介してキャリアガス供給源(Ar、He、N2等)に接続されている。キャリアガス供給源は配管を介してバルブ23bに接続されており、バルブ23bは配管を介して原料容器内に接続されている。
被成膜基板2をチャンバー1内に挿入し、このチャンバー1内の保持電極4上に被成膜基板2を保持する。次いで、排気ポンプによってチャンバー1内を真空排気する。
図5に示すCVD装置は、図4に示す液体MFM25及び気化器27をマスフローコントローラ20に変更したものである。
図6に示すCVD装置は、出発原料16を収容する原料容器、バルブ18,19、マスフローコントローラ20、配管および供給配管28の周囲はヒータ21によって覆われている。
図7に示すCVD装置は、図6に示すマスフローコントローラ20をニードルバルブ22に変更したものである。
図8に示すCVD装置は、図4に示す恒温槽17をヒータ21aに変更したものである。
図9に示すCVD装置は、図5に示す恒温槽17をヒータ21に変更したものである。
本実施形態に係る磁気記録媒体の製造方法では、図1に示すDLC膜13上にCxNyHz膜14を形成するまでの工程は第1の実施形態と同様であるので説明を省略し、図10に示すプラズマCVD装置を用いてCxNyHz膜14の上にフッ化有機膜15を形成する工程から説明する。なお、本実施形態は、フッ化有機膜15を形成する工程以外については第1の実施形態と同様である。
プラズマCVD装置はチャンバー1を有しており、チャンバー1内の下方には被処理基板2を保持する保持電極4が配置されている。
被成膜基板2を図10に示すチャンバー1内に挿入し、このチャンバー1内の保持電極4上に被成膜基板2を保持する。
膜15としてCaFb膜を成膜する場合の有機物原料ガスは、C3F6、C4F6、C6F6、C6F12、C6F14、C7F8、C7F14、C7F16、C8F16、C8F18、C9F18、C9F20、C10F8、C10F18、C11F20、C12F10、C13F28、C15F32、C20F42、及びC24F50の少なくとも一つを有するものである。
図11は、本発明の一態様に係るフッ化有機膜を成膜するためのプラズマCVD装置を模式的に示す断面図であり、図10と同一部分には同一符号を付し、異なる部分についてのみ説明する。
第1の接続状態は、切り替えスイッチ8aによって高周波電源6aと保持電極4を接続し、切り替えスイッチ8bによって接地電位とガスシャワー電極7を接続した状態である。この状態によって膜15を成膜する具体的な方法は、第1の実施形態と同様であるので説明を省略する。
第2の接続状態は、切り替えスイッチ8aによって接地電位と保持電極4を接続し、切り替えスイッチ8bによって高周波電源6bとガスシャワー電極7を接続した状態である。この状態によって膜15を成膜する具体的な方法は以下のとおりである。
基板上にCxNyHz膜を成膜し、このCxNyHz膜をFT-IRによって分析した結果を図12(A)に示す。
基板 : Si
成膜装置 : 図6に示すCVD装置
出発原料 : シアノピラジン
ガス流量 : FULL OPEN(10sccmのトルエン用マスフローを使用)
ガス圧力 : 5Pa
高周波電源の周波数 : 380kHz
高周波出力 : 900W
成膜時間 : 10min
基板 : Si
成膜装置 : 図6に示すCVD装置
出発原料 : トルエン
ガス流量 : 30sccm
ガス圧力 : 0.5Pa
高周波電源の周波数 : 13.56MHz
高周波出力 : 100W
成膜時間 : 20min
図12(A),(B)は、FT-IRによって分析した結果であり、横軸に波数(cm-1)、縦軸に吸光度(a.u.)を示す図である。
図12(A)に示すように、CxNyHz膜ではCN結合およびNH結合が検出され、図12(B)に示すように、DLC膜ではCH結合が検出された。
基板上にCxNyHz膜(CVD-CN)を成膜し、このCxNyHz膜のアッシングレート、水の接触角、XPS(at%)それぞれを測定した結果を表1に示す。表1のXPS測定結果に示すように、本実施例のCxNyHz膜は第1の実施形態におけるCxNyHz膜14のx、y、zの範囲に入っている。
基板 : Si
成膜装置 : 図13に示すCVD装置
出発原料 : シアノピラジン
ガス流量 : 3.3sccm(トルエン用マスフローを使用)
圧力 : 0.3Pa
ホットカソード203 : タンタルフィラメント
交流電源205の出力 : 220W
DC電源207の電流 : 1650mA
DC電源212の電圧 : 250V
外部磁場 : 50G
成膜時間 : XPS:42sec(25nm)、水の接触角:0.8sec(0.5nm)
基板 : Si
成膜装置 : 図13に示すCVD装置
出発原料 : 高純度トルエン
ガス流量 : 3.3sccm
圧力 : 0.3Pa
ホットカソード203 : タンタルフィラメント
交流電源205の出力 : 220W
DC電源207の電流 : 1650mA
DC電源212の電圧 : 250V
外部磁場 : 50G
成膜時間 : XPS:21sec(30nm)、水の接触角:0.7sec(10nm)、RBS/ERDA:42sec(60nm)
ガス : O2
ガス流量 : 50sccm
圧力 : 30Pa
電極 : 平行平板型
電極に印加する高周波の周波数 : 13.56MHz
電極に印加する高周波出力 : 500W
装置 : 島津製作所製IBA-7500
Heエネルギー : 2.3MeV
He電荷 : 72μC
ERDA検出器角度 : 30°
試料入射角 : 75°
補助検出器(RBS)角度 : 160°
装置 : 協和界面株式会社製接触角計DropMaster300
測定方法 : 液滴法
解析方法 : θ/2法
液量 : 1μl
装置 : ULVAC Quantera SXM
Scanning X-ray Microscopy
加速電圧 : 3kV
エミッション電流 : 20μA
図15(A)~(D)は、実施例2のCxNyHz膜をスパッタしながらXPSによって深さ方向に分析した結果を示す図である。図15(A)はCxNyHz膜のOの分析結果であり、図15(B)はCxNyHz膜のNの分析結果であり、図15(C)はCxNyHz膜のCの分析結果であり、図15(D)はCxNyHz膜のSiの分析結果である。なお、図15(A)~(D)は、縦軸が原子含有量を示し、横軸がスパッタ時間を示す。
図17(A)~(D)は、比較例のDLC膜をスパッタしながらXPSによって深さ方向に分析した結果を示す図である。図17(A)はDLC膜のOの分析結果であり、図17(B)はDLC膜のNの分析結果であり、図17(C)はDLC膜のCの分析結果であり、図17(D)はDLC膜のSiの分析結果である。なお、図17(A)~(D)は、縦軸が原子含有量を示し、横軸がスパッタ時間を示す。
表1および表2に示すように、CxNyHz膜のアッシングレートは、DLC膜と同程度の値を有することが確認され、CxNyHz膜の水の接触角は50°以下になることが確認された。
2,100…被成膜基板
3…原料ガスの供給機構
4…保持電極
5…アースシールド
6,6a,6b…高周波電源
7…ガスシャワー電極(対向電極)
8a,8b…切り替えスイッチ
11,101…非磁性基板
12,102…磁性層
13,103…DLC膜
14…CxNyHz膜
15…フッ化有機膜、CaFb膜、CaFbNc膜、CaFbHd膜、CaFbOe膜、CaFbOeHd膜、CaFbNcOe膜及びCaFbNcOeHd膜のいずれかの膜
16…出発原料
17…恒温槽
18,19…バルブ
20…マスフローコントローラ
21,21a…ヒータ
22…ニードルバルブ
23a,23b,24…バルブ
25…液体MFM
27…気化器
28…供給配管
29,30…バルブ
31…マスフローコントローラ
104…CN膜
105…フッ化有機膜
Claims (16)
- 被成膜基板上に成膜されたCxNyHz膜であって、
x,y,zは下記式(1)~(4)を満たすことを特徴とするCxNyHz膜。
(1)0.4<x<0.7
(2)0.01<y<0.5
(3)0≦z<0.3
(4)x+y+z=1 - 請求項1において、
前記CxNyHz膜は水の接触角が50°以下である表面を有することを特徴とするCxNyHz膜。 - 非磁性基板上に形成された磁性層と、
前記磁性層上に形成された請求項1または2に記載のCxNyHz膜と、
前記CxNyHz膜上に形成されたフッ化有機膜と、
を具備することを特徴とする磁気記録媒体。 - 請求項3において、
前記CxNyHz膜と前記磁性層との間に形成されたDLC膜をさらに具備することを特徴とする磁気記録媒体。 - 請求項3または4において、
前記フッ化有機膜は、CaFb膜、CaFbNc膜、CaFbHd膜、CaFbOe膜、CaFbOeHd膜、CaFbNcOe膜及びCaFbNcOeHd膜のいずれかの膜であることを特徴とする磁気記録媒体。
ただし、a,b,c,d,eは、自然数である。 - 請求項5において、
前記CaFb膜、CaFbNc膜、CaFbHd膜、CaFbOe膜、CaFbOeHd膜、CaFbNcOe膜及びCaFbNcOeHd膜それぞれはアモルファス膜であることを特徴とする磁気記録媒体。
ただし、a,b,c,d,eは、自然数である。 - 請求項5または6において、
前記いずれかの膜の厚さは3nm以下であることを特徴とする磁気記録媒体。 - 被成膜基板上に、出発原料を気化させたガスを用いたCVD法により請求項1または2に記載のCxNyHz膜を成膜する成膜方法であって、
前記出発原料は、CXHYNZからなり、常温で液体または固体であり、下記式(1)~(4)を満たすことを特徴とする成膜方法。
ただし、X,Y,Zは自然数である。
(1)4≦X≦12
(2)0≦Y≦4
(3)2≦Z≦12
(4)Y/X<1 - 請求項8において、
前記出発原料は、C4H2N2、C5H3N3、C7H3N3、C6H2N4、C5H2N4、C10H2N4、C12H4N4およびC6N4のいずれか一の原料であることを特徴とする成膜方法。 - 請求項8または9に記載の成膜方法により成膜された前記CxNyHz膜上にフッ化有機膜を形成する磁気記録媒体の製造方法であって、
前記被成膜基板は、非磁性基板上に磁性層を形成したものであり、
前記CxNyHz膜は水の接触角が50°以下である表面を有することを特徴とする磁気記録媒体の製造方法。 - 請求項10において、
前記CxNyHz膜と前記磁性層との間にDLC膜を形成することを特徴とする磁気記録媒体の製造方法。 - 請求項10または11において、
前記フッ化有機膜は、原料ガスを用いたCVD法により形成されたCaFb膜、CaFbNc膜、CaFbHd膜、CaFbOe膜、CaFbOeHd膜、CaFbNcOe膜及びCaFbNcOeHd膜のいずれかの膜であり、
前記原料ガスは、炭素とフッ素を含む有機物原料ガスを有することを特徴とする磁気記録媒体の製造方法。
ただし、a,b,c,d,eは、自然数である。 - 請求項12において、
前記有機物原料ガスが3個以上の炭素を含むことを特徴とする磁気記録媒体の製造方法。 - 請求項12または13において、
前記膜上に前記CaFb膜を形成する場合の前記有機物原料ガスは、C3F6、C4F6、C6F6、C6F12、C6F14、C7F8、C7F14、C7F16、C8F16、C8F18、C9F18、C9F20、C10F8、C10F18、C11F20、C12F10、C13F28、C15F32、C20F42、及びC24F50の少なくとも一つを有し、
前記膜上に前記CaFbNc膜を形成する場合の前記有機物原料ガスは、C3F3N3、C3F9N、C5F5N、C6F4N2、C6F9N3、C6F12N2、C6F15N、C7F5N、C8F4N2、C9F21N、C12F4N4、C12F27N、C14F8N2、C15F33N、C24F45N3、及びトリヘプタフルオロプロピルアミンの少なくとも一つを有し、
前記膜上に前記CaFbOd膜を形成する場合の前記有機物原料ガスは、C3F6O、C4F6O3、C4F8O、C5F6O3、C6F4O2、C6F10O3、C8F4O3、C8F8O、C8F8O2、C8F14O3、C13F10O、C13F10O3、及びC2F6O(C3F6O)n(CF2O)mの少なくとも一つを有し、
前記膜上に前記CaFbNcOd膜を形成する場合の前記有機物原料ガスは、C7F5NOを有することを特徴とする磁気記録媒体の製造方法。 - 請求項12乃至14のいずれか一項において、
前記有機物原料ガスとしてパーフルオロアミン類を用いることを特徴とする磁気記録媒体の製造方法。 - 請求項12乃至15のいずれか一項において、
前記原料ガスを用いたCVD法は、前記CxNyHz膜を保持電極に保持し、前記保持電極に保持された前記CxNyHz膜に対向する対向電極を配置し、前記保持電極および前記対向電極の一方の電極に電力を供給して直流プラズマを形成する際の直流電圧または高周波プラズマを形成する際の直流電圧成分を+150V~-150VとしたプラズマCVD法であることを特徴とする磁気記録媒体の製造方法。
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US20140349140A1 (en) | 2014-11-27 |
JPWO2013061398A1 (ja) | 2015-04-02 |
JP6311963B2 (ja) | 2018-04-18 |
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