WO2015076190A1 - 磁気記録膜形成用スパッタリングターゲット及びその製造方法 - Google Patents

磁気記録膜形成用スパッタリングターゲット及びその製造方法 Download PDF

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WO2015076190A1
WO2015076190A1 PCT/JP2014/080144 JP2014080144W WO2015076190A1 WO 2015076190 A1 WO2015076190 A1 WO 2015076190A1 JP 2014080144 W JP2014080144 W JP 2014080144W WO 2015076190 A1 WO2015076190 A1 WO 2015076190A1
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sputtering
sputtering target
phase
alloy
mol
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PCT/JP2014/080144
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English (en)
French (fr)
Japanese (ja)
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真一 荻野
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Jx日鉱日石金属株式会社
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Priority to CN201480063680.XA priority Critical patent/CN105793465B/zh
Priority to SG11201602163YA priority patent/SG11201602163YA/en
Priority to JP2015549124A priority patent/JP6125661B2/ja
Publication of WO2015076190A1 publication Critical patent/WO2015076190A1/ja

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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
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/851—Coating a support with a magnetic layer by sputtering
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic

Definitions

  • the present invention relates to a ferromagnetic thin film sputtering target used for forming a magnetic thin film of a magnetic recording medium, in particular, a magnetic recording layer of a thermally assisted magnetic recording medium, and provides a stable discharge when sputtering with a magnetron sputtering apparatus.
  • the present invention relates to a FePt ferromagnetic sputtering target that generates less particles.
  • a material based on Co, Fe, or Ni, which is a ferromagnetic metal is used as a material for a magnetic thin film for recording.
  • a Co—Cr-based or Co—Cr—Pt-based ferromagnetic alloy containing Co as a main component has been used for a recording layer of a hard disk employing an in-plane magnetic recording method.
  • a hard disk recording layer employing a perpendicular magnetic recording system that has been put into practical use in recent years often uses a composite material composed of a Co—Cr—Pt-based ferromagnetic alloy mainly composed of Co and non-magnetic inorganic particles. It has been.
  • a magnetic thin film of a magnetic recording medium such as a hard disk is often produced by sputtering a ferromagnetic material sputtering target containing the above material as a component because of high productivity.
  • the recording density of the magnetic recording medium is rapidly increasing year by year, are believed to from a surface density of 100 Gbit / in 2 the current, future reaches 1 Tbit / in 2.
  • the size of the recording bit becomes less than 10 nm.
  • superparamagnetization due to thermal fluctuation is expected to be a problem, and magnetic recording media currently used
  • a material in which Pt is added to a Co—Cr base alloy to increase the magnetocrystalline anisotropy, or a medium in which B is further added to weaken the magnetic coupling between the magnetic grains may not be sufficient. is expected. This is because particles having a size of 10 nm or less and stably acting as ferromagnetism must have higher crystal magnetic anisotropy.
  • FePt phase having an L1 0 structure is attracting attention as a material for an ultra-high density recording medium. Further, FePt phase having an L1 0 structure corrosion and excellent oxidation resistance, it is expected that materials suitable for application as a recording medium.
  • the FePt phase rule to 1573K - has an irregular transformation point, typically having an L1 0 structure by rapid ordering reaction be quenched alloy from the hot.
  • the FePt phase is used as a material for an ultra-high density recording medium, it is necessary to develop a technology that aligns and disperses the ordered FePt particles as densely as possible in a magnetically separated state. It has been.
  • a granular structure magnetic thin film of FePt magnetic particles are magnetically separated by a non-magnetic material such as carbon having an L1 0 structure, as for a magnetic recording medium of the next generation hard disk employing a thermally assisted magnetic recording method Proposed.
  • This granular structure magnetic thin film has a structure in which magnetic particles are magnetically insulated by interposition of a nonmagnetic substance. Examples of the granular type magnetic recording medium and related literature relating thereto include Patent Literature 1, Patent Literature 2, Patent Literature 3, Patent Literature 4, Patent Literature 5, Patent Literature 6, Patent Literature 7, Patent Literature 8, and the like. be able to.
  • the magnetic recording layer is composed of a magnetic phase such as an Fe—Pt alloy and a nonmagnetic phase separating the magnetic phase, and carbon is effective as one of the materials of the nonmagnetic phase.
  • a magnetic phase such as an Fe—Pt alloy
  • a nonmagnetic phase separating the magnetic phase
  • carbon is effective as one of the materials of the nonmagnetic phase.
  • graphite has a crystal structure in which graphene sheets are laminated, and therefore has a two-dimensional orientation that it is easy to conduct electricity in the horizontal direction on the sheet surface and difficult to conduct electricity in the vertical direction. Therefore, if the orientation of graphite can be aligned, the current during sputtering can be stabilized and abnormal discharge can be suppressed.
  • such a magnetic recording layer is formed using a sputtering target made of a sintered body, but depending on the powder sintering method, it is difficult to align the orientation of the graphite in the sintered body. There was a problem that desired stable sputtering characteristics could not be obtained.
  • the magnetic recording layer is composed of a magnetic phase such as an FePt alloy and a nonmagnetic phase separating the magnetic phase, and a ferromagnetic sputtering target using carbon (C) as one of the nonmagnetic phase materials. It is an object of the present invention to provide a ferromagnetic material sputtering target that suppresses generation of particles due to abnormal discharge during sputtering.
  • the present inventor has previously succeeded in aligning the orientation of graphite in the sintered body to some extent (Japanese Patent Application No. 2012-161563).
  • Japanese Patent Application No. 2012-161563 In order to align the orientation of graphite, it is effective to make the Fe—Pt alloy powder used as a magnetic phase flat and to mix it with flaky graphite powder, but the Fe—Pt alloy powder has a particle size of Since it is fine and has a porous structure, it has been difficult to uniformly flatten it.
  • the present inventor has obtained a uniform and flattened treatment by using a dense and controlled particle size as the Fe—Pt alloy powder before the flattening treatment. It was found that Fe—Pt alloy powder can be obtained. Then, by mixing this uniformly flattened Fe—Pt alloy powder and exfoliated graphite, it becomes possible to further improve the orientation of graphite in the sintered body. Furthermore, it has been found that the abnormal discharge of sputtering can be suppressed and the generation of particles can be reduced.
  • the present invention 1) A sputtering target for forming a FePt-based magnetic recording film containing C, wherein the average thickness of the Fe—Pt alloy phase is 10 ⁇ m or more on a polished surface perpendicular to the sputtering surface , 2) A sputtering target for forming an FePt-based magnetic recording film containing C, wherein the average length of the Fe—Pt alloy phase is 20 ⁇ m or more on the polished surface perpendicular to the sputtering surface , 3) A sputtering target for forming an FePt-based magnetic recording film containing C, wherein an average length of the Fe—Pt alloy phase is 20 ⁇ m or more on a polished surface in a horizontal cross section with respect to the sputtering surface.
  • the sputtering target according to 1, 7) The sputtering according to any one of 1) to 6) above, wherein the additive contains one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides. target, 8) After cutting the Fe—Pt alloy into chips, this is pulverized and flattened to obtain Fe—Pt alloy powder.
  • exfoliated graphite powder is mixed with this Fe—Pt alloy powder, Hot-press sintering the mixed powder, and then machining the sintered body into a target shape, a sputtering target manufacturing method, 9) A method for producing a sputtering target as described in 8) above, wherein a powder of one or more metal elements selected from the group consisting of B, Ru, Ag, Au and Cu is mixed. 10) A method for producing a sputtering target as described in 8) or 9) above, wherein one or more inorganic material powders selected from the group consisting of oxides, nitrides, carbides and carbonitrides are mixed. provide.
  • the present invention relates to a sputtering target for forming a magnetic recording layer composed of a magnetic phase such as an Fe—Pt alloy and a nonmagnetic phase such as C that separates the same, and suppresses generation of particles due to abnormal discharge during sputtering. It has the outstanding effect that a ferromagnetic material sputtering target can be provided.
  • FIG. 2 is a laser micrograph showing a vertical cross-section with respect to the sputtering surface of the target structure of Comparative Example 1 (upper photo: vertical 1080 ⁇ m, horizontal 1450 ⁇ m visual field, lower photo: vertical 560 ⁇ m, horizontal 750 ⁇ m visual field). It is a laser micrograph which shows a horizontal cross section with respect to the sputter
  • the present invention relates to a sputtering target having a structure (see FIG. 7) in which a C phase of a nonmagnetic material is dispersed in a specific direction in a Fe—Pt alloy phase of a ferromagnetic material.
  • a sputtering target having a structure (see FIG. 7) in which a C phase of a nonmagnetic material is dispersed in a specific direction in a Fe—Pt alloy phase of a ferromagnetic material.
  • the sputtering target of the present invention is characterized in that the average thickness of the Fe—Pt alloy phase is 10 ⁇ m or more on the polished surface (mirror polished surface by buffing finishing) perpendicular to the sputtering surface. If the average thickness of the Fe—Pt alloy phase is less than 10 ⁇ m, the Fe—Pt alloys are likely to aggregate together, making it difficult to disperse the C phase and align it in a specific direction. By setting the average thickness of the Fe—Pt alloy phase to 10 ⁇ m or more, aggregation of the Fe—Pt alloys can be suppressed, the C phase can be uniformly dispersed in the target structure, and the orientation of the C phase can be made uniform. And stable sputtering becomes possible.
  • the “vertical cross section with respect to the sputtering surface” corresponds to a cross section perpendicular to the surface pressed during hot pressing, as shown in FIG.
  • the average thickness of the Fe—Pt alloy phase in the vertical section is calculated as follows. First, a photomicrograph of a vertical cross-section with respect to the sputtering surface is taken at three arbitrary positions in a field of view that falls in the range of 1000 ⁇ m to 1500 ⁇ m in both length and width. At this time, it adjusts so that the straight line of a perpendicular direction may become parallel to the vertical direction of a microscope picture with respect to a sputtering surface. Next, a straight line is drawn in the vertical direction of the micrograph at three arbitrary positions for each micrograph. At this time, the straight line alternately passes through the Fe—Pt alloy phase, the C phase, and the phase of other additive elements.
  • the length of the line segment from the start of passing through the phase to the end of the phase is defined as the phase thickness, and the thickness of each phase of the Fe—Pt alloy phase is measured.
  • 3 places ⁇ 3 photomicrographs Calculate the average of the measured values at a total of 9 places.
  • the visual field is preferably set to 1000 ⁇ m to 1500 ⁇ m.
  • the sputtering target of the present invention is characterized in that the average length of the Fe—Pt alloy phase is 20 ⁇ m or more on the polished surface (mirror polished surface by buffing finishing) perpendicular to the sputtering surface.
  • the Fe—Pt alloy is preliminarily flattened or thinned before mixing, but by providing a certain length in the longitudinal direction, the C phase can be easily layered in a direction perpendicular to the sputtering surface.
  • the average thickness of the Fe—Pt alloy phase is 10 ⁇ m or more and the average length of the alloy phase is 30 ⁇ m or more on the polished surface perpendicular to the sputtering surface.
  • the average thickness of the Fe—Pt alloy phase is too thick or the average length is too long, it becomes difficult to align the orientation, so the average thickness is set to 100 ⁇ m or less, or the average length is set to 400 ⁇ m or less. Is preferred.
  • the average length of the Fe—Pt alloy phase in the vertical section is calculated as follows. First, a photomicrograph of a vertical cross-section with respect to the sputtering surface is taken at three arbitrary positions in a field of view that falls in the range of 1000 ⁇ m to 1500 ⁇ m in both length and width. At this time, it adjusts so that the straight line of a perpendicular direction may become parallel to the vertical direction of a microscope picture with respect to a sputtering surface. Next, a straight line is drawn in the horizontal direction of the photomicrograph at three arbitrary positions for each photomicrograph. At this time, the straight line alternately passes through the Fe—Pt alloy phase, the C phase, and the phase of other additive elements.
  • the length of the line segment from the start of passing through the phase to the end of the phase is defined as the phase length, and the length of each phase of the Fe—Pt alloy phase is measured.
  • 3 places ⁇ 3 photomicrographs Calculate the average of the measured values at a total of 9 places.
  • the visual field is preferably set to 1000 ⁇ m to 1500 ⁇ m.
  • the sputtering target of the present invention is characterized in that the average length of the Fe—Pt alloy phase is 20 ⁇ m or more on the polishing surface having a horizontal cross section with respect to the sputtering surface (mirror polishing surface by buffing finishing). Since the Fe—Pt alloy phase has a certain length and width, the C phase can be easily layered in a direction perpendicular to the sputtering surface. More preferably, the average thickness of the Fe—Pt alloy phase is 20 ⁇ m or more and / or the average length of the alloy phase is 20 ⁇ m or more on the polished surface perpendicular to the sputtering surface, The average length of the Fe—Pt alloy phase on the polished surface is 20 ⁇ m or more.
  • the “horizontal cross section with respect to the sputter surface” corresponds to a surface that is pressed during hot pressing, as shown in FIG.
  • the average length of the Fe—Pt alloy phase in the horizontal section is calculated as follows. First, a micrograph of a horizontal cross section with respect to the sputtering surface is taken at any three locations in the field of view that falls in the range of 1000 ⁇ m to 1500 ⁇ m in both length and width. At this time, since the Fe—Pt alloy phase does not have a two-dimensional directionality in the horizontal section, it may be photographed in any orientation. Next, a straight line is drawn in the horizontal direction of the photomicrograph at three arbitrary positions for each photomicrograph. At this time, the straight line alternately passes through the Fe—Pt alloy phase, the C phase, and the phase of other additive elements.
  • the length of the line segment from the start of passing through the phase to the end of the phase is defined as the phase length, and the length of each phase of the Fe—Pt alloy phase is measured.
  • the visual field is preferably set to 1000 ⁇ m to 1500 ⁇ m.
  • the sputtering target of the present invention preferably has a Pt content of 5 mol% or more and 60 mol% or less, and the balance Fe and C. This is because if the Pt content is less than 5 mol% or exceeds 60 mol%, desired magnetic properties may not be obtained.
  • the C content is preferably 10 mol% or more and 70 mol% or less, and the balance is Fe and Pt. If the C content is less than 10 mol%, desired magnetic properties may not be obtained. On the other hand, if the C content exceeds 70 mol%, C aggregates and causes an increase in particles.
  • the sputtering target of the present invention contains 0.5 mol% or more and 10 mol% or less of one or more elements selected from the group consisting of B, Ru, Ag, Au, and Cu as additive elements in order to improve magnetic properties. It is preferable. Further, by adding one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides, the magnetic properties can be further improved.
  • the manufacturing method of the sputtering target of this invention is demonstrated.
  • an Fe raw material and a Pt raw material are melt-cast to produce an Fe—Pt alloy ingot, which is made into Fe—Pt alloy chips using a general-purpose lathe or the like.
  • the cutting depth during cutting is 0.1 to 0.3 mm.
  • the Fe raw material and the Pt raw material to be used may have any shape as long as induction heating is possible.
  • the reason why the alloy is formed by melt casting is that when the Fe powder and the Pt powder are sintered, a porous structure is formed, and the Fe—Pt alloy powder is crushed during the flattening treatment described later, and as a result. This is because the alloy powder has a small particle size.
  • the ratio of the Fe raw material and the Pt raw material can be appropriately adjusted in accordance with the desired composition of the Fe—Pt alloy.
  • metal powder such as B, Ru, Ag, Au, Cu, etc.
  • the Fe—Pt alloy chips are pulverized using a Brown horizontal pulverizer until they pass through a sieve having an opening of 150 to 400 ⁇ m. Thereafter, classification is performed using a 63 ⁇ m sieve, and the material remaining on the sieve is used as a raw material. If the particle diameter of the Fe—Pt alloy powder is too small, the alloy powder slips through the grinding media in the next step, which makes it difficult to uniformly flatten the powder. Then, it grind
  • yttria-stabilized zirconia beads having a diameter of 3 to 7 mm as the grinding media and to treat at a rotation speed of 300 rpm for about 2 to 8 hours.
  • the present invention is not limited to this condition, and any method may be used when it is recognized that a processing capability equivalent to this condition can be obtained.
  • the C raw material powder preferably has a particle size of 0.5 ⁇ m to 30 ⁇ m and an average thickness of 0.5 ⁇ m to 30 ⁇ m. If the C raw material is too fine, the C raw materials aggregate together, which is not preferable. If the C raw material is too large, the C raw material itself causes abnormal discharge, which is not preferable.
  • the above raw material powders are weighed so as to have a desired composition, and these powders are mixed using a mortar or a sieve having an opening of 150 to 500 ⁇ m.
  • metal powders such as B, Ru, Ag, Au, and Cu
  • inorganic materials such as oxides, nitrides, carbides, and carbonitrides
  • metal powders and inorganic material powders preferably have a particle size of 0.5 ⁇ m or more and 30 ⁇ m or less. If the raw material is too fine, it is not preferable because the raw materials aggregate together, and if the raw material is too large, the raw material itself causes abnormal discharge.
  • the mixed powder is filled into a carbon mold and molded and sintered by a uniaxially pressurized hot press.
  • the C phase is aligned in a specific direction during such uniaxial pressurization hot pressing.
  • the holding temperature at the time of sintering depends on the composition of the sputtering target, but in most cases, it is in the temperature range of 800 to 1600 ° C.
  • a hot isostatic pressing process can be performed to the sintered compact taken out from the hot press as needed. Hot isostatic pressing is effective for improving the density of the sintered body.
  • the holding temperature during hot isostatic pressing depends on the composition of the sintered body, but is often in the temperature range of 800 to 1600 ° C.
  • the applied pressure is set to 100 Mpa or more.
  • Example 1 First, the Fe raw material and the Pt raw material were melted by vacuum melting casting to obtain an alloy ingot having a cylindrical composition ratio of Fe-50Pt (at.%) Of about ⁇ 150. Next, after removing the surface oxide film of the obtained alloy ingot, it was set on a general-purpose lathe and cut with a cutting depth of 0.3 mm to produce Fe—Pt alloy chips. Thereafter, the Fe—Pt alloy cut powder was pulverized using a Brown horizontal pulverizer until it passed through a sieve having an opening of 150 ⁇ m, and then the fine powder was removed using a sieve having an opening of 63 ⁇ m.
  • the Fe-Pt pulverized powder is put into a medium stirring mill having a tank capacity of 5 L, and yttria-stabilized zirconia beads having a diameter of 5 mm are used as the pulverizing medium, and the processing is performed for 4 hours.
  • the processing is performed for 4 hours.
  • a wet particle size distribution made by HORIBA was used, and isopropyl alcohol was used as a dispersion solvent. As a result, a dense Fe-Pt alloy was measured.
  • the average particle size of the powder was 85 ⁇ m.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were as follows: temperature increase rate of 300 ° C./hour, holding temperature of 1100 ° C., holding time of 2 hours, and gradually increasing the Ar gas pressure from the start of temperature rising and holding at 1100 ° C.
  • the inside was pressurized at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at arbitrarily selected locations on the tissue surface with a field size of 1080 ⁇ m in length and 1450 ⁇ m in width, and a field size of 560 ⁇ m in length and 750 ⁇ m in width.
  • the captured images are shown in FIGS. 1 and 2, respectively.
  • a white portion in the tissue observation image corresponds to the Fe—Pt phase.
  • the black part corresponds to the C phase.
  • the average thickness of the Fe—Pt phase in the cross section perpendicular to the sputtering surface was measured and found to be 11.9 ⁇ m. Further, when the average length of the Fe—Pt phase in the direction parallel to the sputtering surface in the cross section perpendicular to the sputtering surface was measured, it was 29.7 ⁇ m. Furthermore, when the average length of the Fe—Pt phase in the horizontal cross section with respect to the sputtering surface was measured, it was 27.6 ⁇ m.
  • this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva) and subjected to sputtering.
  • the sputtering conditions were an input power of 1 kW and an Ar gas pressure of 1.7 Pa. After performing 2 kWhr of pre-sputtering, a film was formed on a 4-inch diameter silicon substrate for 20 seconds.
  • the number of particles adhering to the substrate was measured by a surface foreign matter inspection apparatus (Surfscan 6420, manufactured by KLA-Tencor), and as a result, it was significantly reduced from 103 to Comparative Example 1 described later. A summary of the above is shown in Table 1.
  • Example 2 First, the Fe raw material and the Pt raw material were melted by vacuum melting casting to obtain an alloy ingot having a cylindrical composition ratio of Fe-50Pt (at.%) Of about ⁇ 150. Next, after removing the surface oxide film of the obtained alloy ingot, it was set on a general-purpose lathe and cut with a cutting depth of 0.1 mm to produce Fe—Pt alloy chips. Thereafter, the Fe—Pt alloy chips were pulverized using a Brown horizontal pulverizer until they passed through a 150 ⁇ m sieve, and then fine particles were removed using a 63 ⁇ m sieve.
  • Fe—Pt chips are put into a medium stirring mill with a tank capacity of 5 L, and yttria-stabilized zirconia beads having a diameter of 5 mm are used as the grinding media for 4 hours.
  • a wet particle size distribution manufactured by HORIBA was used, and isopropyl alcohol was used as a dispersion solvent.
  • the average particle size of the Pt alloy powder was 80 ⁇ m.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were as follows: temperature increase rate of 300 ° C./hour, holding temperature of 1100 ° C., holding time of 2 hours, and gradually increasing the Ar gas pressure from the start of temperature rising and holding at 1100 ° C.
  • the inside was pressurized at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at arbitrarily selected locations on the tissue surface with a field size of 1080 ⁇ m in length and 1450 ⁇ m in width, and a field size of 560 ⁇ m in length and 750 ⁇ m in width.
  • the captured images are shown in FIGS. 3 and 4, respectively.
  • the white part of the tissue observation image corresponds to the Fe—Pt phase.
  • the black part corresponds to the C phase.
  • the average thickness of the Fe—Pt phase in the cross section perpendicular to the sputtering surface was measured and found to be 12.3 ⁇ m. Further, when the average length of the Fe—Pt phase in the direction parallel to the sputtering surface in the cross section perpendicular to the sputtering surface was measured, it was 37.1 ⁇ m. Further, when the average length of the Fe—Pt phase in the horizontal cross section with respect to the sputtering surface was measured, it was 31.9 ⁇ m.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva) and subjected to sputtering.
  • the sputtering conditions were an input power of 1 kW and an Ar gas pressure of 1.7 Pa. After performing 2 kWhr of pre-sputtering, a film was formed on a 4-inch diameter silicon substrate for 20 seconds.
  • an Fe powder having an average particle size of 3 ⁇ m and a Pt powder having an average particle size of 3 ⁇ m were prepared as raw material powders so that the composition ratio was Fe-50 Pt (at.%), And mixed for 2 hours using a mortar. It was heated to 800 ° C. in an inert atmosphere and alloyed. Thereafter, the mixture was sealed in a 5 liter medium stirring mill together with yttria-stabilized zirconia beads having a diameter of 5 mm and pulverized at 300 rpm for 4 hours to obtain an Fe—Pt alloy powder.
  • the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
  • hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were as follows: temperature increase rate of 300 ° C./hour, holding temperature of 1100 ° C., holding time of 2 hours, and gradually increasing the Ar gas pressure from the start of temperature rising and holding at 1100 ° C.
  • the inside was pressurized at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
  • tissue images were taken at arbitrarily selected locations on the tissue surface with a field size of 1080 ⁇ m in length and 1450 ⁇ m in width, and a field size of 560 ⁇ m in length and 750 ⁇ m in width.
  • the captured images are shown in FIGS. 5 and 6, respectively.
  • the white portion of the tissue observation image corresponds to the Fe—Pt phase.
  • the black part corresponds to the C phase.
  • the average thickness of the Fe—Pt phase in the cross section perpendicular to the sputtering surface was measured to be 4.4 ⁇ m. Further, when the average length of the Fe—Pt phase in the direction parallel to the sputtering surface in the cross section perpendicular to the sputtering surface was measured, it was 14.3 ⁇ m. Further, when the average length of the Fe—Pt phase in the horizontal cross section with respect to the sputtering surface was measured, it was 9.2 ⁇ m.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva) and subjected to sputtering.
  • the sputtering conditions were an input power of 1 kW and an Ar gas pressure of 1.7 Pa.
  • a film was formed on a 4-inch diameter silicon substrate for 20 seconds.
  • a surface foreign matter inspection apparatus Surfscan 6420, manufactured by KLA-Tencor
  • the present invention provides a sputtering target having a structure in which a C phase of a nonmagnetic material is dispersed in a specific direction in an Fe—Pt alloy phase. By aligning the direction of the C phase in a specific direction, the current during sputtering can be stabilized, and an excellent effect that abnormal discharge can be suppressed is obtained.
  • INDUSTRIAL APPLICABILITY The present invention is useful for a magnetic thin film of a magnetic recording medium, particularly a ferromagnetic material sputtering target for forming a granular type magnetic recording layer.

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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
PCT/JP2014/080144 2013-11-22 2014-11-14 磁気記録膜形成用スパッタリングターゲット及びその製造方法 WO2015076190A1 (ja)

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WO2023079857A1 (ja) * 2021-11-05 2023-05-11 Ｊｘ金属株式会社 Ｆｅ－Ｐｔ－Ｃ系スパッタリングターゲット部材、スパッタリングターゲット組立品、成膜方法、及びスパッタリングターゲット部材の製造方法

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WO2013046882A1 (ja) * 2011-09-26 2013-04-04 Jx日鉱日石金属株式会社 Ｆｅ－Ｐｔ－Ｃ系スパッタリングターゲット

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JP5590322B2 (ja) * 2010-11-12 2014-09-17 三菱マテリアル株式会社 磁気記録媒体膜形成用スパッタリングターゲットおよびその製造方法
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JP5041262B2 (ja) * 2011-01-31 2012-10-03 三菱マテリアル株式会社 磁気記録媒体膜形成用スパッタリングターゲットおよびその製造方法
JP5912559B2 (ja) * 2011-03-30 2016-04-27 田中貴金属工業株式会社 ＦｅＰｔ−Ｃ系スパッタリングターゲットの製造方法
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WO2023079857A1 (ja) * 2021-11-05 2023-05-11 Ｊｘ金属株式会社 Ｆｅ－Ｐｔ－Ｃ系スパッタリングターゲット部材、スパッタリングターゲット組立品、成膜方法、及びスパッタリングターゲット部材の製造方法

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CN105793465B (zh) 2019-03-22
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MY191633A (en) 2022-07-04
CN109943814A (zh) 2019-06-28
TW201531575A (zh) 2015-08-16
JPWO2015076190A1 (ja) 2017-03-16
CN105793465A (zh) 2016-07-20
JP6484276B2 (ja) 2019-03-13
MY177997A (en) 2020-09-29
SG11201602163YA (en) 2016-04-28
TWI642799B (zh) 2018-12-01

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