WO2014065201A1 - Cible de pulvérisation compacte frittée à base de fer et de platine et procédé de fabrication de cette dernière - Google Patents

Cible de pulvérisation compacte frittée à base de fer et de platine et procédé de fabrication de cette dernière Download PDF

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WO2014065201A1
WO2014065201A1 PCT/JP2013/078264 JP2013078264W WO2014065201A1 WO 2014065201 A1 WO2014065201 A1 WO 2014065201A1 JP 2013078264 W JP2013078264 W JP 2013078264W WO 2014065201 A1 WO2014065201 A1 WO 2014065201A1
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sputtering
powder
plane
holding
sintered body
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PCT/JP2013/078264
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English (en)
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 CN201380046762.9A priority Critical patent/CN104781446B/zh
Priority to SG11201500762SA priority patent/SG11201500762SA/en
Priority to JP2014543263A priority patent/JP5913620B2/ja
Publication of WO2014065201A1 publication Critical patent/WO2014065201A1/fr

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    • 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
    • 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
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • 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
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/851—Coating a support with a magnetic layer by sputtering

Definitions

  • the present invention relates to an Fe—Pt-based sintered sputtering target used for manufacturing a magnetic thin film in a heat-assisted magnetic recording medium and a manufacturing method thereof.
  • materials based on Co, Fe, or Ni which are ferromagnetic metals, are used as materials for magnetic thin films in magnetic recording media.
  • a Co—Cr-based or Co—Cr—Pt-based ferromagnetic alloy containing Co as a main component has been used.
  • hard magnetic thin films employing perpendicular magnetic recording that have been put into practical use in recent years often use a composite material composed of Co—Cr—Pt-based ferromagnetic alloy mainly composed of Co and non-magnetic inorganic particles. It has been.
  • the said magnetic thin film is high in productivity, it is often produced by sputtering the sputtering target which uses the said material as a component with a DC magnetron sputtering apparatus.
  • the recording density of hard disks is rapidly increasing year by year, and it is considered that the future will reach 1 Tbit / in 2 from the current surface density of 600 Gbit / in 2 .
  • the size of the recording bit becomes less than 10 nm.
  • superparamagnetization due to thermal fluctuation is expected to be a problem.
  • a material such as a material in which Pt is added to a Co—Cr base alloy to increase the magnetocrystalline anisotropy is not sufficient. This is because magnetic particles that behave stably as ferromagnetism with a size of 10 nm or less need to 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.
  • the FePt phase is expected to be a material suitable for application as a magnetic recording medium because it has high crystal magnetic anisotropy and excellent corrosion resistance and oxidation resistance.
  • it is necessary to develop a technique that aligns and disperses ordered FePt magnetic particles with as high a density as possible in a magnetically isolated state. It has been.
  • a granular structure magnetic thin film of FePt magnetic particles are isolated by a non-magnetic material such oxides or 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.
  • a granular magnetic thin film having an Fe—Pt phase is formed using an Fe—Pt sintered sputtering target.
  • Patent Document 1 discloses a technique related to a ferromagnetic sputtering target using a metal oxide.
  • Patent Document 2 discloses a sputtering target for forming a magnetic recording medium film made of a sintered body having a structure in which a C layer is dispersed in an FePt alloy phase.
  • a sputtering target for forming a magnetic recording medium film comprising two phases, an FePt alloy phase, and an interdiffusion phase is disclosed.
  • Patent Document 4 discloses a Fe—Pt ferromagnetic sputtering target composed of Pt, SiO 2 , Sn, and the balance Fe
  • Patent Document 5 discloses quartz with respect to background intensity in X-ray diffraction. Discloses a sputtering target for a magnetic recording film having a (011) plane peak intensity ratio of 1.40 or more.
  • Hexagonal BN (a compound of boron and nitrogen) as the nonmagnetic material exhibits excellent performance as a lubricant, but when used as a raw material for powder metallurgy, it has a high density due to poor sinterability. It is difficult to produce a sintered body. And when the density of such a sintered compact is low, when processing a sintered compact into a target, defects, such as a crack and chipping, raise
  • the present invention provides an Fe—Pt-based sintered body using hexagonal BN as a nonmagnetic material, which makes it possible to produce a magnetic thin film of a heat-assisted magnetic recording medium. It is an object to provide a sputtering target with a reduced amount.
  • the present inventors have conducted intensive research.
  • the hexagonal BN which is a nonmagnetic material, has a two-dimensional crystal structure. It has been found that if the crystal orientation of the crystalline BN is random, the electric conduction is affected and abnormal discharge is generated, which causes the sputtering to become unstable.
  • the present invention 1) A Fe—Pt sintered sputtering target containing BN, which is hexagonal in a cross section perpendicular to the sputtering surface with respect to the X-ray diffraction peak intensity of the hexagonal BN (002) surface in the horizontal plane with respect to the sputtering surface.
  • a sintered body sputtering target wherein the intensity ratio of the X-ray diffraction peak intensity of the crystal BN (002) plane is 2 or more, 2) The sintered sputtering target according to 1) above, wherein the average thickness of the hexagonal BN phase in a cross section perpendicular to the sputtering surface is 30 ⁇ m or less, 3) The sintered sputtering target according to 1) or 2) above, wherein the Pt content is 5 mol% or more and 60 mol% or less. 4) The BN content is 1 mol% or more and 60 mol% or less.
  • Conjugate sputtering target 7) The sputtering target according to any one of 1) to 6) above, wherein flaky or plate-like raw material powders are mixed, molded, and then the compact is uniaxially pressed and sintered.
  • a method for producing a sputtering target is provided.
  • the Fe—Pt-based sintered body using BN as the nonmagnetic material of the present invention can suppress abnormal discharge during sputtering by improving the orientation of hexagonal BN and reduce the amount of generated particles. It has an excellent effect of being able to.
  • Example 1 It is a microscope picture of the target of Example 1 (a horizontal plane with respect to a sputtering surface and a vertical cross section with respect to a sputtering surface). It is a microscope picture of the target (a horizontal surface with respect to a sputtering surface, and a perpendicular cross section with respect to a sputtering surface) of Example 2. It is a microscope picture of the target of Example 3 (a horizontal surface with respect to a sputtering surface, and a perpendicular cross section with respect to a sputtering surface). It is a microscope picture of the target of Comparative Example 1 (horizontal plane with respect to the sputtering surface and vertical cross section with respect to the sputtering surface).
  • hexagonal BN which is a nonmagnetic material, has a two-dimensional crystal structure, if the orientation of this hexagonal BN crystal is random in the target, it will affect electrical conduction, Sputtering may become unstable. Therefore, stable sputtering can be achieved by aligning the hexagonal BN crystal in one direction.
  • the Fe—Pt-based sintered sputtering target of the present invention contains hexagonal BN as a nonmagnetic material, and has a sputter strength against the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the horizontal plane with respect to the sputtering plane.
  • the intensity ratio of the X-ray diffraction peak intensity of the hexagonal BN (002) plane in a cross section perpendicular to the plane is set to 2 or more.
  • the hexagonal BN phase is preferably flaky or plate-like, and more preferably the average of the hexagonal BN phase in a cross section perpendicular to the sputtering surface.
  • the thickness is 30 ⁇ m or less.
  • the Pt content is preferably 5 mol% or more and 60 mol% or less. By setting the Pt content to 5 mol% or more and 60 mol% or less, good magnetic properties can be obtained.
  • the content of hexagonal BN is preferably 1 mol% or more and 60 mol% or less. Magnetic insulation can be improved by making BN content as a nonmagnetic material into 1 mol% or more and 60 mol% or less.
  • the balance is Fe, except for Pt, hexagonal BN, and additional elements and additives described later.
  • additive elements selected from the group consisting of C, Ru, Ag, Au, and Cu as additive elements in a total amount of 0.5 mol% or more and 40.0 mol% or less.
  • inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides.
  • the Fe—Pt magnetic material sintered body of the present invention can be produced, for example, by the following method. First, each raw material powder (Fe powder, Pt powder, BN powder) is prepared. Moreover, alloy powder (Fe—Pt powder) may be used as the raw material powder. The alloy powder containing Pt is effective for reducing the amount of oxygen in the raw material powder, although it depends on its composition. Furthermore, each raw material powder which is an additional component hung up above is prepared as needed.
  • the metal powder (Fe powder, Pt powder) or the alloy powder (Fe—Pt alloy powder) is pulverized using a ball mill, a medium stirring mill or the like.
  • a raw material powder of metal is used in a spherical shape, a lump shape, or other irregular shape, but since hexagonal BN has a plate shape or a flake shape, when these are mixed and sintered, It becomes difficult to align the directions of hexagonal BN in the sintered body. Therefore, by making the metal raw material powder into a plate shape or a flake shape by grinding, the metal raw material and the hexagonal BN can be stacked on each other, and the orientation of the hexagonal BN can be made uniform. Become.
  • the metal powder or alloy powder obtained by pulverization in this way and the hexagonal BN powder are mixed using a mortar, a medium stirring mill, a sieve or the like.
  • Additive components and additives should be added together with the metal raw material powder, added together with the hexagonal BN powder, or mixed at the stage where the metal raw material powder and the hexagonal BN powder are mixed. Can do. Thereafter, this mixed powder is molded and sintered by hot pressing. In addition to hot pressing, a plasma discharge sintering method or a hot isostatic pressing method can also be used.
  • 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 ° C. to 1400 ° C.
  • Hot isostatic pressing is performed on the sintered body taken out from the hot press.
  • Hot isostatic pressing is effective in improving the density of the sintered body.
  • the holding temperature during hot isostatic pressing depends on the composition of the sintered body, but in many cases is in the temperature range of 800 ° C to 1200 ° C.
  • the pressing force is set to 100 MPa or more.
  • a sputtering target is producible by processing the sintered compact obtained in this way into a desired shape with a lathe.
  • the X-ray of the hexagonal BN (002) plane in the cross section perpendicular to the sputter plane with respect to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the horizontal plane with respect to the sputter plane is contained.
  • An Fe—Pt-based sintered sputtering target having a diffraction peak intensity ratio of 2 or more can be produced.
  • an X-ray diffractometer was used to measure the X-ray diffraction intensity of the horizontal plane and the cross section perpendicular to the sputtering surface with respect to the sputtering surface of the sintered body for sputtering target under the following measurement conditions. .
  • Apparatus manufactured by Rigaku Corporation (Ultima IV protectus), tube bulb: Cu, tube voltage: 40 kV, tube current: 30 mA, scanning range (2 ⁇ ): 10 ° to 90 °, measurement step (2 ⁇ ): 0.01 °, Scan speed (2 ⁇ ): 1 ° per minute, scan mode 2 ⁇ / ⁇ .
  • the diffraction peak of the hexagonal BN (002) plane appears in the vicinity of (2 ⁇ ): 26.75 °.
  • Fe—Pt alloy powder and hexagonal BN powder (flakes) were prepared as raw material powders, and these powders were weighed so as to be 70 (50Fe-50Pt) -30BN (mol%).
  • the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours.
  • the average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m.
  • the powder taken out from the medium stirring mill and the BN powder were mixed with a V-type mixer, and further mixed using a 150 ⁇ m sieve, and this mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of temperature rising to the end of holding. After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., a holding time of 2 hours, and gradually increasing the Ar gas pressure from the start of the temperature increase to 1100 ° While being held at C, it was pressurized at 150 MPa.
  • the layer has a layered structure in the direction perpendicular to the sputtering surface, and BN is oriented. Further, from FIG. 1, the average thickness of the hexagonal BN phase was 3 ⁇ m.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • 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.
  • Fe—Pt alloy powder, BN powder (flakes), and SiO 2 powder were prepared as raw material powders. These powders were weighed so as to be 70 (50Fe-50Pt) -5SiO 2 -25BN (mol%). Next, the Fe—Pt alloy powder and the SiO 2 powder were put together with a zirconia ball as a grinding medium into a medium stirring mill having a capacity of 5 L and treated at a rotational speed of 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m.
  • the powder taken out from the medium stirring mill and the BN powder were mixed with a V-type mixer, and further mixed using a 100 ⁇ m sieve, and the mixed powder was filled into a carbon mold and hot pressed.
  • the hot pressing conditions were the same as in Example 1, with a vacuum atmosphere, a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours, and the pressure was increased from 30 MPa to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours.
  • the pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • observation was performed by in-furnace SEM.
  • FIG. 2 it can be seen that BN is oriented with a layered structure in the direction perpendicular to the sputtering surface. Further, from FIG. 2, the average thickness of the hexagonal BN phase was 9 ⁇ m.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 566
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 45
  • the intensity ratio was 12.6.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 30 and good results were obtained.
  • Fe—Pt alloy powder, BN powder (flaky), Ag powder, and C (flaky graphite) powder were prepared as raw material powders. These powders were weighed so as to be 58 (35Fe-10Pt) -20Ag-20BN-2C (mol%).
  • the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m.
  • the powder taken out from the medium stirring mill, BN powder, C powder and Ag powder were mixed with a V-type mixer, mixed in a mortar, filled into a carbon mold, and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C.
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 327
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 45
  • the intensity ratio was 7.3.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, good results were obtained with 25 particles.
  • Example 4 Fe—Pt alloy powder, BN powder (flakes), and Ag powder were prepared as raw material powders. These powders were weighed so as to be 55 (45Fe-45Pt-10Ag) -45BN (mol%). Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m. The powder taken out from the medium agitation mill, BN powder and Ag powder were mixed with a V-type mixer, then mixed using a 150 ⁇ m sieve, filled into a carbon mold, and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C.
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 713
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 52
  • the intensity ratio was 13.7.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 83 particles.
  • Fe—Pt alloy powder, BN powder (flakes), Ag powder, and SiO 2 powder were prepared as raw material powders. These powders were weighed so as to be 80 (50Fe-40Pt-10Ag) -5SiO 2 -15BN (mol%).
  • the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m.
  • the powder taken out from the medium stirring mill, BN powder, Ag powder, and SiO 2 were mixed with a V-type mixer, mixed in a mortar, filled into a carbon mold, and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C.
  • the film had a layered structure in the direction perpendicular to the sputtering surface and BN was oriented.
  • the average thickness of the hexagonal BN phase was 2.4 ⁇ m.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 158
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 46
  • the intensity ratio was 3.4.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, good results were obtained with 25 particles.
  • Fe-Pt alloy powder, BN powder (flakes), and Cu powder were prepared as raw material powders. These powders were weighed so as to be 80 (50Fe-45Pt-5Cu) -20BN (mol%).
  • the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m.
  • the powder taken out from the medium agitating mill, BN powder and Cu powder were mixed with a V-type mixer, and further mixed using a 150 ⁇ m sieve, filled into a carbon mold and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C.
  • the film had a layered structure in the direction perpendicular to the sputtering surface and BN was oriented.
  • the average thickness of the hexagonal BN phase was 3 ⁇ m.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 498
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 43
  • the intensity ratio was 11.6.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. Good results were obtained with 126 particles at this time.
  • Example 7 Fe—Pt alloy powder, BN powder (flakes), and Au powder were prepared as raw material powders. These powders were weighed so as to be 80 (50Fe-45Pt-5Au) -20BN (mol%). Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m. The powder taken out from the medium agitating mill, BN powder and Au powder were mixed with a V-type mixer, and further mixed using a 150 ⁇ m sieve, filled into a carbon mold and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C.
  • the film had a layered structure in the direction perpendicular to the sputtering surface and BN was oriented.
  • the average thickness of the hexagonal BN phase was 2.5 ⁇ m.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 523
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 46
  • the intensity ratio was 11.4.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 174 particles.
  • Fe—Pt alloy powder, BN powder (flakes), Ru powder, SiO 2 powder, and TiO 2 powder were prepared as raw material powders. These powders were weighed so as to be 74 (48Fe-48Pt-4Ru) -3SiO 2 -3TiO 2 -20BN (mol%).
  • the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours.
  • the average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m.
  • the powder taken out from the medium stirring mill, BN powder, Ru powder, SiO 2 powder and TiO 2 powder were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours.
  • the pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface and BN was oriented.
  • the average thickness of the hexagonal BN phase was 2.4 ⁇ m.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • XRD X-ray diffraction method
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 369
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 42
  • the intensity ratio was 8.8.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 36 particles.
  • Example 9 Fe—Pt alloy powder, BN powder (flakes), and Cr 2 O 3 powder were prepared as raw material powders. These powders were weighed so as to be 75 (55Fe-45Pt) -5Cr 2 O 3 -20BN (mol%). Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m. The powder taken out from the medium agitating mill, BN powder and Cr 2 O 3 powder were mixed with a V-type mixer, then mixed in a mortar, filled into a carbon mold and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C.
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 252 and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 48, The intensity ratio was 5.3.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 76 particles.
  • Fe—Pt alloy powder, BN powder (flakes), Ag powder, and TiN powder were prepared as raw material powders. These powders were weighed to be 75 (45Fe-55Pt-10Ag) -3TiN-22BN (mol%).
  • the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m.
  • the powder taken out from the medium stirring mill, BN powder and TiN powder were mixed with a V-type mixer, then mixed in a mortar, filled in a carbon mold and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C.
  • the film had a layered structure in the direction perpendicular to the sputtering surface and BN was oriented.
  • the average thickness of the hexagonal BN phase was 5 ⁇ m.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 289
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 43
  • the intensity ratio was 6.7.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 129 and good results were obtained.
  • Fe—Pt alloy powder, BN powder (flakes), Ag powder, and SiC powder were prepared as raw material powders. These powders were weighed to be 75 (45Fe-55Pt-10Ag) -3TiN-22BN (mol%).
  • the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m.
  • the powder taken out from the medium agitation mill, BN powder and SiC powder were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C.
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 304
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 49
  • the intensity ratio was 6.2.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. A good result was obtained with 137 particles.
  • Example 12 Fe—Pt alloy powder and BN powder (flakes) were prepared as raw material powders. These powders were weighed so as to be 40 (55Fe-45Pt) -60BN (mol%). Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 ⁇ m. The powder taken out from the medium stirring mill and the BN powder were mixed with a V-type mixer, and further mixed using a 150 ⁇ m sieve, filled into a carbon mold and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C.
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 810
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 53
  • the intensity ratio was 15.3.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 358 particles.
  • hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours.
  • the pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. The result is shown in FIG. From FIG. 4, it was found that the layered structure was not formed in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • XRD X-ray diffraction method
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 52
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 44
  • the intensity ratio was 1.2.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 1100, which was significantly increased as compared with the example.
  • Example 2 As raw material powder, Fe powder having an average particle diameter of 5 ⁇ m, Pt powder having an average particle diameter of 6 ⁇ m, BN powder (flaky), and Ag powder were prepared. These powders were weighed so as to be 55 (45Fe-45Pt-10Ag) -45BN (mol%). Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed. The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding.
  • hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours.
  • the pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • XRD X-ray diffraction method
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 67
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 52
  • the intensity ratio was 1.3.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 860, which was significantly increased as compared with the example.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 58, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 46, The intensity ratio was 1.3.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 712, which was significantly increased as compared with the example.
  • a magnetron sputtering apparatus C-3010 sputtering system manufactured by Canon Anelva
  • hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours.
  • the pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • XRD X-ray diffraction method
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 71
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 43
  • the intensity ratio was 1.7.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 616, which was remarkably increased as compared with the example.
  • hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours.
  • the pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • XRD X-ray diffraction method
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 64
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 46
  • the intensity ratio was 1.4.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 732, which was significantly increased as compared with the example.
  • Fe powder having an average particle diameter of 5 ⁇ m, Pt powder having an average particle diameter of 6 ⁇ m, BN powder (flaky), Ru powder, TiO 2 powder, and SiO 2 powder were prepared. These powders were weighed so as to be 74 (48Fe-48Pt-4Ru) -3TiO 2 -3SiO 2 -20BN (mol%). Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 46, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 42, The intensity ratio was 1.1.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 1047, which was significantly increased as compared with the example.
  • a magnetron sputtering apparatus C-3010 sputtering system manufactured by Canon Anelva
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 52, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 48, The intensity ratio was 1.1.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 823, which was remarkably increased as compared with the example.
  • a magnetron sputtering apparatus C-3010 sputtering system manufactured by Canon Anelva
  • Fe powder having an average particle diameter of 5 ⁇ m, Pt powder having an average particle diameter of 6 ⁇ m, BN powder (flaky), Ag powder, and TiN powder were prepared as raw material powders. These powders were weighed to be 75 (45Fe-55Pt-10Ag) -3TiN-22BN (mol%). Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 53, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 43, The intensity ratio was 1.2.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. The number of particles at this time was 1079, which was significantly increased as compared with the example.
  • a magnetron sputtering apparatus C-3010 sputtering system manufactured by Canon Anelva
  • the hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber. Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 77, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 49, The intensity ratio was 1.6.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 1055, which was remarkably increased as compared with the example.
  • a magnetron sputtering apparatus C-3010 sputtering system manufactured by Canon Anelva
  • hot isostatic pressing was performed on the sintered body taken out from the hot press mold.
  • the conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours.
  • the pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C.
  • the end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface.
  • the cross section of the sintered body was measured using an X-ray diffraction method (XRD).
  • XRD X-ray diffraction method
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 82
  • the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 53
  • the intensity ratio was 1.5.
  • the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 2530, which was remarkably increased as compared with the example.
  • the Fe—Pt sintered body using BN as the nonmagnetic material of the present invention has an excellent effect of providing a sputtering target with a reduced amount of particles generated during sputtering. Therefore, it is useful as a sputtering target used for forming a magnetic thin film having a granular structure.

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Abstract

La présente invention se rapporte à une cible de pulvérisation compacte frittée à base de fer (Fe) et de platine (Pt) qui contient du nitrure de bore (BN), ladite cible de pulvérisation étant caractérisée en ce que le rapport d'intensité entre l'intensité du pic de diffraction des rayons X d'un plan (002) BN hexagonal selon un niveau plan avec la surface de pulvérisation et l'intensité du pic de diffraction des rayons X d'un plan (002) BN hexagonal selon une coupe transversale perpendiculaire à la surface de pulvérisation est égal ou supérieur à 2. La présente invention traite le problème de fournir une cible de pulvérisation avec laquelle la fabrication d'un film magnétique sur des supports d'enregistrement magnétique thermo-assisté est possible et les particules qui sont produites pendant la pulvérisation, sont réduites.
PCT/JP2013/078264 2012-10-23 2013-10-18 Cible de pulvérisation compacte frittée à base de fer et de platine et procédé de fabrication de cette dernière WO2014065201A1 (fr)

Priority Applications (3)

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CN201380046762.9A CN104781446B (zh) 2012-10-23 2013-10-18 Fe‑Pt基烧结体溅射靶及其制造方法
SG11201500762SA SG11201500762SA (en) 2012-10-23 2013-10-18 Fe-Pt-BASED SINTERED COMPACT SPUTTERING TARGET AND MANUFACTURING METHOD THEREFOR
JP2014543263A JP5913620B2 (ja) 2012-10-23 2013-10-18 Ｆｅ−Ｐｔ系焼結体スパッタリングターゲット及びその製造方法

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JP2012233999 2012-10-23

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10600440B2 (en) 2014-09-22 2020-03-24 Jx Nippon Mining & Metals Corporation Sputtering target for forming magnetic recording film and method for producing same
US20200332410A1 (en) * 2016-06-24 2020-10-22 Tosoh Smd, Inc. Tungsten-boron sputter targets and films made thereby
JP2021008641A (ja) * 2019-06-28 2021-01-28 田中貴金属工業株式会社 Ｆｅ−Ｐｔ−ＢＮ系スパッタリングターゲット及びその製造方法
US11060180B2 (en) 2016-09-12 2021-07-13 Jx Nippon Mining & Metals Corporation Ferromagnetic material sputtering target

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017141558A1 (fr) * 2016-02-19 2017-08-24 Ｊｘ金属株式会社 Cible de pulvérisation pour support d'enregistrement magnétique, et film mince magnétique
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JP6989427B2 (ja) 2018-03-23 2022-01-05 昭和電工株式会社 磁気記録媒体および磁気記録再生装置
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CN114072536B (zh) * 2019-07-12 2024-06-07 田中贵金属工业株式会社 Fe-Pt-BN系溅射靶及其制造方法
TWI752655B (zh) * 2020-09-25 2022-01-11 光洋應用材料科技股份有限公司 鐵鉑基靶材及其製法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06122504A (ja) * 1992-07-02 1994-05-06 Shin Etsu Chem Co Ltd 熱分解窒化ほう素容器
JPH0786038A (ja) * 1993-09-09 1995-03-31 Amorphous Denshi Device Kenkyusho:Kk 磁性薄膜及びその製造方法
JPH0883418A (ja) * 1994-07-11 1996-03-26 Toshiba Corp 磁気記録媒体および磁気記録再生装置
JPH0950618A (ja) * 1995-08-04 1997-02-18 Victor Co Of Japan Ltd 磁気記録媒体及びその製造方法
JP2000311329A (ja) * 1999-04-26 2000-11-07 Univ Tohoku 磁気記録媒体及び磁気記録媒体の製造方法
JP2003313659A (ja) * 2002-04-22 2003-11-06 Toshiba Corp 記録媒体用スパッタリングターゲットと磁気記録媒体
US20080210555A1 (en) * 2007-03-01 2008-09-04 Heraeus Inc. High density ceramic and cermet sputtering targets by microwave sintering

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101255546A (zh) * 2007-03-01 2008-09-03 贺利氏有限公司 通过微波烧结制备高密度陶瓷和金属陶瓷溅射靶

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06122504A (ja) * 1992-07-02 1994-05-06 Shin Etsu Chem Co Ltd 熱分解窒化ほう素容器
JPH0786038A (ja) * 1993-09-09 1995-03-31 Amorphous Denshi Device Kenkyusho:Kk 磁性薄膜及びその製造方法
JPH0883418A (ja) * 1994-07-11 1996-03-26 Toshiba Corp 磁気記録媒体および磁気記録再生装置
JPH0950618A (ja) * 1995-08-04 1997-02-18 Victor Co Of Japan Ltd 磁気記録媒体及びその製造方法
JP2000311329A (ja) * 1999-04-26 2000-11-07 Univ Tohoku 磁気記録媒体及び磁気記録媒体の製造方法
JP2003313659A (ja) * 2002-04-22 2003-11-06 Toshiba Corp 記録媒体用スパッタリングターゲットと磁気記録媒体
US20080210555A1 (en) * 2007-03-01 2008-09-04 Heraeus Inc. High density ceramic and cermet sputtering targets by microwave sintering

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LI BAO-HE: "Magnetic properties and nicrostructure of FePt/BN nanocomposite films with perpendicular magnetic anisotropy", APPL PHYS LETT, vol. 91, no. 15, 8 October 2007 (2007-10-08), pages 152502 - 1-152502-3 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10600440B2 (en) 2014-09-22 2020-03-24 Jx Nippon Mining & Metals Corporation Sputtering target for forming magnetic recording film and method for producing same
US20200332410A1 (en) * 2016-06-24 2020-10-22 Tosoh Smd, Inc. Tungsten-boron sputter targets and films made thereby
US11060180B2 (en) 2016-09-12 2021-07-13 Jx Nippon Mining & Metals Corporation Ferromagnetic material sputtering target
JP2021008641A (ja) * 2019-06-28 2021-01-28 田中貴金属工業株式会社 Ｆｅ−Ｐｔ−ＢＮ系スパッタリングターゲット及びその製造方法
JP7104001B2 (ja) 2019-06-28 2022-07-20 田中貴金属工業株式会社 Ｆｅ－Ｐｔ－ＢＮ系スパッタリングターゲット及びその製造方法

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