US20210172050A1 - Sputtering target, method for producing laminated film, laminated film and magnetic recording medium - Google Patents

Sputtering target, method for producing laminated film, laminated film and magnetic recording medium Download PDF

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US20210172050A1
US20210172050A1 US16/468,769 US201816468769A US2021172050A1 US 20210172050 A1 US20210172050 A1 US 20210172050A1 US 201816468769 A US201816468769 A US 201816468769A US 2021172050 A1 US2021172050 A1 US 2021172050A1
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sputtering target
magnetic
content
mol
metal
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Masayoshi Shimizu
Yasuyuki Iwabuchi
Manami Masuda
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JX Nippon Mining and Metals Corp
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JX Nippon Mining and Metals Corp
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Assigned to JX NIPPON MINING & METALS CORPORATION reassignment JX NIPPON MINING & METALS CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SHIMIZU, MASAYOSHI, IWABUCHI, Yasuyuki, MASUDA, MANAMI
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • 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
    • G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
    • G11B5/65—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition
    • G11B5/656—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition containing Co
    • 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
    • G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
    • G11B5/65—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition
    • G11B5/658—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition containing oxygen, e.g. molecular oxygen or magnetic oxide
    • 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
    • G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
    • G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
    • G11B5/706—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material
    • G11B5/70605—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material metals or alloys
    • G11B5/70621—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material metals or alloys containing Co metal or alloys
    • 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
    • G11B5/73—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer
    • G11B5/735—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer characterised by the back layer
    • G11B5/7353—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer characterised by the back layer for a thin film medium where the magnetic recording layer structure has no bonding agent
    • 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
    • G11B5/851—Coating a support with a magnetic layer by sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/3426—Material
    • 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
    • G11B5/73—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer
    • G11B5/739—Magnetic recording media substrates
    • G11B5/73911—Inorganic substrates
    • G11B5/73917—Metallic substrates, i.e. elemental metal or metal alloy substrates
    • G11B5/73919—Aluminium or titanium elemental or alloy substrates
    • 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
    • G11B5/73—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer
    • G11B5/739—Magnetic recording media substrates
    • G11B5/73911—Inorganic substrates
    • G11B5/73921—Glass or ceramic substrates

Definitions

  • the present invention relates to a sputtering target which contains Co and Pt as metal components and is suitable for use in forming a magnetic layer onto an intermediate layer or the like of a perpendicular magnetic recording medium, for example; to a method for producing a laminated film; and to a magnetic recording medium. More particularly, the present invention proposes a technique capable of contributing to production of a hard disk drive having high density.
  • the magnetic recording medium in the perpendicular magnetic recording method generally has a structure in which a base layer such as an adhesion layer, a soft magnetic layer, a seed layer and a Ru layer, an intermediate layer, a magnetic layer, and a protective layer, and the like are sequentially laminated on a substrate such as aluminum or glass.
  • a base layer such as an adhesion layer, a soft magnetic layer, a seed layer and a Ru layer, an intermediate layer, a magnetic layer, and a protective layer, and the like
  • a substrate such as aluminum or glass.
  • the intermediate layer laminated on a lower side of the magnetic layer includes a structure having a Co—Cr—Ru based alloy or the like dispersing the similar metal oxide therein.
  • the intermediate layer may contain a relatively large amount of Ru, Cr or the like in order to render the intermediate layer nonmagnetic.
  • the above metal oxide that will be a nonmagnetic material is precipitated at grain boundaries of magnetic particles such as a Co alloy or the like oriented in the vertical direction to reduce magnetic interaction, thereby improving noise characteristics and achieving high recording density.
  • each layer such as the magnetic layer and the intermediate layer is formed by sputtering a material onto a substrate using a sputtering target having a predetermined composition or structure to form a film.
  • a sputtering target having a predetermined composition or structure to form a film.
  • Patent Document 1 such a type of technology is disclosed in Patent Document 1 and the like.
  • Patent Document 1 Japanese Patent No. 5960287 B
  • the magnetic layer having high saturation magnetization Ms as described above has a strong exchange coupling between the magnetic particles, so that the magnetic layer has poor magnetic separation of the magnetic particles.
  • the metal oxide will enter the magnetic particles to deteriorate crystallinity of the magnetic particles, whereby the saturation magnetization Ms and the magnetic anisotropy Ku are decreased accordingly.
  • An object of this invention is to solve such problems of the prior art.
  • An object of this invention is to provide a sputtering target, a method for producing a laminated film, a laminated film and a magnetic recording medium, which can improve magnetic separation between the magnetic particles, without significantly lowering magnetic anisotropy of a magnetic layer in a magnetic recording medium.
  • the inventors have found that when Nb 2 O 5 is used as a metal oxide for a nonmagnetic material to be dispersed in a Co alloy which is a magnetic material for a magnetic layer and an intermediate layer, in addition to or in place of SiO 2 conventionally used, the magnetic separation between the magnetic particles can be significantly improved even if the content of the metal oxide is not increased so much. Further, the present inventors have found that this can allow high saturation magnetization Ms and high magnetic anisotropy Ku of the magnetic layer mainly based on Co—Pt to be maintained. Furthermore, the present inventors have found that containing both Nb 2 O 5 and TiO 2 provides further higher Ms and Ku while maintaining magnetic separation.
  • Nb 2 O 5 has reasonable wettability to Co and can form a stable oxide even if a part of oxygen is lacked so that a grain boundary having a uniform width can be formed around the magnetic grains without penetrating the oxide in the magnetic grains, although the present invention is limited to such a theory.
  • a sputtering target according to the present invention contains Co and Pt as metal components, wherein a molar ratio of a content of Pt to a content of Co is from 5/100 to 45/100, and wherein the sputtering target contains Nb 2 O 5 as a metal oxide component.
  • the sputtering target according to the present invention further contains TiO 2 as a metal oxide component.
  • the sputtering target according to the present invention has a content of Nb 2 O 5 of from 0.5 mol % to 5 mol %.
  • the content of TiO 2 is preferably from 0.5 mol % to 15 mol %.
  • the sputtering target according to the present invention has a phase including all of Ti, Nb and O.
  • the sputtering target according to the present invention further contains at least one metal oxide of SiO 2 and B 2 O 3 as a metal oxide component, and wherein the sputtering target has a total content of metal oxides including Nb 2 O 5 of from 20 vol % to 40 vol %.
  • the sputtering target according to the present invention has a molar ratio of a content of Pt to a content of Co of from 15/100 to 35/100.
  • the sputtering target according to the present invention contains Pt in an amount of from 2 mol % to 25 mol %.
  • the sputtering target according to the present invention may further contain Cr and/or Ru as a metal component(s) in an amount of from 0.5 mol % to 20 mol %.
  • a method for producing a laminated film according to the present invention comprises forming, by sputtering using any one of the sputtering targets described above, a magnetic layer on a base layer containing Ru or on an intermediate layer formed on the base layer by sputtering using a sputtering target containing Co and at least one metal selected from the group consisting of Cr and Ru as a metal component.
  • a laminated film according to the present invention comprises: a base layer containing Ru; and a magnetic layer directly formed on the base layer or indirectly formed on the base layer via an intermediate layer containing Co and at least one metal selected from the group consisting of Cr and Ru as a metal component, the magnetic layer containing Co and Pt as metal components and having a molar ratio of a content of Pt to a content of Co of from 5/100 to 45/100; wherein the magnetic layer contains Nb 2 O 5 , preferably TiO 2 in addition to Nb 2 O 5 , as a metal oxide component(s).
  • a magnetic recording medium according to the present invention comprises the laminated film as described above.
  • At least Nb 2 O 5 preferably Nb 2 O 5 together with TiO 2 is/are contained as a metal oxide component(s), so that it is possible to achieve both good magnetic separation between magnetic particles and high magnetic anisotropy Ku.
  • FIG. 1 is a schematic view showing a layer structure of a laminated film produced in Examples.
  • FIG. 2 is a graph showing a change of saturation magnetization Ms relative to a ratio Pt/Co in Examples.
  • FIG. 3 is a graph showing a change of magnetic anisotropy Ku relative to a ratio Pt/Co in Examples.
  • FIG. 4 is a graph showing a change of a slope a of a magnetization curve relative to a ratio Pt/Co in Examples.
  • FIG. 5 is SEM/EDS mapping images of targets in Examples.
  • FIG. 6 is a graph showing a result of identification of a crystal structure using XRD of a target in Examples.
  • a sputtering target according to the present invention contains Co and Pt as metal components, and has a molar ratio of a content of Pt to a content of Co of from 5/100 to 45/100, and contains Nb 2 O 5 or Nb 2 O 5 and SiO 2 as a metal oxide component(s).
  • the sputtering target has a structure in which metal oxides containing Nb 2 O 5 are dispersed in an alloy made of Co and Pt.
  • the sputtering target has a structure in which a solid solution of TiO 2 and Nb 2 O 5 is dispersed as metal oxides.
  • the sputtering target is preferably used for forming a magnetic layer, in particular located onto an intermediate layer in a perpendicular magnetic recording type magnetic recording medium.
  • the above metal components form magnetic grains and the metal oxides containing Nb 2 O 5 form nonmagnetic materials which are uniformly distributed around the magnetic grains oriented in the vertical direction, so that the magnetic interaction between the magnetic grains is effectively reduced.
  • the metal component of the sputtering target is mainly composed of Co, and, in addition, contains Pt.
  • the metal component is a Co alloy containing Pt.
  • the content of Pt is preferably from 2 mol % to 25 mol %. If the total content of Pt is too high, magnetic anisotropy may be decreased or crystallinity of the magnetic grains may be decreased. On the other hand, if the ratio of the total content of Pt to Co is too low, the magnetic anisotropy may be insufficient.
  • Pt is contained in an amount such that a molar ratio to a content of Co is from 5/100 to 45/100, because if the molar ratio of the Pt content to the Co content is less than 5/100 or more than 45/100, the magnetic anisotropy is lowered.
  • the molar ratio of the Pt content to the Co content is more preferably from 15/100 to 35/100.
  • the content of Co is too high, the magnetic anisotropy may be lowered.
  • the saturation magnetization and the magnetic anisotropy may be decreased.
  • the sputtering target according to the embodiment of the present invention may further contain Cr and/or Ru in an amount of from 0.5 mol % to 20 mol % as a metal component(s).
  • the containing of such a metal(s) provides an advantage that the saturation magnetization and the magnetic anisotropy can be adjusted while maintaining the crystallinity of the magnetic grains.
  • many of these metals are usually contained as metal components, but some of them may be included as metal oxides by being oxidized by sintering in the production, which will be described below.
  • the sputtering target according to the present invention contains at least Nb 2 O 5 as a metal oxide component.
  • Nb 2 O 5 has better wettability to Co as compared with SiO 2 or the like which is the main metal oxide in the conventional sputtering target, and forms a stable oxide even if a part of oxide is lacked. Therefore, by containing Nb 2 O 5 , the separation of magnetic grains can be improved while maintaining the magnetic anisotropy. Further, by containing both Nb 2 O 5 and TiO 2 , higher Ms and Ku can be obtained while maintaining the magnetic separation.
  • the content of Nb 2 O 5 is preferably from 0.5 mol % to 5 mol %. If the content of Nb 2 O 5 is lower, there is a possibility that the above effect cannot be sufficiently obtained. On the other hand, if the content of Nb 2 O 5 is higher, the magnetic anisotropy may be decreased. Therefore, it is even more preferable that the content of Nb 2 O 5 is from 0.5 mol % to 3 mol %.
  • the content of TiO 2 is preferably from 0.5 mol % to 15 mol %. If the content of TiO 2 is lower, there is a possibility that the above effect cannot be sufficiently obtained. On the other hand, if the content of TiO 2 is higher, an oxide volume may be increased and the magnetic anisotropy may be decreased.
  • the sputtering target more preferably has a phase containing all of Ti, Nb and O.
  • a phase includes a solid solution phase in which Nb is mixed with TiO 2 , or a solid solution phase in which Ti is mixed with Nb 2 O 5 , and a complex oxide phase such as TiNb 2 O 7 and TiNb 6 O 17 .
  • a part of oxygen may be lacked.
  • the phases in which Ti, Nb and O are mixed can be confirmed by intensity signals of Nb, Ti and O from the same position by element mapping using SEM/EDS, for example. Further, the solid solution phase and the complex oxide phase can be confirmed by XRD evaluation using X rays.
  • the sputtering target according to the embodiment of the present invention may contain metal oxides such as SiO 2 and B 2 O 3 in addition to Nb 2 O 5 and TiO 2 as metal oxide components.
  • the total content of all of the metal oxides including Nb 2 O 5 is preferably from 20 vol % to 40 vol %. If the total content of the metal oxides is less than 20 vol %, the separation of the magnetic grains may become insufficient. On the other hand, if it is more than 40 vol %, the saturation magnetization may be decreased. For these reasons, it is more preferable that the total content of metal oxides is from 25 vol % to 35 vol %.
  • the above sputtering target can be produced by a powder sintering method, and specific examples thereof are as follows.
  • the metal powder may be powder of not only a single element but also an alloy.
  • the particle diameter of the metal power is preferably in a range of from 1 ⁇ m to 10 ⁇ m, in terms of enabling homogeneous mixing to prevent segregation and coarse crystallization.
  • oxide particles as described below may not be uniformly dispersed, and when it is less than 1 ⁇ m, the sputtering target may deviate from the desired composition due to the oxidation of the metal powder.
  • the oxide powder at least Nb 2 O 5 powder and optionally at least one powder selected from the group consisting of TiO 2 powder, SiO 2 powder and B 2 O 3 powder are prepared.
  • the oxide powder has a particle diameter in a range of from 1 ⁇ m to 30 ⁇ m. This can lead to more uniform dispersion of the oxide particles in the metal phase when the oxide powder is mixed with the metal powder, and fired under pressure. If the particle diameter of the oxide powder is more than 30 ⁇ m, coarse oxide particles may be formed after firing under pressure. On the other hand, if it is less than 1 ⁇ m, agglomeration of the oxide powders may occur.
  • the above metal powder and oxide powder are weighed so as to provide a desired composition, and mixed and pulverized using a known way such as a ball mill.
  • a known way such as a ball mill.
  • This can provide mixed powder in which predetermined metal powder and oxide powder are uniformly mixed.
  • the mixed powder thus obtained is then sintered under pressure in a vacuum atmosphere or an inert gas atmosphere, and formed into a predetermined shape such as a disk shape.
  • various pressure sintering methods can be employed such as a hot press sintering method, a hot hydrostatic sintering method, a plasma discharge sintering method and the like.
  • the hot hydrostatic sintering method is effective in terms of improvement of density of a sintered body.
  • a retention temperature during the sintering is in a temperature range of from 700 to 1500° C., and particularly preferably from 800° C. to 1400° C.
  • a time for maintaining the temperature in this range is preferably 1 hour or more.
  • a pressing pressure during the sintering is preferably from 10 MPa to 40 MPa, and more preferably from 25 MPa to 35 MPa.
  • the sintered body obtained by the pressure sintering can be subjected to cutting into a desired shape using a lathe or the like or other mechanical processing to produce a sputtering target.
  • the laminated film includes, at least, a base layer; and a magnetic layer formed on the base layer.
  • the base layer contains Ru, and generally, it is composed of Ru, or it is a layer mainly based on Ru.
  • An intermediate layer can be provided between the base layer and the magnetic layer.
  • the intermediate layer contains, as metal components, Co and at least one metal selected from the group consisting of Cr and Ru, has a molar ratio of the content of at least one metal selected from the group consisting of Cr and Ru to the content of Co of 1 ⁇ 2 or more.
  • the intermediate layer preferably contains at least one selected from the group consisting of Nb 2 O 5 , TiO 2 , SiO 2 , B 2 O 3 , CoO, Co 3 O 4 , Cr 2 O 3 , Ta 2 O 5 , ZnO and MnO as a metal oxide component.
  • Nb 2 O 5 is preferably contained.
  • the content of Nb 2 O 5 in the intermediate layer may be from 5 mol % to 15 mol %, or when the intermediate layer contains other metal oxides, the content of Nb 2 O 5 may be from 2 mol % to 5 mol %.
  • the intermediate layer may further contain the above metal oxides other than Nb 2 O 5 and may have a total content of metal oxides including Nb 2 O 5 of 30 vol % or more.
  • the Co content in the intermediate layer may be from 15 mol % to 60 mol %, and the total content of Cr and Ru may be from 30 mol % to 60 mol %.
  • the intermediate layer may further contain Pt in an amount of from 2 mol % to 25 mol % as a metal component.
  • the magnetic layer contains Co and Pt as metal components, has a molar ratio of a content of Pt to a content of Co of from 5/100 to 45/100, and preferably from 15/100 to 35/100, and contains Nb 2 O 5 as a metal oxide component.
  • the containing of Nb 2 O 5 in the magnetic layer can lead to improved magnetic separation of the magnetic grains. Further, the containing of both Nb 2 O 5 and TiO 2 can increase Ms and Ku while maintaining magnetic separation.
  • the magnetic layer can be formed on the intermediate layer by sputtering using the above sputtering target.
  • the magnetic layer has a content of Nb 2 O 5 of from 0.5 mol % to 5 mol %, and when TiO 2 is contained, it has a content of TiO 2 of from 0.5 mol % to 15 mol %, and when the magnetic layer further contains at least one metal oxide selected from the group consisting of SiO 2 and B 2 O 3 as a metal oxide components, it has the total content of metal oxides including Nb 2 O 5 of from 20 vol % to 40 mol %, and the magnetic layer contains Pt in an amount of from 2 mol % to 25 mol %, and the magnetic layer further contains Cr and/or Ru in an amount of from 0.5 mol % to 20 mol % as a metal component(s).
  • Each layer in the laminated film can be produced by forming each film with a magnetron sputtering apparatus or the like using a sputtering target having a composition and a structure corresponding to each layer thereof.
  • the intermediate layer in the laminated film is formed on the base layer by sputtering using a sputtering target containing Co and at least one metal selected from the group consisting of Cr and Ru.
  • the magnetic layer in the laminated film can be formed on the intermediate layer by sputtering using the sputtering target as described above.
  • the magnetic recording medium is provided with the laminated film including the base layer, the intermediate layer formed on the base layer, and the magnetic layer formed on the intermediate layer as described above.
  • the magnetic recording medium is usually produced by sequentially forming a soft magnetic layer, a base layer, an intermediate layer, a magnetic layer, a protective layer, and the like on a substrate made of aluminum, glass or the like.
  • the sputtering target according to present invention was experimentally conducted and effects exerted by a magnetic layer formed by the sputtering target were confirmed as described below.
  • the description herein is merely for the purpose of illustration and is not intended to be limited thereto.
  • each laminated film having the layer structure shown in FIG. 1 was produced.
  • the magnetic layers shown as “Mag” in FIG. 1 were formed from the sputtering targets having different compositions as shown in Table 1. Saturation magnetization Ms, magnetic anisotropy Ku, and a slope ⁇ of a magnetization curve for a coercive force of each laminated film having each of the magnetic layers were measured, respectively.
  • the saturation magnetization Ms and the slope a of the magnetization curve were measured with a vibrated sample type magnetometer (VSM) available from TAMAGAWA CO., LTD.
  • VSM vibrated sample type magnetometer
  • TRQ magnetic torque meter
  • a volume fraction of the oxide was determined by calculating a volume of the entire target and a volume of the oxide based on the density and weight of the raw material powder, and obtaining a ratio of them.
  • FIGS. 5 and 6 Two graphs (which correspond to Invention Examples 19 and 18, respectively) of SEM/EDS mapping images of the targets and the identification results of the crystal structures of the targets using XRD are shown in FIGS. 5 and 6 .
  • the magnetic separation between the magnetic particles can be improved without greatly decreasing the magnetic anisotropy in the magnetic layer of the magnetic recording medium.

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US16/468,769 2017-09-21 2018-08-16 Sputtering target, method for producing laminated film, laminated film and magnetic recording medium Pending US20210172050A1 (en)

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MY202419A (en) 2024-04-28
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