WO2013190943A1 - 磁気記録膜用スパッタリングターゲット - Google Patents
磁気記録膜用スパッタリングターゲット Download PDFInfo
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- WO2013190943A1 WO2013190943A1 PCT/JP2013/064242 JP2013064242W WO2013190943A1 WO 2013190943 A1 WO2013190943 A1 WO 2013190943A1 JP 2013064242 W JP2013064242 W JP 2013064242W WO 2013190943 A1 WO2013190943 A1 WO 2013190943A1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- 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
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- 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
- 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
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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
- 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
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
- G11B5/65—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition
- G11B5/658—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition containing oxygen, e.g. molecular oxygen or magnetic oxide
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
- H01F41/183—Sputtering targets therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3411—Constructional aspects of the reactor
- H01J37/3414—Targets
- H01J37/3426—Material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3411—Constructional aspects of the reactor
- H01J37/3414—Targets
- H01J37/3426—Material
- H01J37/3429—Plural materials
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- 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 sputtering target used for manufacturing a heat-assisted magnetic recording medium, and more particularly to an Fe—Pt sputtering target in which C particles are dispersed.
- 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 for a magnetic thin film of a hard disk employing an in-plane magnetic recording method.
- 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 above-mentioned magnetic thin film is often produced by sputtering a sputtering target containing the above material as a component with a DC magnetron sputtering apparatus because of its high productivity.
- FePt phase having an L1 0 structure is attracting attention as a material for an ultra-high density recording medium.
- FePt phase having an L1 0 structure with a high magnetocrystalline anisotropy, corrosion resistance and excellent oxidation resistance is what is expected as a material suitable for the application as a magnetic recording medium.
- 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.
- Patent Document 1, Patent Document 2, Patent Document 3, Patent Document 4, and Patent Document 5 can be cited as examples of magnetic recording media having a magnetic thin film having a granular structure and related documents.
- the granular structure magnetic thin film having a Fe-Pt phase with the L1 0 structure, a magnetic thin film containing 10-50% of C as a nonmagnetic material as a volume ratio, have attracted attention particularly because of their high magnetic properties . It is known that such a granular structure magnetic thin film is produced by simultaneously sputtering an Fe target, a Pt target, and a C target, or by simultaneously sputtering an Fe—Pt alloy target and a C target. However, in order to simultaneously sputter these sputtering targets, an expensive simultaneous sputtering apparatus is required.
- the magnetic recording layer is composed of a magnetic phase such as Fe—Pt and a nonmagnetic phase separating the magnetic phase, and it is known that carbon is effective as one of the nonmagnetic phases.
- carbon is a material that is difficult to sinter, and has a problem that an aggregate is easily formed between carbons. Accordingly, there is a problem that carbon lump is easily detached during sputtering, and many particles are generated on the film after sputtering. As described above, attempts have been made to improve the magnetic recording layer by introducing carbon, but the present situation has not yet solved the problem during sputtering of the target.
- Patent Document 7 the intensity I G of the band G (graphite) having a peak at approximately 1550 ⁇ 1650 cm -1 for surface enhanced Raman spectrum, the band D having a peak at approximately 1350 ⁇ 1450 cm -1 of the (disorder)
- a carbon film evaluation method having a step of evaluating the film quality of the carbon film based on the ratio I D / I G to the strength ID, and confirming that I D / I G is in the range of 0.1 to 0.5
- a carbon film evaluation method and a magnetic recording medium manufacturing method are described.
- Patent Documents 6 and 7 are merely evaluations of carbon films, and a considerable amount of carbon is included in the magnetic metal that is the main constituent material of a sputtering target for forming a magnetic recording film. If present, how the target will be affected, how it will behave during the manufacturing process of the target, and how it will be deposited when sputtered using such a target. It is not directly related to whether or not it will have a significant impact, and it cannot be said that these technologies have been fully elucidated.
- Patent Document 8 and Patent Document 9 although the magnetic recording medium is evaluated by Raman spectrum of SiC or carbon-based thin film, carbon is the main constituent material of the sputtering target for forming the magnetic recording film. How it affects the target when it is present in a significant amount in a magnetic metal, how it behaves during the manufacturing process of the target, and using such a target It is not directly related to how the film formation is affected by sputtering, and it cannot be said that these techniques have been sufficiently elucidated.
- An object of the present invention is to enable the production of a granular structure magnetic thin film without using an expensive simultaneous sputtering apparatus.
- Carbon is a material that is difficult to sinter, and has the problem of easily forming aggregates between carbons. Carbon lumps are easily detached during sputtering, and the film after sputtering
- the present inventors have conducted intensive research. As a result, the material of C, which is a nonmagnetic material, is improved, and C particles having a predetermined size are uniformly dispersed in the base metal. As a result, it is possible to prevent carbon from aggregating during pulverization and mixing, and it is possible to manufacture a high-density sputtering target that has very few particles. That is, it was found that the yield during film formation can be improved.
- a sputtering target for a magnetic recording film containing C wherein the peak intensity ratio (I G / I D ) of G band and D band in Raman scattering spectroscopy is 5.0 or more.
- Sputtering target for recording film 2)
- the sputtering target for a magnetic recording film of the present invention makes it possible to produce a magnetic thin film having a granular structure without using an expensive simultaneous sputtering apparatus.
- the sputtering target for a magnetic recording film in which C particles are dispersed, particularly Fe— It is possible to provide a Pt-based sputtering target.
- Carbon is a material that is difficult to sinter, solves the problem of easy formation of aggregates between carbons, and carbon lumps are easily detached during sputtering. It has an excellent effect that the problem that many particles are generated on the subsequent film can be solved.
- Patent Document 10 The inventors previously thought that by intentionally destroying the crystallinity of carbon, the sputtering characteristics of the carbon material can be improved and particles during sputtering can be reduced.
- extremely fine carbon particles may agglomerate, and this agglomerate may cause generation of particles during sputtering. Therefore, the inventors selected in advance a carbon material that does not easily agglomerate, and the carbon material is uniformly dispersed in the base metal (matrix) so that the carbon is not crushed during mixing. As a result, it was found that the sinterability of carbon can be improved, and particles during sputtering can be reduced.
- the sputtering target for magnetic recording film of the present invention is a sputtering target for magnetic recording film containing C, and the peak intensity ratio (I G / I D ) of G band and D band in Raman scattering spectroscopic measurement is 5 0 or more.
- the present invention is particularly effective for a sputtering target for a magnetic recording film composed of a metal having a composition in which Pt is 5 mol% or more and 60 mol% or less and the balance is Fe and C. The content of these components is a condition for obtaining good magnetic properties.
- the C content is preferably 10 mol% or more and 70 mol% or less.
- the amount of C if the content in the target composition is less than 10 mol%, good magnetic properties may not be obtained, and if it exceeds 70 mol%, C particles aggregate and many particles are generated. This is because there is a case.
- it can be set as the sputtering target for magnetic recording films whose relative density is 90% or more. It is one of the requirements of the present invention that the relative density is 90% or more. When the relative density is high, there are few problems due to degassing from the sputtering target at the time of sputtering, and the adhesion between the alloy and the C particles is improved, so that the generation of particles can be effectively suppressed. More preferably, it is 95% or more.
- the relative density is a value obtained by dividing the actually measured density of the target by the calculated density (also called the theoretical density).
- the calculated density is a density when it is assumed that the constituent elements of the target are mixed without diffusing or reacting with each other, and is calculated by the following equation.
- Calculated density Sigma ⁇ (atomic weight of constituent element x atomic ratio of constituent element) / ⁇ (atomic weight of constituent element x atomic ratio of constituent element / document value density of constituent element)
- ⁇ means taking the sum of all the constituent elements of the target.
- the sputtering target for a magnetic recording film can further contain 0.5 mol% or more and 20 mol% or less of one or more elements selected from B, Ru, Ag, Au, and Cu as additive elements. These additions are optional, but can be added depending on the material in order to improve the magnetic properties.
- the sputtering target for magnetic recording films can use ceramic materials, such as an oxide and nitride, as an additive.
- ceramic materials such as an oxide and nitride
- 0.5 mol% or more and 20 mol% or less of at least one oxide selected from SiO 2 , Cr 2 O 3 , CoO, Ta 2 O 5 , B 2 O 3 , MgO, and Co 3 O 4 is contained. It is.
- the use of these additives is optional, but can be added depending on the material in order to improve the magnetic properties.
- the primary particle diameter of the carbon raw material increases, the planar structure of the graphite increases. Therefore, the primary particle diameter is considered to have a high correlation with the crystallinity. Therefore, the inventors evaluated the crystallinity of carbon by Raman scattering spectroscopy and compared it with the amount of particles generated during sputtering, and found that there is a high correlation between the two.
- a generally known ratio of G band and D band of Raman scattering spectroscopy can be used as an index for evaluating the crystallinity (completeness of sp 2 hybrid orbitals) of the carbon material.
- the G band is a vibration mode derived from the six-membered ring structure of graphite. A peak appears in the vicinity of 1570 cm ⁇ 1 , and the peak intensity increases as the crystal structure becomes more complete.
- the D band is a vibration mode derived from the defect structure of graphite. A peak appears near 1350 cm ⁇ 1 , and the peak intensity increases as the defect increases. That is, the higher the crystallinity, the higher the I G / ID ratio. The greater the intensity of the G band, the more complete the crystal structure (higher crystallinity), and the smaller the intensity, the incomplete crystal structure (low crystalline).
- Renishaw in Via Raman Microscope was used as the Raman scattering spectrometer.
- the excitation light was Compass TM 315M Diode-Pumped Laser (manufactured by COHERENT), the excitation wavelength was 532 nm, the output of the excitation light source was 5 mW, and the diffraction grating was 1800 L / mm.
- the measurement range of Raman shift was 1033 to 1842 cm ⁇ 1 .
- the Lorentz function was used for curve fitting of measurement results. For convenience of curve fitting, a D ′ band near 1620 cm ⁇ 1 also appears, but the D ′ band is a vibration mode derived from the defect structure of graphite, and this is not directly related to the present invention. Just keep it on display.
- the present invention uses a laser excitation wavelength of 532 nm.
- the excitation light source other than this, an Ar laser, He—Ne A gas laser such as a laser or a Kr laser can be used. These lasers are appropriately selected according to the required excitation wavelength.
- the intensity I G of the G band having a peak at 1520 ⁇ 1600 cm -1 of the Raman spectrum
- the intensity I D of D band appears having a peak in 1320 ⁇ 1450 cm -1.
- the present invention can be applied. From the above, the crystallinity of the carbon material can be evaluated by calculating the peak intensity ratio between the G band and the D band (referred to as the I G / ID ratio).
- the present invention improves the sputtering characteristics by increasing the crystallinity and reduces the particles during sputtering, and the peak intensity ratio between the G band and the D band in Raman scattering spectroscopy measurement ( I G / I D ) is 5.0 or more.
- the upper limit value of the peak intensity ratio (I G / I D ) between the G band and the D band is not particularly limited, but is often 20 or less in many cases. If the peak intensity ratio (I G / ID ) is 5.0 or more, the generation of particles can be effectively suppressed.
- the peak intensity ratio of this invention measures the intensity ratio of arbitrary 10 places of a target, and makes it the average value.
- the sputtering target of the present invention is produced by a powder sintering method.
- each raw material powder for example, Fe powder, Pt powder, C powder as a typical example
- the C raw material powder has an average particle size of 0.5 to 50 ⁇ m.
- the type of C powder to be used is not particularly limited, and can be arbitrarily selected and used depending on the type of target, but exfoliated graphite has higher conductivity than graphite that has not been exfoliated and has abnormal discharge. This is preferable because Moreover, since it will become easy to aggregate when the particle diameter of C powder is too small, it is desirable to set it as 0.5 micrometer or more. On the other hand, if the particle size of the C powder is large, it may cause abnormal discharge during sputtering.
- an alloy powder Fe—Pt powder, Fe—Cu powder, Pt—Cu powder, Fe—Pt—Cu powder
- an alloy powder containing Pt is effective for reducing the amount of oxygen in the raw material powder, although it depends on its composition.
- the above powder is weighed so as to have a desired composition, mixed and pulverized. What is important is to remove a mass of several hundred ⁇ m to several mm contained in the C raw material powder by crushing or sieving in order to uniformly disperse the carbon raw material in the matrix.
- a stirring mixer, a stirring rolling mixer, a sieve of about 100 to 200 mesh, or the like can be used.
- the sieve has not only the removal of coarse particles but also the function of crushing and mixing. Further, such crushing and sieving of the C raw material powder can be performed after mixing the carbon raw material and other raw materials.
- a vertical mixer, a V-type mixer, or a mixer having performance equivalent to this can be used.
- a carbon raw material and other raw material powders are mixed.
- a mixing method a device for mixing by shearing force can be used.
- a mortar, a stirring mixer (high speed), a stirring tumbling mixer (high speed), or the like can be used.
- other devices can be used as long as shearing force is generated and the raw material is not pulverized.
- a mixing apparatus that finely pulverizes the raw material with an impact force such as a ball mill or a medium stirring mill is not preferable because it promotes the fine pulverization of the carbon raw material and promotes the aggregation of the carbon raw materials. .
- such an apparatus can be used as long as it is used for a very short time or other conditions that suppress the influence of fine grinding.
- the mixed powder thus obtained is molded and sintered with a hot press.
- 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 1000 to 1500 ° C. 25 MPa to 35 MPa. Even under this sintering condition, it is necessary to suppress aggregation of C particles.
- 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 1000 to 1500 ° C. Further, the pressure is set to 100 Mpa or more.
- the peak intensity ratio (I G / I D ) of G band and D band in the Raman scattering spectroscopic measurement in which C particles are uniformly dispersed in the alloy and high density C particles are dispersed is 5.0 or more. It is possible to produce a sputtering target for a magnetic recording film, which is characterized.
- the sputtering target of the present invention produced as described above is useful as a sputtering target used for forming a granular structure magnetic thin film.
- Example 1 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, and C powder having an average particle diameter of 15 ⁇ m were prepared as raw material powders, and weighed so that the composition was 30Fe-30Pt-40C (mol%).
- the C powder exfoliated graphite having an average particle diameter of 15 ⁇ m was used.
- the weighed C powder was sealed in a stirring mixer and crushed by rotating at 800 rpm for 5 minutes. Thereafter, the crushed C powder, Fe powder, and Pt powder were placed in a mortar and mixed for 2 hours. Next, the mixed powder taken out from the mortar was filled into a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., and 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 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. After completion of the holding, it was naturally cooled in the furnace.
- a structural photograph of the sintered body thus produced is shown in FIG. Thus, it can be seen that C particles having the same size as the particle diameter of the input raw material remain.
- the density of the sintered body was measured by the Archimedes method, and the relative density was calculated to be 97.1%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- FIG. 2 shows the results of Raman scattering spectroscopy measurement and curve fitting of Fe—Pt—C.
- the I G / ID ratio was 7.05, which satisfied the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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 number of particles at this time was 64 as shown in Table 1. It was a piece. Compared to the comparative example, it was greatly reduced.
- Example 2 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, and C powder having an average particle diameter of 15 ⁇ m were prepared as raw material powders, and weighed so that the composition was 30Fe-30Pt-40C (mol%).
- the C powder exfoliated graphite having an average particle diameter of 15 ⁇ m was used.
- the weighed C powder was sealed in a stirring mixer and crushed by rotating at 800 rpm for 5 minutes. Thereafter, the pulverized C powder, Fe powder, and Pt powder were put into a 5 L-type medium stirring mill and mixed by rotating at 300 rpm for 1 hour. Next, the mixed powder taken out from the stirring mill was filled in a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., and 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 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. After completion of the holding, it was naturally cooled in the furnace.
- a structural photograph of the sintered body thus produced is shown in FIG. Thus, it can be seen that C particles having the same size as the particle diameter of the input raw material remain. Further, the density of the sintered body was measured by the Archimedes method, and the relative density was calculated to be 97.0%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- FIG. 4 shows the results of Raman scattering spectroscopy measurement and curve fitting of Fe—Pt—C.
- the I G / ID ratio was 5.02, satisfying the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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
- Example 3 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, and C powder having an average particle diameter of 0.5 ⁇ m were prepared as raw material powders, and weighed so that the composition would be 30Fe-30Pt-40C (mol%).
- the C powder graphite having an average particle diameter of 0.5 ⁇ m was used.
- the weighed C powder was sealed in a stirring mixer and crushed by rotating at 800 rpm for 5 minutes. Thereafter, the pulverized C powder, Fe powder, and Pt powder were placed in a 5 L-type medium agitating mill and mixed by rotating at 300 rpm for 30 minutes. Next, the mixed powder taken out from the stirring mill was filled in a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., and 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.
- FIG. 5 shows a structure photograph of the sintered body thus produced.
- C particles having the same size as the particle diameter of the input raw material remain.
- the density of the sintered body was measured by the Archimedes method, and the relative density was calculated to be 96.5%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- FIG. 6 shows the results of Raman scattering spectroscopy measurement and curve fitting of Fe—Pt—C.
- the I G / ID ratio was 5.93, satisfying the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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
- Example 4 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, and C powder having an average particle diameter of 20 ⁇ m were prepared as raw material powders, and weighed so that the composition would be 30Fe-30Pt-40C (mol%).
- the C powder graphite having an average particle diameter of 20 ⁇ m was used.
- the weighed raw material powder was passed through a 100 mesh sieve, and then put into a stirring mixer (high speed), and mixed by rotating at 1300 rpm for 5 minutes.
- the mixed powder taken out from the stirring mixer was filled in a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., and 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.
- FIG. 7 shows a structure photograph of the sintered body thus produced.
- C particles having the same size as the particle diameter of the input raw material remain.
- the density of the sintered body was measured by Archimedes method, and the relative density was calculated to be 96.6%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- FIG. 8 shows the results of Raman scattering spectroscopy measurement and curve fitting of Fe—Pt—C.
- the I G / ID ratio was 6.52, satisfying the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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
- Example 5 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, Ag powder having an average particle diameter of 3 ⁇ m, and C powder having an average particle diameter of 20 ⁇ m are prepared as raw material powders, and the composition is 35Fe-25Pt-35C-5Ag (mol%) ).
- the C powder graphite having an average particle diameter of 20 ⁇ m was used.
- the weighed raw material powder was sealed in a vertical mixer and mixed. Then, after passing through a 200 mesh sieve, the raw material powder was mixed in a mortar for 2 hours. Next, the mixed powder taken out from the mortar was filled into a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressure was applied 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.
- FIG. 9 shows a structure photograph of the sintered body thus produced.
- C particles having the same size as the particle diameter of the input raw material remain.
- the density of the sintered body was measured by the Archimedes method, and the relative density was calculated to be 97.0%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- FIG. 10 shows the results of Raman scattering spectroscopy measurement and curve fitting of Fe—Pt—C.
- the I G / ID ratio was 5.84, which satisfied the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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 device Surfscan 6420, manufactured by KLA-Tencor
- Example 6 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, and C powder having an average particle diameter of 15 ⁇ m were prepared as raw material powders, and weighed so that the composition was 25Fe-25Pt-50C (mol%).
- the C powder exfoliated graphite having an average particle diameter of 15 ⁇ m was used.
- the weighed raw material powder was sealed in a V-type mixer and mixed. Thereafter, the mixture was crushed at 800 rpm for 5 minutes using a stirring mixer, and then mixed in a mortar for 2 hours. Next, the mixed powder taken out from the mortar was filled into a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., and 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 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. After completion of the holding, it was naturally cooled in the furnace.
- the density of the sintered body thus produced was measured by the Archimedes method, and the relative density was calculated to be 96.1%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- the I G / ID ratio was 6.93, which satisfied the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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
- Example 7 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, and C powder having an average particle diameter of 15 ⁇ m were prepared as raw material powders, and weighed so that the composition would be 45Fe-45Pt-10C (mol%).
- the C powder exfoliated graphite having an average particle diameter of 15 ⁇ m was used.
- the weighed raw material powder was sealed in a V-type mixer and mixed. Thereafter, the mixture was crushed at 800 rpm for 5 minutes using a stirring mixer, and then mixed in a mortar for 2 hours. Next, the mixed powder taken out from the mortar was filled into a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1300 ° C., and 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 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. After completion of the holding, it was naturally cooled in the furnace.
- the density of the sintered body thus produced was measured by the Archimedes method, and the relative density was calculated to be 97.6%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- the I G / ID ratio was 6.85, which satisfied the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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
- Example 8 As raw material powder, Fe powder having an average particle size of 3 ⁇ m, Pt powder having an average particle size of 3 ⁇ m, Ru powder having an average particle size of 3 ⁇ m, C powder having an average particle size of 20 ⁇ m, TiO 2 powder having an average particle size of 1 ⁇ m, and an average particle size of 0.5 ⁇ m. SiO 2 powder and Cr 2 O 3 powder having an average particle size of 0.5 ⁇ m were prepared and weighed so that the composition was 39Fe-40Pt-2Ru-10C-3TiO 2 -3SiO 2 -3Cr 2 O 3 (mol%) did. As the C powder, graphite having an average particle diameter of 20 ⁇ m was used.
- the weighed raw material powder was sealed in a vertical mixer and mixed. Thereafter, the mixture was crushed at 800 rpm for 5 minutes using a stirring mixer, and then mixed in a mortar for 2 hours. Next, the mixed powder taken out from the mortar was filled into a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1100 ° C., and 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 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. After completion of the holding, it was naturally cooled in the furnace.
- the density of the sintered body thus produced was measured by the Archimedes method, and the relative density was calculated to be 99.1%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- the I G / ID ratio was 6.27, which satisfied the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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 device Surfscan 6420, manufactured by KLA-Tencor
- Example 9 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, and C powder having an average particle diameter of 15 ⁇ m were prepared as raw material powders, and weighed so that the composition would be 30Fe-60Pt-10C (mol%).
- the C powder exfoliated graphite having an average particle diameter of 15 ⁇ m was used.
- the weighed raw material powder was passed through a 100 mesh sieve, and then placed in a mortar and mixed for 2 hours.
- the mixed powder taken out from the mortar was filled into a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1300 ° C., and 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 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. After completion of the holding, it was naturally cooled in the furnace.
- the density of the sintered body thus produced was measured by Archimedes method, and the relative density was calculated to be 97.9%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- the I G / ID ratio was 7.02, satisfying the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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.
- the number of particles at this time was 23 as shown in Table 1. It was a piece. Compared to the comparative example, it was greatly reduced.
- Example 10 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, and C powder having an average particle diameter of 15 ⁇ m were prepared as raw material powders, and weighed so that the composition would be 55Fe-5Pt-40C (mol%).
- the C powder exfoliated graphite having an average particle diameter of 6 ⁇ m was used.
- the weighed raw material powder was passed through a 100 mesh sieve, and then placed in a mortar and mixed for 2 hours.
- the mixed powder taken out from the mortar was filled into a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., and 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 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. After completion of the holding, it was naturally cooled in the furnace.
- the density of the sintered body thus produced was measured by the Archimedes method, and the relative density was calculated to be 96.7%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- the I G / ID ratio was 6.94, which satisfied the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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
- Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, C powder having an average particle diameter of 15 ⁇ m, and Au powder having an average particle diameter of 5 ⁇ m are prepared as raw material powder, and the composition is 30Fe-45Pt-20C-5Au (mol%). ).
- the C powder exfoliated graphite having an average particle diameter of 15 ⁇ m was used.
- the weighed raw material powder was sealed in a vertical mixer, mixed, and then crushed using a stirring mixer at 800 rpm for 5 minutes. Then, it mixed at 1300 rpm for 5 minutes using the stirring mixer (high speed). Next, the mixed powder taken out from the stirring mixer was filled in a carbon mold and hot-pressed.
- the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1350 ° 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.
- 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. After completion of the holding, it was naturally cooled in the furnace.
- the density of the sintered body thus produced was measured by the Archimedes method, and the relative density was calculated to be 96.8%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- the I G / ID ratio was 6.69, which satisfied the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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
- Example 12 Fe powder having an average particle diameter of 3 ⁇ m, Pt powder having an average particle diameter of 3 ⁇ m, C powder having an average particle diameter of 15 ⁇ m, and Cu powder having an average particle diameter of 5 ⁇ m are prepared as raw material powders, and the composition is 35Fe-35Pt-20C-10Cu (mol%). ).
- the C powder exfoliated graphite having an average particle diameter of 15 ⁇ m was used.
- the weighed raw material powder was sealed in a vertical mixer, mixed, and then crushed using a stirring mixer at 800 rpm for 5 minutes. Then, it mixed at 1300 rpm for 5 minutes using the stirring mixer (high speed). Next, the mixed powder taken out from the stirring mixer was filled in 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 1350 ° C., and a holding time of 2 hours. 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 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. After completion of the holding, it was naturally cooled in the furnace.
- the density of the sintered body thus produced was measured by the Archimedes method, and the relative density was calculated to be 97.2%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- the I G / ID ratio was 6.92, which satisfied the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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.
- the number of particles at this time was 42 as shown in Table 1. It was a piece. Compared to the comparative example, it was greatly reduced.
- Fe powder having an average particle size of 3 ⁇ m, Pt powder having an average particle size of 3 ⁇ m, C powder having an average particle size of 15 ⁇ m, and B powder having an average particle size of 10 ⁇ m are prepared as raw material powder, and the composition is 43Fe-45Pt-2B-10C (mol%).
- the C powder exfoliated graphite having an average particle diameter of 15 ⁇ m was used.
- the weighed raw material powder was sealed in a vertical mixer, mixed, and then crushed using a stirring mixer at 800 rpm for 5 minutes. Then, it mixed at 1300 rpm for 5 minutes using the stirring mixer (high speed). Next, the mixed powder taken out from the stirring mixer was filled in 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.
- 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. After completion of the holding, it was naturally cooled in the furnace.
- the density of the sintered body thus produced was measured by the Archimedes method, and the relative density was calculated to be 97.1%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- the I G / ID ratio was 6.88, which satisfied the condition that the I G / ID ratio of the present invention was 5.0 or more.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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
- Fe powder with an average particle size of 3 ⁇ m, Pt powder with an average particle size of 3 ⁇ m, C powder with an average particle size of 15 ⁇ m, Ta 2 O 5 powder with an average particle size of 1 ⁇ m, B 2 O 3 powder with an average particle size of 1 ⁇ m, average A 3MgO powder having a particle diameter of 1 ⁇ m and a CoO powder having an average particle diameter of 1 ⁇ m were prepared and weighed so that the composition was 40Fe-40Pt-10C-3Ta 2 O 5 -3B 2 O 3 -3MgO-1CoO (mol%).
- the C powder exfoliated graphite having an average particle diameter of 15 ⁇ m was used.
- the weighed raw material powder was sealed in a vertical mixer, mixed, and then crushed using a stirring mixer at 800 rpm for 5 minutes. Then, it mixed for 2 hours using the mortar. Next, the mixed powder taken out from the stirring mixer was filled in a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1100 ° C., and 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 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. After completion of the holding, it was naturally cooled in the furnace.
- the density of the sintered body thus produced was measured by the Archimedes method, and the relative density was calculated to be 98.2%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- the I G / ID ratio was 6.29, and the condition that the I G / ID ratio of the present invention was 5.0 or more was satisfied.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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 weighed raw material powder was sealed in a vertical mixer and mixed. Then, after passing through a 200 mesh sieve, it was mixed for 20 hours at 300 rpm using a 5 L medium stirring mill. Next, the mixed powder taken out from the stirring mill was filled in a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., and 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.
- FIG. 11 shows a structure photograph of the sintered body thus produced.
- the density of the sintered body was measured by the Archimedes method, and the relative density was calculated to be 96.7%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- FIG. 12 shows the results of Raman scattering spectroscopy measurement and curve fitting of Fe—Pt—C.
- the I G / ID ratio was 2.05, and the condition that the I G / ID ratio of the present invention was 5.0 or more was not satisfied.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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 weighed raw material powder was sealed in a vertical mixer and mixed. Then, after passing through a 100 mesh sieve, mixing was performed at 300 rpm for 48 hours using a 5 L medium stirring mill. Next, the mixed powder taken out from the stirring mill was filled in a carbon mold and hot-pressed.
- the hot press conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1400 ° C., and 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 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. After completion of the holding, it was naturally cooled in the furnace.
- the structure of the sintered body thus produced is shown in FIG. Thus, it can be seen that there are C particles in which the input raw material is finely pulverized.
- the density of the sintered body was measured by the Archimedes method, and the relative density was calculated to be 96.8%.
- this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to obtain a target.
- Raman scattering spectroscopic measurement conditions were an excitation wavelength of 532 nm, an output of 5 mW, and a diffraction grating of 1800 L / mm.
- the Lorentz function was used for curve fitting of measurement results.
- FIG. 14 shows the results of Raman scattering spectroscopy measurement and curve fitting of Fe—Pt—C.
- the I G / ID ratio was 1.70, and the condition that the I G / ID ratio of the present invention was 5.0 or more was not satisfied.
- this target was attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), and sputtering was performed.
- 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 sputtering target for a magnetic recording film of the present invention makes it possible to produce a granular structure magnetic thin film without using an expensive simultaneous sputtering apparatus.
- a sputtering target can be provided, and carbon is a material that is difficult to sinter, which solves the problem of easy formation of aggregates between carbons, and carbon lumps are easily detached during sputtering. It has an excellent effect that the problem that a large number of particles are generated on the film can be solved. Therefore, it is useful as a sputtering target for forming a magnetic thin film having a granular structure.
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Abstract
Description
また、近年実用化された垂直磁気記録方式を採用するハードディスクの磁性薄膜には、Coを主成分とするCo-Cr-Pt系の強磁性合金と非磁性の無機物粒子からなる複合材料が多く用いられている。そして上記の磁性薄膜は、生産性の高さから、上記材料を成分とするスパッタリングターゲットをDCマグネトロンスパッタ装置でスパッタして作製されることが多い。
そしてFePt相を超高密度記録媒体用材料として使用する場合には、規則化したFePt磁性粒子を磁気的に孤立させた状態で出来るだけ高密度に方位をそろえて分散させるという技術の開発が求められている。
このグラニュラー構造磁性薄膜は、磁性粒子同士が非磁性物質の介在により磁気的に絶縁される構造となっている。
グラニュラー構造の磁性薄膜を有する磁気記録媒体及びこれに関連する公知文献としては、特許文献1、特許文献2、特許文献3、特許文献4、特許文献5を挙げることができる。
また、一般に磁気記録層はFe-Ptなどの磁性相とそれを分離している非磁性相から構成されており、非磁性相の一つとして炭素が有効であることが知られている。
このように、炭素を導入することによる磁気記録層の改善が試みられているが、ターゲットのスパッタリング時の問題を解決するには至っていないのが現状である。
一つの波形(A)のピーク位置が1545cm-1以下、他の波形(B)のピーク位置が1320~1360cm-1であり、これらの波形の半値幅における面積比(B/A)が0.3~0.7となる非晶質水素化カーボン層からなる磁気ディスク及びその製造方法が記載されている。
1)Cを含有する磁気記録膜用スパッタリングターゲットであって、ラマン散乱分光測定におけるGバンドとDバンドのピーク強度比(IG/ID)が5.0以上であることを特徴とする磁気記録膜用スパッタリングターゲット。
2)Ptが5mol%以上60mol%以下、残余がFeである組成の金属とCからなる上記1)記載の磁気記録膜用スパッタリングターゲット。
3)Cの含有割合が10mol%以上70mol%以下であることを特徴とする上記1)又は2)記載の磁気記録膜用スパッタリングターゲット。
4)相対密度が90%以上であることを特徴とする上記1)~3)のいずれか一項に記載の磁気記録膜用スパッタリングターゲット。
5)添加元素として、B、Ru、Ag、Au、Cuから選択した1元素以上を、0.5mol%以上20mol%以下含有することを特徴とする上記1)~4)のいずれか一項に記載の磁気記録膜用スパッタリングターゲット、
6)添加剤として、SiO2、Cr2O3、CoO、Ta2O5、B2O3、MgO、Co3O4から選択した1種以上の酸化物を、0.5mol%以上20mol%以下を含有することを特徴とする上記1)~5)のいずれか一項に記載の磁気記録膜用スパッタリングターゲット。
そこで、発明者らは、炭素の原料として凝集しにくい大きさのものをあらかじめ選択し、混合中に炭素が粉砕されないように、かつ、炭素原料を母材金属(マトリックス)中に一様に分散させることによって、炭素の焼結性を向上させることができ、スパッタリング時のパーティクルを低減できることを見出した。
この場合、Ptが5mol%以上60mol%以下、残余がFeである組成の金属とCからなる磁気記録膜用スパッタリングターゲットに、特に有効である。これらの成分の含有量は、良好な磁気特性を得るための条件である。
また、相対密度が90%以上の磁気記録膜用スパッタリングターゲットとすることができる。相対密度が90%以上であることは、本発明の要件の一つである。相対密度が高いと、スパッタ時にスパッタリングターゲットからの脱ガスによる問題が少なく、また、合金とC粒子の密着性が向上するため、パーティクル発生を効果的に抑制できるからである。より好ましくは95%以上とする。
式:計算密度=シグマΣ(構成元素の原子量×構成元素の原子数比)/Σ(構成元素の原子量×構成元素の原子数比/構成元素の文献値密度)
ここで、Σは、ターゲットの構成元素の全てについて、和をとることを意味する。
炭素材料の結晶性(sp2混成軌道の完全性)を評価するための指標として、一般的に知られているラマン散乱分光測定のGバンドとDバンドの比を用いることができる。
また、Dバンドは、グラファイトの欠陥構造に由来する振動モードであり、1350cm-1付近にピークが現れ、欠陥が大きいほどピーク強度は大きくなる。
すなわち、結晶性が高い炭素材料ほどIG/ID比が高くなる。Gバンドの強度が大きいほど結晶構造が完全(結晶性が高い)、小さいほど結晶構造が不完全(結晶性が低い)である。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。なお、カーブフィッティングをする都合上、1620cm-1付近のD´バンドも現れるが、D´バンドはグラファイトの欠陥構造に由来する振動モードであり、これは本願発明には、直接関係しないので、図において表示するに留める。
この場合は、ラマンスペクトルの1520~1600cm-1にピークを有するGバンドの強度IG と、1320~1450cm-1にピークを有するDバンドの強度IDが現れる。これらの場合においても、本願発明を適用できるものである。
以上から、GバンドとDバンドのピーク強度比(IG/ID比と呼ぶことにする)を計算することで、炭素材料の結晶性を評価できる。
これによって、炭素同士で凝集体を形成し易いという問題を解決し、さらにスパッタリング中に炭素が容易に脱離し、スパッタリング後の膜上にパーティクルが多数発生するのを抑制することができる。
GバンドとDバンドのピーク強度比(IG/ID)の上限値は、特に制限はないが、多くの場合20以下となる。ピーク強度比(IG/ID)が5.0以上であれば、パーティクルの発生を効果的に抑制できる。なお、本発明のピーク強度比は、ターゲットの任意10箇所の強度比を測定し、その平均値としている。
Fe粉末やPt粉末は、平均粒径が0.5μm以上10μm以下のものを用いることが望ましい。これらの原料粉末の粒径が小さ過ぎると、酸化が促進されてスパッタリングターゲット中の酸素濃度が上昇するなどの問題があるため、0.5μm以上とすることが望ましい。一方、これらの原料粉末の粒径が大きいと、C粒子を合金中に微細分散することが難しくなるため10μm以下のものを用いることがさらに望ましい。
また、C粉末の粒子径が小さ過ぎると、凝集しやすくなるため0.5μm以上とすることが望ましい。一方、C粉末の粒子径が大きいと、スパッタリング時の異常放電の原因となるため、50μm以下とすることが望ましい。
重要なことは、炭素原料をマトリックス中に一様に分散させるために、C原料粉末に含まれている数百μm~数mmの大きさの塊を解砕あるいはふるいで取り除くことである。方法としては、攪拌混合機、攪拌転動混合機、100~200メッシュ程度のふるい等を使用することができる。なお、ふるいは、粗大粒の除去だけではなく、解砕や混合の機能も兼ね備えるものである。
また、このようなC原料粉末の解砕やふるい分けは、炭素原料とその他の原料を混合した後に行うこともできる。混合装置としては、縦型ミキサー、V型混合機もしくはこれに準ずる性能を有する混合機を使用することができる。
このようにしてC原料粉末に含まれる大きな塊を排除した後に、炭素原料とその他の原料粉を混合する。混合方法としては、せん断力によって混合する装置を使用することができる。例えば、乳鉢、攪拌混合機(高速)、攪拌転動混合機(高速)等を使用することができる。また、せん断力が発生し、かつ原料が微粉砕しない装置であれば、その他の装置を使用することもできる。
一方で、ボールミルや媒体攪拌ミル等のように衝撃力で原料を微粉砕してしまうような混合装置は、炭素原料の微粉砕を促進し、炭素原料同士の凝集を助長してしまうため好ましくない。但し、ごく短時間の使用その他の微粉砕の影響を抑える条件であれば、このような装置を使用することも可能である。
このようにして得られた焼結体を旋盤で所望の形状に加工することにより、本発明のスパッタリングターゲットは作製できる。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末を用意し、組成が30Fe-30Pt-40C(mol%)となるように秤量した。C粉末には平均粒子径15μmの薄片化黒鉛を使用した。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。Fe-Pt-Cのラマン散乱分光測定結果とカーブフィッティング結果を図2に示す。IG/ID比は7.05となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は64個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末を用意し、組成が30Fe-30Pt-40C(mol%)となるように秤量した。C粉末には平均粒子径15μmの薄片化黒鉛を使用した。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。Fe-Pt-Cのラマン散乱分光測定結果とカーブフィッティング結果を図4に示す。IG/ID比は5.02となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は153個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径0.5μmのC粉末を用意し、組成が30Fe-30Pt-40C(mol%)となるように秤量した。C粉末には平均粒子径0.5μmのグラファイトを使用した。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。Fe-Pt-Cのラマン散乱分光測定結果とカーブフィッティング結果を図6に示す。IG/ID比は5.93となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は116個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径20μmのC粉末を用意し、組成が30Fe-30Pt-40C(mol%)となるように秤量した。C粉末には平均粒子径20μmのグラファイトを使用した。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。Fe-Pt-Cのラマン散乱分光測定結果とカーブフィッティング結果を図8に示す。IG/ID比は6.52となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は121個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒径3μmのAg粉末、平均粒子径20μmのC粉末を用意し、組成が35Fe-25Pt-35C-5Ag(mol%)となるように秤量した。C粉末には平均粒子径20μmのグラファイトを使用した。
次に、乳鉢から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度950°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。Fe-Pt-Cのラマン散乱分光測定結果とカーブフィッティング結果を図10に示す。IG/ID比は5.84となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は28個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末を用意し、組成が25Fe-25Pt-50C(mol%)となるように秤量した。C粉末には平均粒子径15μmの薄片化黒鉛を使用した。
次に、乳鉢から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1400°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。その結果、IG/ID比は6.93となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は102個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末を用意し、組成が45Fe-45Pt-10C(mol%)となるように秤量した。C粉末には平均粒子径15μmの薄片化黒鉛を使用した。
次に、乳鉢から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1300°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。その結果、IG/ID比は6.85となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は24個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒径3μmのRu粉末、平均粒子径20μmのC粉末、平均粒径1μmのTiO2粉末、平均粒径0.5μmのSiO2粉末、平均粒径0.5μmのCr2O3粉末を用意し、組成が39Fe-40Pt-2Ru-10C-3TiO2-3SiO2-3Cr2O3(mol%)となるように秤量した。C粉末には平均粒子径20μmのグラファイトを使用した。
次に、乳鉢から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1100°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。その結果、IG/ID比は6.27となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は13個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末を用意し、組成が30Fe-60Pt-10C(mol%)となるように秤量した。C粉末には平均粒子径15μmの薄片化黒鉛を使用した。
次に、乳鉢から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1300°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。その結果、IG/ID比は7.02となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は23個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末を用意し、組成が55Fe-5Pt-40C(mol%)となるように秤量した。C粉末には平均粒子径6μmの薄片化黒鉛を使用した。
次に、乳鉢から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1400°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。その結果、IG/ID比は6.94となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は97個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末、平均粒径5μmのAu粉末を用意し、組成が30Fe-45Pt-20C-5Au(mol%)となるように秤量した。C粉末には平均粒子径15μmの薄片化黒鉛を使用した。
次に、攪拌混合機から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1350°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。その結果、IG/ID比は6.69となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は56個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末、平均粒径5μmのCu粉末を用意し、組成が35Fe-35Pt-20C-10Cu(mol%)となるように秤量した。C粉末には平均粒子径15μmの薄片化黒鉛を使用した。
次に、攪拌混合機から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1350°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。その結果、IG/ID比は6.92となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は42個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末、平均粒径10μmのB粉末を用意し、組成が43Fe-45Pt-2B-10C(mol%)となるように秤量した。C粉末には平均粒子径15μmの薄片化黒鉛を使用した。
次に、攪拌混合機から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1200°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。その結果、IG/ID比は6.88となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は72個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径15μmのC粉末、平均粒径1μmのTa2O5粉末、平均粒径1μmのB2O3粉末、平均粒径1μmの3MgO粉末、平均粒径1μmのCoO粉末を用意し、組成が40Fe-40Pt-10C-3Ta2O5-3B2O3-3MgO-1CoO(mol%)となるように秤量した。C粉末には平均粒子径15μmの薄片化黒鉛を使用した。
次に、攪拌混合機から取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1100°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。その結果、IG/ID比は6.29となり、本願発明のIG/ID比が5.0以上という条件を満たしていた。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は24個であった。比較例に比べて大きく減少した。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径20μmのC粉末を用意し、組成が30Fe-30Pt-40C(mol%)となるように秤量した。C粉末には平均粒子径20μmのグラファイトを使用した。
次に、攪拌ミルから取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1400°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。Fe-Pt-Cのラマン散乱分光測定結果とカーブフィッティング結果を図12に示す。IG/ID比は2.05となり、本願発明のIG/ID比が5.0以上という条件を満たしていなかった。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は35000個と非常に多かった。
原料粉末として平均粒径3μmのFe粉末、平均粒径3μmのPt粉末、平均粒子径20μmのC粉末を用意し、組成が30Fe-30Pt-40C(mol%)となるように秤量した。C粉末には平均粒子径20μmのグラファイトを使用した。
次に、攪拌ミルから取り出した混合粉末をカーボン製の型に充填しホットプレスした。ホットプレスの条件は、真空雰囲気、昇温速度300°C/時間、保持温度1400°C、保持時間2時間とし、昇温開始時から保持終了まで30MPaで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
また、測定結果のカーブフィッティングにはローレンツ関数を使用した。Fe-Pt-Cのラマン散乱分光測定結果とカーブフィッティング結果を図14に示す。IG/ID比は1.70となり、本願発明のIG/ID比が5.0以上という条件を満たしていなかった。
スパッタリングの条件は、投入電力1kW、Arガス圧1.7Paとし、2kWhrのプレスパッタリングを実施した後、4インチ径のシリコン基板上に20秒間成膜した。そして基板上へ付着した粒径0.25~3μmのパーティクルの個数を表面異物検査装置(Surfscan6420、KLA-Tencor社製)で測定した結果、表1に示すように、このときのパーティクル個数は90000個と非常に多かった。
Claims (6)
- Cを含有する磁気記録膜用スパッタリングターゲットであって、ラマン散乱分光測定におけるGバンドとDバンドのピーク強度比(IG/ID)が5.0以上であることを特徴とする磁気記録膜用スパッタリングターゲット。
- Ptが5mol%以上60mol%以下、残余がFeである組成の金属とCからなる請求項1記載の磁気記録膜用スパッタリングターゲット。
- Cの含有割合が10mol%以上70mol%以下であることを特徴とする請求項1又は2記載の磁気記録膜用スパッタリングターゲット。
- 相対密度が90%以上であることを特徴とする請求項1~3のいずれか一項に記載の磁気記録膜用スパッタリングターゲット。
- 添加元素として、B、Ru、Ag、Au、Cuから選択した1元素以上を、0.5mol%以上20mol%以下含有することを特徴とする請求項1~4のいずれか一項に記載の磁気記録膜用スパッタリングターゲット。
- 添加剤として、SiO2、Cr2O3、CoO、Ta2O5、B2O3、MgO、Co3O4から選択した1種以上の酸化物を、0.5mol%以上20mol%以下を含有することを特徴とする請求項1~5のいずれか一項に記載の磁気記録膜用スパッタリングターゲット。
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| JPWO2019220675A1 (ja) * | 2018-05-14 | 2021-07-15 | Jx金属株式会社 | スパッタリングターゲット及びスパッタリングターゲットの製造方法 |
| JP7242652B2 (ja) | 2018-05-14 | 2023-03-20 | Jx金属株式会社 | スパッタリングターゲット及びスパッタリングターゲットの製造方法 |
| JPWO2023079857A1 (ja) * | 2021-11-05 | 2023-05-11 | ||
| 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 |
| JP7657960B2 (ja) | 2021-11-05 | 2025-04-07 | 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| US20140346039A1 (en) | 2014-11-27 |
| JPWO2013190943A1 (ja) | 2016-05-26 |
| SG11201404067PA (en) | 2014-10-30 |
| MY167825A (en) | 2018-09-26 |
| TW201413019A (zh) | 2014-04-01 |
| JP5592022B2 (ja) | 2014-09-17 |
| CN104145306B (zh) | 2017-09-26 |
| TWI564416B (zh) | 2017-01-01 |
| US9540724B2 (en) | 2017-01-10 |
| CN104145306A (zh) | 2014-11-12 |
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