WO2014132746A1 - FePt-C系スパッタリングターゲット及びその製造方法 - Google Patents
FePt-C系スパッタリングターゲット及びその製造方法 Download PDFInfo
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- WO2014132746A1 WO2014132746A1 PCT/JP2014/052341 JP2014052341W WO2014132746A1 WO 2014132746 A1 WO2014132746 A1 WO 2014132746A1 JP 2014052341 W JP2014052341 W JP 2014052341W WO 2014132746 A1 WO2014132746 A1 WO 2014132746A1
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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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
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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
- C23C14/22—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
- G11B5/84—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 FePt—C-based sputtering target and a method for producing the same.
- FePt alloys can be equipped with an fct (Ordered Face Centered Tetragonal) structure with high crystal magnetic anisotropy by heat treatment at a high temperature (for example, 600 ° C or higher), and thus attract attention as a magnetic recording medium.
- a high temperature for example, 600 ° C or higher
- FePt particles small and uniform in the FePt alloy thin film it has been proposed to include a predetermined amount of carbon (C) in the FePt thin film (for example, Patent Document 1).
- Patent Document 1 uses Fe, Pt, and C on a MgO (100) substrate by using a 2-inch diameter Fe target and a C target and a Pt target having a length and width of 5 mm. It is the method of vapor deposition simultaneously. In this method, it is difficult to strictly control the composition of the obtained film. In addition, since three targets are required and a cathode, a power source, and the like are required for each target, it takes time to prepare for sputtering, and the cost of the apparatus increases.
- Patent Document 2 discloses an FePt—C-based sputtering target that can form an FePtC-based thin film independently without using a plurality of targets, and a manufacturing method thereof.
- An FePt—C-based sputtering target capable of forming an FePtC-based thin film with a high carbon content independently without using a plurality of targets and a method for producing the same are disclosed.
- Patent Document 4 includes SiO 2 instead of carbon (C), and has a general formula: (Fe x Pt (100 ⁇ x) ) (100 ⁇ y) (SiO 2 ) y , where 40 ⁇ x ⁇ 60 (Unit: mol%)
- a sputtering target for forming a magnetic recording medium film is disclosed.
- the sputtering target is generally required to reduce the number of particles generated during sputtering, and this is also required for a sputtering target that is considered to be capable of forming a thin film containing an FePt alloy alone. ing.
- the present invention has been made in view of such a point, and can form a thin film containing an FePt-based alloy that can be used as a magnetic recording medium without using a plurality of targets, and at the time of sputtering. It is an object of the present invention to provide an FePt—C-based sputtering target that generates less particles and a manufacturing method thereof.
- the present inventor has found that the above problems can be solved by the following FePt—C-based sputtering target and a method for producing the same, and has led to the present invention.
- the first aspect of the FePt—C-based sputtering target according to the present invention is an FePt—C-based sputtering target containing Fe, Pt, and C, containing Pt in a range of 33 at% to 60 at%, with the balance remaining.
- FePt alloy when it is described as an FePt alloy, it means an alloy containing Fe and Pt as main components, and not only a binary alloy containing only Fe and Pt but also Fe and Pt as main components.
- An alloy of a ternary system or higher including metal elements other than Fe and Pt is also meant.
- FePt—C-based sputtering target means a sputtering target containing Fe, Pt, and C as main components, and includes a sputtering target further containing elements other than the main components Fe, Pt, and C.
- FePtC-based thin film means a thin film containing Fe, Pt, and C as main components, and includes a thin film that further includes elements other than the main components Fe, Pt, and C.
- FePtC-based layer means a layer containing Fe, Pt, and C as main components, and includes a layer further containing elements other than Fe, Pt, and C as main components.
- a second aspect of the FePt—C based sputtering target according to the present invention is an FePt—C based sputtering target containing Fe, Pt and C, and further containing one or more metal elements other than Fe and Pt.
- Pt is contained at 33 at% or more and less than 60 at%
- the one or more metal elements other than Fe and Pt are contained in an amount of more than 0 at% and 20 at% or less
- the total of Pt and the one or more metal elements is 60 at%.
- FePt- characterized in that the FePt-based alloy phase is dispersed in a FePt-based alloy phase consisting of Fe and inevitable impurities so that Cs of primary particles containing inevitable impurities are not in contact with each other.
- C-based sputtering target characterized in that the FePt-based alloy phase is dispersed in a FePt-based alloy phase consisting of Fe and inevitable impurities so that Cs of primary particles containing inevitable impurities are
- the one or more metal elements other than Fe and Pt are Cu, Ag, Mn, Ni, Co, Pd, Cr, V, and B. Or more.
- the average particle diameter of the primary particles is preferably 1 ⁇ m or more and 30 ⁇ m or less.
- the crystal structure of C is preferably an amorphous structure or a diamond structure from the viewpoint of reducing particles generated during sputtering.
- the volume fraction with respect to the whole target of C is 5 vol% or more and 60 vol% or less, and among the total surface areas of C, the surface area covered with the FePt alloy phase is 80% of the total surface area of C. % Or more is preferable.
- an oxide phase may be further dispersed in the FePt-based alloy phase.
- the volume fraction of the C target relative to the entire target is 5 vol% or more and less than 60 vol%, and the entire target of the oxide phase It is preferable that the volume fraction with respect to the total target of the total of C and the oxide phase is not less than 8 vol% and not more than 60 vol%.
- the oxide phase SiO 2, TiO 2, Ti 2 O 3, Ta 2 O 5, Cr 2 O 3, CoO, Co 3 O 4, B 2 O 3, Fe 2 O 3, CuO, Cu 2 O, Of Y 2 O 3 , MgO, Al 2 O 3 , ZrO 2 , Nb 2 O 5 , MoO 3 , CeO 2 , Sm 2 O 3 , Gd 2 O 3 , WO 2 , WO 3 , HfO 2 , NiO 2 You may comprise so that at least 1 sort (s) may be included.
- the C may be, for example, a substantially spherical shape having a value obtained by dividing the major axis by the minor axis of 2 or less.
- the relative density is preferably 90% or more.
- the first aspect of the method for producing an FePt—C-based sputtering target according to the present invention is a FePt-based alloy powder containing Pt in an amount of 33 at% to 60 at% and the balance being Fe and inevitable impurities and having an average particle size of 20 ⁇ m or less.
- C powder which is composed of primary particles containing inevitable impurities and which does not constitute secondary particles is added and mixed within a range in which the primary particle diameter of the C powder is not substantially reduced.
- This is a method for producing an FePt—C sputtering target, characterized in that after the mixed powder for bonding is manufactured, the formed mixed powder for pressure sintering is heated and molded under pressure.
- mixing within a range where the primary particle diameter of the C powder is not substantially reduced means that the primary particle diameter of the C powder is reduced by mixing, and as a result, the number of particles generated does not increase. This is mixing within the range, and is a concept including mixing in which the primary particle diameter of the C powder is reduced to some extent if the number of generated particles does not increase.
- the second aspect of the method for producing an FePt—C-based sputtering target according to the present invention includes a Pt powder containing unavoidable impurities and an average particle size of 20 ⁇ m or less, and an Fe powder containing unavoidable impurities and an average particle size of 20 ⁇ m or less.
- the Pt powder is weighed so that the content ratio of Pt with respect to the total of Pt and Fe is not less than 33 at% and not more than 60 at%, and consists of the weighed Pt powder, the weighed Fe powder, and primary particles containing inevitable impurities.
- Pt powder may be referred to as Pt simple substance powder
- Fe powder may be referred to as Fe simple substance powder
- Pt is contained at 33 at% or more and less than 60 at%, and at least one metal element other than Fe and Pt is contained at 0 to 20 at%.
- the FePt alloy powder having an average particle diameter of 20 ⁇ m or less, in which the total of Pt and the one or more metal elements is 60 at% or less, and the balance is Fe and inevitable impurities includes primary particles containing inevitable impurities.
- the fourth aspect of the method for producing an FePt—C-based sputtering target according to the present invention includes an FePt-based alloy powder having an average particle size of 20 ⁇ m or less composed of Pt, Fe and unavoidable impurities, including unavoidable impurities and other than Fe and Pt.
- Secondary particles comprising the weighed FePt alloy powder, the weighed metal powder comprising one or more metal elements, and primary particles containing inevitable impurities.
- C powder that does not constitute a child is mixed within a range in which the primary particle diameter of the C powder is not substantially reduced to produce a mixed powder for pressure sintering, and then the pressure sintering produced
- the fifth aspect of the method for producing an FePt—C-based sputtering target according to the present invention includes a Pt powder containing inevitable impurities and an average particle size of 20 ⁇ m or less, and an Fe powder containing inevitable impurities and an average particle size of 20 ⁇ m or less.
- the ratio is 33 at% or more and less than 60 at%, the ratio of the one or more metal elements to the total is more than 0 at% and 20 at% or less, and the total ratio of Pt and the one or more metal elements to the total is
- the Pt powder weighed so as to be 60 at% or less, the weighed Fe powder, the weighed metal powder composed of one or more metal elements, and unavoidable C powder composed of primary particles containing impurities and not constituting secondary particles was mixed within a range where the primary particle diameter of the C powder was not substantially reduced to produce a mixed powder for pressure sintering. Then, the produced mixed powder for pressure sintering is heated and molded under pressure, and is a method for producing an FePt—C-based sputtering target.
- the volume fraction of the C powder with respect to the entire mixed powder for pressure sintering is 5 vol% or more and 60 vol% or less. Is preferred.
- an unavoidable impurity is added to an FePt-based alloy powder containing Pt in an amount of 33 at% to 60 at% and the balance being Fe and inevitable impurities.
- a first mixed powder is prepared by adding an oxide powder containing and mixing to such an extent that mechanical alloy is generated, and the first mixed powder is composed of primary particles containing inevitable impurities and constitutes secondary particles.
- C powder that has not been added is added and mixed within a range where the primary particle size of the C powder is not substantially reduced to produce a mixed powder for pressure sintering.
- a Pt powder containing inevitable impurities and an Fe powder containing inevitable impurities have a Pt content ratio of 33 at to the total of Pt and Fe.
- the Pt powder weighed, the weighed Pt powder, the weighed Fe powder, and the oxide powder containing unavoidable impurities are mixed and mixed to the extent that mechanical alloying occurs.
- a powder is prepared, and C powder which is composed of primary particles containing inevitable impurities and does not constitute secondary particles is added to the prepared first mixed powder, so that the primary particle diameter of the C powder is substantially FePt-C, wherein the mixture is mixed within a range that does not become smaller and a pressure-sintered mixed powder is prepared, and then the pressure-sintered mixed powder is heated and molded under pressure. It is a method of manufacturing a sputtering target.
- the eighth aspect of the method for producing a FePt—C-based sputtering target according to the present invention comprises Pt in a range of 33 at% to less than 60 at% and one or more metal elements other than Fe and Pt in an amount of more than 0 at% and not more than 20 at%.
- an oxide powder containing inevitable impurities is added to FePt alloy powder in which the total of Pt and the one or more metal elements is 60 at% or less and the balance is Fe and inevitable impurities.
- a first mixed powder is prepared by mixing to the extent that an alloy is generated, and C powder which is composed of primary particles containing inevitable impurities and does not constitute secondary particles is added to the first mixed powder thus prepared.
- Molding It is FePt-C based sputtering target manufacturing method according to claim.
- the ninth aspect of the method for producing an FePt—C-based sputtering target according to the present invention includes an FePt-based alloy powder comprising Pt, Fe and unavoidable impurities, and one or more metals other than Fe and Pt containing unavoidable impurities.
- the ratio of the Pt to the total of the Pt, the Fe, and the one or more metal elements is 33 at% or more and less than 60 at%, and the ratio of the one or more metal elements to the total is More than 0 at% and not more than 20 at%, and the total ratio of the Pt and the one or more metal elements to the total is 60 at% or less, and the weighed FePt alloy powder, the weighed 1 Mix metal powder consisting of more than one kind of metal element and oxide powder containing inevitable impurities, and mix to the extent that mechanical alloying occurs.
- a tenth aspect of the method for producing an FePt—C-based sputtering target according to the present invention includes a Pt powder containing inevitable impurities, an Fe powder containing inevitable impurities, an inevitable impurity containing Fe, and one or more kinds other than Pt.
- the ratio of the Pt to the total of the Pt, the Fe, and the one or more metal elements is 33 at% or more and less than 60 at%, and the ratio of the one or more metal elements to the total Is more than 0 at% and not more than 20 at%, and the total ratio of the Pt and the one or more metal elements to the total is 60 at% or less, the weighed Pt powder, the weighed Fe powder
- the weighed metal powder composed of one or more kinds of metal elements and the oxide powder containing inevitable impurities, and mechanical alloy is produced.
- C powder which is composed of primary particles containing inevitable impurities and does not constitute secondary particles is added to the first mixed powder.
- the primary particle diameter of the mixture is mixed within a range where the primary particle diameter is not substantially reduced, and a mixed powder for pressure sintering is prepared, and then the formed powder for pressure sintering is heated and molded under pressure. This is a feature of producing a FePt—C based sputtering target.
- the volume fraction of the C powder with respect to the entire mixed powder for pressure sintering is 5 vol% or more and less than 60 vol%
- the volume fraction of the oxide powder with respect to the whole powder mixture for pressure sintering is 3 vol% or more and less than 55 vol%
- the total powder mixture for pressure sintering of the C powder and the oxide powder It is preferable that the volume fraction with respect to the whole is 8 vol% or more and 60 vol% or less.
- the one or more metal elements other than Fe and Pt are Cu. , Ag, Mn, Ni, Co, Pd, Cr, V, and B.
- the oxide powder may be SiO 2 , TiO 2 , Ti 2 O 3 , Ta 2 O 5 , Cr 2 O. 3 , CoO, Co 3 O 4 , B 2 O 3 , Fe 2 O 3 , CuO, Cu 2 O, Y 2 O 3 , MgO, Al 2 O 3 , ZrO 2 , Nb 2 O 5 , MoO 3 , CeO 2 , Sm 2 O 3 , Gd 2 O 3 , WO 2 , WO 3 , HfO 2 , NiO 2 may be included.
- the average particle diameter of the primary particles of the C powder is preferably 1 ⁇ m or more and 30 ⁇ m or less.
- the crystal structure of the C powder is preferably an amorphous structure or a diamond structure.
- primary particles C (carbon) are dispersed in the FePt-based alloy phase so as not to contact each other, and the periphery of the primary particles C (carbon) is FePt. Since it is easy to be covered with an alloy, C (carbon) is prevented from falling out of the target in a lump state to form particles during sputtering, and good sputtering with less generation of particles is realized. Can do.
- the manufacturing method according to the present invention uses a sintering method instead of a casting method, the C content relative to the entire target can be increased, and the volume fraction of C relative to the entire target is 5 vol% or more and 60 vol%.
- the following FePt—C-based sputtering target can be produced. For this reason, by performing sputtering using the FePt—C-based sputtering target produced by the production method according to the present invention, it is possible to use the target alone, that is, without using a plurality of targets, as a magnetic recording medium. In addition, a thin film containing an FePt alloy can be formed.
- Metal micrograph of the structure of the sintered body in Example 1 (photo magnification at the time of photographing is 1000 times, scale scale in the photograph is 50 ⁇ m)
- the graph figure which shows the relationship between sputtering accumulation continuation time and the number of generated particles in the sputtering target of Examples 1 to 3, Comparative Example 1, and Reference Example 1 The graph which shows the relationship between sputtering accumulation continuation time and the number of generated particles in the sputtering target of Examples 1 to 3 and Reference Example 1
- Metal micrograph of the structure of the sintered body in Example 2 (photo magnification at the time of photographing is 1000 times, scale scale in the photograph is 50 ⁇ m)
- Metallic micrograph of the structure of the sintered body in Example 3 (photo magnification at the time of photographing is 1000 times, scale scale in the photograph is 50 ⁇ m)
- Metallic micrograph of the structure of the sintered body in Comparative Example 1 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m)
- Metal micrograph of the structure of the sintered body in Comparative Example 2 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m)
- Metal micrograph of the structure of the sintered body in Comparative Example 3 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m)
- Metal micrograph of the structure of the sintered body in Reference Example 2 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m)
- the FePt—C based sputtering target according to the first embodiment of the present invention is an FePt—C based sputtering target containing Fe, Pt and C, and Pt is 33 at% or more and 60 at% or less. It is characterized by having a structure in which the primary particles C containing inevitable impurities are dispersed so as not to contact each other in the FePt-based alloy phase containing Fe and the inevitable impurities.
- “ ⁇ to ⁇ ” may be expressed as “ ⁇ to ⁇ ” when the numerical range is expressed.
- FePt-based alloys FePt-based alloys can be provided with an fct structure having high crystal magnetic anisotropy by heat treatment at a high temperature (for example, 600 ° C. or higher), and thus serve as a recording layer of a magnetic recording medium. And is a main component in the FePt—C-based sputtering target according to the embodiment of the present invention.
- the Pt content in the FePt-based alloy phase is defined as 33 to 60 at% is that if the Pt content in the FePt-based alloy phase is out of 33 to 60 at%, the fct (rectangular face) structure may not be developed. Because there is. From the viewpoint of ensuring that an fct (face-centered rectangular parallelepiped) structure appears in the FePt-based alloy phase, the Pt content in the FePt-based alloy phase is preferably 45 to 55 at%, and 49 to 51 at%. Is more preferable, and 50 at% is particularly preferable.
- C (carbon) C (carbon) serves as a partition wall for partitioning the FePt-based alloy particles, which are magnetic particles, in the FePtC-based layer obtained by sputtering, and serves to make the FePt-based alloy particles small and uniform in the FePtC-based layer. And is one of the main components in the FePt—C-based sputtering target according to the first embodiment.
- the volume fraction of C (carbon) with respect to the entire target is preferably 5 to 60 vol%, and the volume fraction of C (carbon) with respect to the entire target is set to 5 to 60 vol%, whereby an FePtC-based layer obtained by sputtering.
- C (carbon) serves as a partition wall for partitioning the FePt-based alloy particles, which are magnetic particles, and it is possible to increase the certainty of expressing the effect of making the FePt-based alloy particles small and uniform. If the volume fraction of C (carbon) is less than 5 vol%, this effect may not be sufficiently exhibited.
- the volume fraction of C (carbon) exceeds 60 vol%, in the FePtC-based layer obtained by sputtering, the number of FePt-based alloy particles per unit volume in the FePtC-based layer decreases, and in terms of storage capacity. Disadvantageous. From the viewpoint of increasing the certainty of expressing the effect of making the FePt-based alloy particles small and uniform in the FePtC-based layer and from the viewpoint of the storage capacity of the FePtC-based layer to be formed, the volume fraction of C (carbon) relative to the entire target is 10 to More preferably, it is 50 vol%, more preferably 20 to 40 vol%, and particularly preferably 25 to 35 vol%.
- the structure of the FePt—C-based sputtering target according to the first embodiment of the present invention is unavoidable in the FePt-based alloy phase containing 33 to 60 at% of Pt and the balance being Fe and inevitable impurities.
- the primary particle C (carbon) containing impurities is dispersed so as not to contact each other, and the primary particle C (carbon) does not constitute a secondary particle.
- the FePt-C sputtering target according to the first embodiment has a structure in which C (carbon) of primary particles that do not constitute secondary particles are dispersed so as not to contact each other in the FePt alloy phase.
- C (carbon) which is the primary particle
- C (carbon) in the target constitutes secondary particles
- the periphery of the primary particles C existing inside the secondary particles is not easily covered with the FePt-based alloy phase.
- C in the primary particles present in the film may fall out of the target during sputtering and become particles.
- the average particle size of C (carbon) of the primary particles is reduced, the average particle size of the FePt alloy powder (or Fe powder and Pt powder) in the mixed powder for pressure sintering is also reduced to the same level or more. Otherwise, the portion of the surface of C (carbon) that is the primary particle in the obtained target is not covered with the FePt-based alloy, and there is a risk of falling out of the target as a lump during sputtering. There is a risk that the number of Therefore, the average particle diameter of C (carbon) in the primary particles is preferably larger than a predetermined size. On the other hand, if the average particle size of C (carbon) in the primary particles becomes too large, the sputtering rate during sputtering greatly varies depending on the location, which is not preferable.
- the average particle diameter of C (carbon) of the primary particle is preferably 1 to 30 ⁇ m, and preferably 3 to 115 ⁇ m. It is more preferable that the thickness is 5 to 10 ⁇ m.
- the average particle diameter is a particle diameter at which a frequency cumulative curve of particle size distribution measured by a laser diffraction method becomes 50%, and is a median diameter.
- the total surface area of the portions covered with the FePt-based alloy is 80% of the total surface area of C (carbon) in the target from the viewpoint of suppressing particles generated during sputtering. % Or more is preferable, 90% or more is more preferable, and 95% or more is particularly preferable.
- the shape of C (carbon) which is a primary particle is not particularly limited, and may be, for example, a substantially spherical shape in which a value obtained by dividing a major axis by a minor axis is 2 or less. With such a shape, the surface area of C can be reduced, and the effect of easily increasing the ratio of the surface area of the C portion covered with the FePt-based alloy (relative to the total surface area of C) can be obtained. In addition, C (carbon) having a large average particle size of primary particles is easily available.
- the crystal structure of C (carbon) as the primary particle is preferably an amorphous structure or a diamond structure. This is because, in an amorphous structure or a diamond structure, since the bonding force between C atoms in the crystal is strong, there is little possibility that primary particles of C (carbon) will collapse during sputtering. If primary particles of C (carbon) are destroyed during sputtering, particles may be generated.
- the relative density of the target the larger the value, the smaller the voids in the target, which is preferable for good sputtering.
- the relative density of the target is preferably 90% or more, and more preferably 95% or more.
- the FePt—C-based sputtering target according to the first embodiment includes only Fe and Pt as metal elements, but includes a metal element other than Fe and Pt in the FePt-based alloy phase. It is also possible (a modification of the first embodiment).
- the FePt-based alloy phase has a Pt content of 33 at% or more and less than 60 at%, and the one type other than Fe and Pt FePt alloy phase containing more than 0 at% and not more than 20 at% of the above metal element, and the total of Pt and the one or more metal elements is not more than 60 at%, with the balance being Fe and inevitable impurities do it.
- the Pt content in the FePt-based alloy phase is 45 to It is preferably 55 at%, more preferably 49 to 51 at%.
- the total content of Fe and Pt is less than 100 at%
- the total content of the one or more metal elements other than Fe and Pt is more than 0 at% and not more than 20 at%
- Fe It is assumed that the total of the one or more metal elements other than Pt and the total of Pt is 60 at% or less.
- metal elements other than Fe and Pt that can be included in the FePt-based alloy phase include Cu, Ag, Mn, Ni, Co, Pd, Cr, V, and B. One or more of them may be included.
- the heat treatment temperature for example, 600 ° C.
- the heat treatment cost for the FePtC layer obtained by sputtering is reduced.
- the crystal structure of the obtained FePtC-based layer can be converted into an fct structure by heat generated during sputtering without a separate heat treatment.
- the FePt—C-based sputtering target according to the first embodiment is a FePt-based alloy powder containing Pt in an amount of 33 at% to 60 at% and the balance being Fe and inevitable impurities and having an average particle size of 20 ⁇ m or less.
- the mixed powder for pressure sintering is prepared by mixing within the range in which the number of particles generated during the process does not increase), and then the pressure-sintered mixed powder is heated and molded under pressure. Can be manufactured.
- the FePt-based alloy powder may not sufficiently cover the periphery of the primary particles of the C powder, and when performing sputtering using the resulting sputtering target, There is a possibility that the number of generated particles increases.
- the atmosphere at which the FePt alloy powder and the C powder are mixed to produce the mixed powder for pressure sintering is not particularly limited, and may be mixed in the air.
- the FePt-based alloy powder instead of the FePt-based alloy powder, a single Fe powder having an average particle size of 20 ⁇ m or less and a single Pt powder having an average particle size of 20 ⁇ m or less may be used.
- the Fe simple substance powder and the Pt simple substance powder are weighed so that the ratio of Pt to the total of Fe and Pt is 33 at% or more and 60 at% or less.
- the weighed Fe powder, the weighed Pt powder, and the C powder which is composed of primary particles containing inevitable impurities and does not constitute secondary particles the primary particle diameter of the C powder is substantially small. After mixing within the range which does not become and producing the mixed powder for pressure sintering, this produced mixed powder for pressure sintering is heated and shape
- Fe simple powder has high activity and may ignite in the atmosphere, it is necessary to be careful when handling it.
- FePt alloy powder By forming FePt alloy powder by alloying Fe with Pt, the activity can be lowered even in a powder state, and in this respect, it is preferable to use FePt alloy powder.
- the method for heating and molding the mixed powder for pressure sintering produced as described above is not particularly limited, and examples thereof include a hot press method, a hot isostatic press method (HIP method), and discharge plasma.
- a sintering method (SPS method) or the like can be used.
- These molding methods are preferably carried out in a vacuum or in an inert atmosphere when carrying out the present invention. Thereby, even if oxygen is contained in the mixed powder for pressure sintering to some extent, the amount of oxygen in the obtained sintered body is reduced.
- an FePt alloy powder having an average particle diameter of 20 ⁇ m or less made of Pt, Fe and unavoidable impurities, and a metal powder having an average particle diameter of 20 ⁇ m or less containing unavoidable impurities and one or more metal elements other than Fe and Pt may be used.
- an FePt alloy powder having an average particle size of 20 ⁇ m or less made of Pt, Fe and unavoidable impurities, and a metal powder having an average particle size of 20 ⁇ m or less containing unavoidable impurities and one or more metal elements other than Fe and Pt The ratio of the Pt to the total of the Pt, the Fe, and the one or more metal elements is 33 at% or more and less than 60 at%, and the ratio of the one or more metal elements to the total is more than 0 at% It is weighed so that the total ratio of the Pt and the one or more metal elements with respect to the total is 20 at% or less and 60 at% or less.
- the weighed FePt-based alloy powder, the weighed metal powder composed of one or more kinds of metal elements, and the C powder composed of primary particles containing inevitable impurities and not constituting secondary particles After mixing within a range in which the primary particle diameter is not substantially reduced to produce a powder mixture for pressure sintering, the produced powder mixture for pressure sintering is heated and molded under pressure.
- Pt single powder having an average particle size of 20 ⁇ m or less containing unavoidable impurities Fe single powder having an average particle size of 20 ⁇ m or less containing unavoidable impurities, and one or more metal elements other than Fe and Pt containing unavoidable impurities
- a metal powder having an average particle diameter of 20 ⁇ m or less may be used.
- a Pt simple substance powder having an average particle diameter of 20 ⁇ m or less, an Fe simple substance powder having an average particle diameter of 20 ⁇ m or less, and a metal powder having an average particle diameter of 20 ⁇ m or less composed of one or more metal elements other than Fe and Pt The ratio of Pt to the total of the Fe and the one or more metal elements is 33 at% or more and less than 60 at%, the ratio of the one or more metal elements to the total is more than 0 at% and 20 at% or less, Weigh so that the total ratio of Pt and the one or more metal elements to the total is 60 at% or less.
- the weighed Pt simple powder, the weighed Fe simple powder, the weighed metal powder composed of one or more kinds of metal elements, and primary particles containing inevitable impurities do not constitute secondary particles.
- the powder is mixed within a range where the primary particle diameter of the C powder is not substantially reduced to produce a mixed powder for pressure sintering, and then the pressure-sintered mixed powder thus prepared is heated under pressure. And then molded.
- the primary particles C (carbon) that do not constitute the secondary particles are dispersed in the FePt-based alloy phase to form primary particles. Since the periphery of C (carbon) is easily covered with the FePt-based alloy, it is prevented that C (carbon) falls off from the target in the state of a lump and becomes particles during sputtering. Less favorable sputtering can be realized.
- the manufacturing method of the first embodiment uses a sintering method instead of a casting method, the C content with respect to the entire target can be increased, and the volume fraction of C with respect to the entire target is 5 vol% or more.
- An FePt—C-based sputtering target with a volume of 60 vol% or less can be produced. Therefore, by performing sputtering using the FePt—C-based sputtering target according to the first embodiment, the target can be used as a magnetic recording medium alone, that is, without using a plurality of targets. A thin film containing an FePt-based alloy can be formed.
- Second Embodiment 2-1 Components and Structure of Sputtering Target
- the FePt—C-based sputtering target according to the first embodiment contains Fe and Pt as alloy components, and contains C (carbon) in addition to the alloy components (Fe, Pt).
- the FePt—C-based sputtering target according to the second embodiment of the present invention contains Fe and Pt as alloy components, and contains an oxide in addition to C (carbon) in addition to the alloy components (Fe, Pt). This point is different from the FePt—C-based sputtering target according to the first embodiment.
- the FePt—C-based sputtering target according to the second embodiment of the present invention contains unavoidable impurities in the FePt-based alloy phase containing Pt in a range of 33 at% to 60 at% and the balance being Fe and inevitable impurities. It has a structure in which C of primary particles contained and a metal oxide containing inevitable impurities are dispersed, and C of the primary particles is not in contact with each other.
- C and Metal Oxide C and metal oxide may be referred to as an FePt-based alloy obtained by sputtering and a layer containing C and metal oxide (hereinafter referred to as FePt—C—metal oxide layer). ) In the FePt-C-metal oxide layer, and has a role of making the FePt-based alloy particles small and uniform in the FePt-C-metal oxide layer.
- the main component in a -C sputtering target The main component in a -C sputtering target.
- an FePt alloy powder (or FePt alloy powder (or Fe powder and Pt powder) and a metal oxide powder are sufficiently mixed to obtain an FePt alloy powder (or , Fe powder and Pt powder) can be prepared to reduce the average particle size. Since the average particle diameter of the FePt-based alloy powder (or Fe powder and Pt powder) in the first mixed powder can be sufficiently reduced by sufficiently mixing, such first mixed powder And C powder composed of primary particles C are mixed within a range where the primary particle diameter of C powder is not substantially reduced to obtain a mixed powder for pressure sintering, the diameter is substantially reduced. The surrounding of the primary particles C, which are not present, is easily covered densely with FePt alloy powder (or Fe powder and Pt powder). A target in which the periphery of particle C is sufficiently covered with an FePt-based alloy phase can be produced.
- the volume fraction of C with respect to the entire target is 5 vol% or more and less than 60 vol%
- the volume fraction of the metal oxide with respect to the entire target is 3 vol% or more and less than 55 vol%
- C and metal The volume fraction of the total target with oxide is 8 vol% or more and 60 vol% or less.
- the reason why the volume fraction of C with respect to the entire target is 5 vol% or more and less than 60 vol% is that the partition walls partition FePt-based alloy particles in which C is magnetic particles in the FePt—C—metal oxide layer obtained by sputtering. This is because the effect of making the FePt-based alloy particles small and uniform is exhibited.
- the reason why the volume fraction of the metal oxide target with respect to the entire target is 3 vol% or more and less than 55 vol% is that the average particle size of the FePt alloy powder is obtained by sufficiently mixing the FePt alloy powder and the metal oxide powder first. This is because the first mixed powder having a reduced diameter can be produced.
- the metal oxide e.g., SiO 2, TiO 2, Ti 2 O 3, Ta 2 O 5, Cr 2 O 3, CoO, Co 3 O 4, B 2 O 3, Fe 2 O 3 , CuO, Cu 2 O, Y 2 O 3 , MgO, Al 2 O 3 , ZrO 2 , Nb 2 O 5 , MoO 3 , CeO 2 , Sm 2 O 3 , Gd 2 O 3 , WO 2 , WO 3
- a metal oxide containing at least one of HfO 2 and NiO 2 can be used.
- the structure of the FePt—C-based sputtering target according to the second embodiment of the present invention is inevitable in the FePt-based alloy phase containing 33 to 60 at% of Pt and the balance being Fe and inevitable impurities.
- the FePt-C sputtering target according to the second embodiment has a structure in which C (carbon) of primary particles that do not constitute secondary particles are dispersed so as not to contact each other in the FePt alloy phase.
- C (carbon) which is the primary particle
- C (carbon) in the target constitutes secondary particles
- the periphery of the primary particles C existing inside the secondary particles is not easily covered with the FePt-based alloy phase.
- C in the primary particles present in the film may fall out of the target during sputtering and become particles.
- the average particle size of C (carbon) of the primary particles is small, the average particle size of the FePt-based alloy powder in the pressure-sintering mixed powder is not less than the same level, and 1 in the obtained target. Because the portion of the surface of C (carbon), which is the next particle, is not covered with the FePt-based alloy, there is a risk of falling off from the target as a lump during sputtering, and the number of particles generated during sputtering may increase.
- the average particle size of C (carbon) in the primary particles is preferably larger than a predetermined size. On the other hand, if the average particle size of C (carbon) in the primary particles becomes too large, the sputtering rate during sputtering greatly varies depending on the location, which is not preferable.
- the average particle diameter of C (carbon) of the primary particle is preferably 1 to 30 ⁇ m, and preferably 3 to 115 ⁇ m. It is more preferable that the thickness is 5 to 10 ⁇ m.
- the total surface area of the portions covered with the FePt-based alloy is 80% of the total surface area of C (carbon) in the target from the viewpoint of suppressing particles generated during sputtering. % Or more is preferable, 90% or more is more preferable, and 95% or more is particularly preferable.
- the shape of C (carbon) which is a primary particle is not particularly limited, and may be, for example, a substantially spherical shape in which a value obtained by dividing a major axis by a minor axis is 2 or less.
- the crystal structure of C (carbon) as the primary particle is preferably an amorphous structure or a diamond structure.
- the relative density of the target the larger the value, the smaller the voids in the target, which is preferable for good sputtering.
- the relative density of the target is preferably 90% or more, and more preferably 95% or more.
- the FePt—C-based sputtering target according to the second embodiment contains only Fe and Pt as metal elements, but as with the FePt—C-based sputtering target according to the first embodiment, Metal elements other than Fe and Pt may be included in the FePt-based alloy phase (modified example of the second embodiment).
- the metal elements other than Fe and Pt that may be included in the FePt-based alloy phase are described in “1-1-4. Metal elements other than Fe and Pt” in the first embodiment. The description is omitted because it is the same as the contents described in FIG.
- FePt-based alloy powder containing 33 to 60 at% of Pt and the balance being Fe and inevitable impurities and metal oxidation are used.
- the first mixed powder in which the average particle size of the FePt-based alloy powder is sufficiently small is produced by sufficiently mixing the product powder (mixing to the extent that mechanical alloy is generated).
- the average particle size is often 30 ⁇ m or more. Even with such a large average particle size, the FePt-based alloy powder is sufficiently mixed with the metal oxide powder.
- the average particle size can be made sufficiently small by mixing (to the extent that mechanical alloy is generated).
- the first mixed powder and C powder composed of C of the primary particles are mixed for pressure sintering.
- the periphery of primary particle C is easily covered with FePt-based alloy powder, and by pressing and sintering the obtained powder for pressure sintering, the periphery of C of primary particle It is possible to produce a target that is sufficiently covered with an FePt-based alloy phase.
- C powder composed of C as primary particles that do not constitute secondary particles is added to the first mixed powder, and the particle size of C particles as primary particles is not substantially reduced.
- the mixed powder for pressure sintering was prepared after mixing in the range where the number of particles generated when sputtering was performed using the obtained target was mixed to prepare the mixed powder for pressure sintering.
- the FePt—C-based sputtering target according to the second embodiment can be manufactured.
- the atmosphere at the time of doing is not specifically limited, You may mix in air
- the FePt-based alloy powder instead of the FePt-based alloy powder, an Fe simple substance powder and a Pt simple substance powder may be used.
- the first mixed powder is prepared by sufficiently mixing the Fe simple substance powder, the Pt simple substance powder, and the metal oxide powder to sufficiently reduce the average particle size of the Fe simple substance powder and the Pt simple substance powder.
- the subsequent steps are the same as in the case of using FePt alloy powder.
- Fe simple powder has high activity and may ignite in the atmosphere, it is necessary to be careful when handling it.
- FePt alloy powder By forming FePt alloy powder by alloying Fe with Pt, the activity can be lowered even in a powder state, and in this respect, it is preferable to use FePt alloy powder.
- the method for heating and molding the mixed powder for pressure sintering produced as described above is not particularly limited, and examples thereof include a hot press method, a hot isostatic press method (HIP method), and discharge plasma.
- a sintering method (SPS method) or the like can be used.
- These molding methods are preferably carried out in a vacuum or in an inert atmosphere when carrying out the present invention. Thereby, even if oxygen is contained in the mixed powder to some extent, the amount of oxygen in the obtained sintered body is reduced.
- Pt used in the second embodiment is contained at 33 at% or more and 60 at% or less.
- FePt-based alloy powder consisting of Fe and inevitable impurities instead of using FePt-based alloy powder consisting of Fe and inevitable impurities as the balance, Pt is 33 at% to less than 60 at%, and one or more metal elements other than Fe and Pt are more than 0 at% and less than 20 at%
- a FePt alloy powder containing Pt and the one or more metal elements is 60 at% or less and the balance is Fe and inevitable impurities may be used. This is the same as when no metal element other than Fe and Pt is included (in the case of the second embodiment).
- FePt-based alloy powder made of Pt, Fe and inevitable impurities and metal powder made of one or more metal elements other than Fe and Pt containing inevitable impurities may be used.
- an FePt-based alloy powder composed of Pt, Fe and unavoidable impurities, and a metal powder composed of one or more metal elements other than Fe and Pt containing unavoidable impurities, the Pt, Fe and the one or more kinds.
- the ratio of the Pt to the total sum of metal elements is 33 at% or more and less than 60 at%, the ratio of the one or more metal elements to the total total is more than 0 at% and less than 20 at%, the Pt and the total to the total total Weigh so that the total ratio of one or more metal elements is 60 at% or less.
- the weighed FePt alloy powder, the weighed metal powder composed of one or more kinds of metal elements, and the oxide powder containing unavoidable impurities are mixed together and mixed to the extent that mechanical alloy is generated.
- the C powder which consists of primary particles containing an inevitable impurity and which does not constitute the secondary particles is added to the produced first mixed powder, and the primary particle diameter of the C powder is not substantially reduced.
- the produced powder mixture for pressure sintering is heated and molded under pressure.
- Pt simple substance powder containing inevitable impurities Fe simple substance powder containing inevitable impurities, and metal powder containing inevitable impurities and including one or more metal elements other than Fe and Pt may be used.
- the ratio of the Pt to the total amount of the Pt, the Fe, and the one or more metal elements is the Pt simple powder, the Fe simple powder, and the metal powder composed of one or more metal elements other than Fe and Pt. Is 33 at% or more and less than 60 at%, the ratio of the one or more metal elements to the total is more than 0 at% and 20 at% or less, and the total ratio of the Pt and the one or more metal elements to the total is Weigh so that it becomes 60 at% or less. Then, the weighed Pt simple substance powder, the weighed Fe simple substance powder, the weighed metal powder composed of one or more kinds of metal elements, and the oxide powder containing inevitable impurities are mixed and mixed to the extent that mechanical alloy is generated.
- a first mixed powder is produced.
- the C powder which consists of primary particles containing an inevitable impurity and which does not constitute the secondary particles is added to the produced first mixed powder, and the primary particle diameter of the C powder is not substantially reduced.
- the produced powder mixture for pressure sintering is heated and molded under pressure.
- the FePt—C-based sputtering target according to the second embodiment contains a metal oxide
- the FePt-based alloy powder (or Fe metal powder) is first prepared when preparing the mixed powder for pressure sintering.
- a Pt metal powder) and a metal oxide powder are sufficiently mixed to produce a first mixed powder in which the average particle size of the FePt alloy powder (or Fe metal powder and Pt metal powder) is reduced. Can do.
- the average particle diameter of the FePt-based alloy powder (or Fe metal powder and Pt metal powder) in the first mixed powder can be sufficiently reduced by sufficiently mixing with the metal oxide powder.
- the periphery of the primary particles C is FePt alloy powder (or Fe metal).
- the powder and Pt metal powder are easily covered with a fine powder, and the resulting powder mixture for pressure sintering is pressure-sintered, so that the periphery of the primary particles C is sufficiently covered with the FePt-based alloy phase.
- a target can be produced.
- the FePt alloy powder is produced at the stage of producing the first mixed powder.
- a target in which the periphery of C of the primary particles is sufficiently covered with the FePt-based alloy phase can be produced.
- the manufacturing method of the second embodiment uses a sintering method instead of a casting method, the content of C and metal oxide in the entire target can be increased, and the volume fraction of C in the entire target is increased. Is 5 vol% or more and less than 60 vol%, the volume fraction of the oxide phase with respect to the entire target is 3 vol% or more and less than 55 vol%, and the total volume fraction of the total of C and the oxide phase with respect to the target
- a FePt—C-based sputtering target having a content of 8 vol% or more and 60 vol% or less can be produced.
- the target can be used as a magnetic recording medium alone, that is, without using a plurality of targets.
- a thin film containing an FePt-based alloy can be formed.
- Example 1 The target of the composition of the mixed powder, sintered body, and target in Example 1 is 60.50 (50Fe-50Pt) -39.50C. That is, the target of the composition of the metal component is 50 at% Fe-50 at% Pt, and the target of the composition ratio between the FePt alloy and C (carbon) is 60.50 at% for the FePt alloy and 39.50 at% for C. When the content of C (carbon) is expressed in vol% instead of at%, the target of the composition of the mixed powder and target in Example 1 is (50Fe-50Pt) -30 vol% C.
- Fe atomized powder was prepared by a gas atomization method.
- the average particle diameter (median diameter) of the obtained Fe atomized powder was 45 ⁇ m.
- the obtained Fe atomized powder was classified with a sieve having an opening of 20 ⁇ m, and an Fe atomized powder having passed through a sieve with an opening of 20 ⁇ m was obtained.
- amorphous carbon having an average particle diameter of 8 ⁇ m were added to obtain amorphous carbon.
- the mixture was weakly mixed with a tumbler mixer (mixing for 15 minutes with a tumbler mixer using a ball) within a range in which the particle size of the powder was not substantially reduced to obtain a mixed powder for pressure sintering.
- the amorphous carbon used has an average particle size (median diameter) of C of primary particles of 8 ⁇ m and does not form secondary particles.
- the obtained powder mixture for pressure sintering was hot pressed under vacuum conditions of temperature: 1300 ° C., pressure: 26.2 MPa, time: 60 min, atmosphere: 5 ⁇ 10 ⁇ 2 Pa or less, and sintered body was made.
- the density of the produced sintered body was measured by the Archimedes method, and the measured value was divided by the theoretical density to obtain the relative density, which was 92.26%.
- a part of C (carbon) reacts with oxygen, and the composition ratio of FePt alloy and C (carbon) is obtained in the obtained target. Is slightly deviated from the target value, and the relative density of the obtained sintered body was calculated in consideration of the variation of C (carbon) (in other examples, comparative examples and reference examples in this specification).
- the relative density is calculated in consideration of the variation of C (carbon).
- FIG. 1 shows a metallographic micrograph of the sintered body of Example 1 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m).
- the dark gray circular portion is amorphous carbon
- the light gray portion is the FePt alloy phase.
- the C phase has a substantially spherical shape with a value obtained by dividing the major axis by the minor axis of 2 or less.
- a sputtering target having a diameter of 152 mm and a thickness of 2 mm was produced and joined to a backing plate having a diameter of 161 mm and a thickness of 4 mm.
- the sputter target after bonding was set in a sputtering apparatus, and sputtering was performed at an output of 500 W and an Ar gas pressure in the chamber of 1 Pa, and the number of generated particles was evaluated.
- the sputtering is temporarily stopped at each time point of the cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours, and a circular glass substrate having a diameter of 2.5 inches is set in the sputtering apparatus at each time point.
- Sputtering was performed for seconds.
- the sputtering cumulative duration is the cumulative time during which sputtering is performed.
- a circular glass substrate having a diameter of 2.5 inches that was sputtered for 2 seconds at each time point was taken out of the sputtering apparatus, set in an optical surface analyzer (optical surface analyzer), and the number of particles was measured. The number of pre-sputtering particles previously counted from the number of particles after sputtering at each time point was subtracted to obtain the number of particles at each time point.
- the number of particles at each time point of the cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours was 1080, 634, 1005, and 814, respectively.
- the graph which plotted those values is shown in FIG. 2, FIG. 3 with the result in another Example, a comparative example, and a reference example. 2 and 3, the horizontal axis represents the cumulative sputtering duration (h), and the vertical axis represents the number of particles (number). 2 and 3 are different in the step of the scale on the vertical axis, FIG. 2 has a large step of the scale on the vertical axis, and FIG. 3 has a small step of the scale on the vertical axis.
- Example 2 In this Example 2, a sintered body and sputtering were performed in the same manner as in Example 1 except that 107.19 g of Fe powder having an average particle size of 10 ⁇ m was used instead of 107.19 g of Fe atomized powder used in Example 1. A target was produced.
- FIG. 4 shows a metallographic micrograph of the sintered body of Example 2 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m).
- the dark gray circular portion is amorphous carbon
- the light gray portion is the FePt alloy phase.
- the C phase was substantially spherical with a value obtained by dividing the major axis by the minor axis of 2 or less.
- Example 2 similarly to Example 1, sputtering was performed using the obtained sputtering target, and the number of generated particles was evaluated. The number of particles at each time point of the cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours was 1643, 1258, 484, and 636, respectively.
- the graph which plotted those values is shown in FIG. 2, FIG. 3 with the result in another Example, a comparative example, and a reference example.
- Example 3 In this Example 3, when the mixed powder for pressure sintering was produced, weak mixing with a tumbler mixer (with a tumbler mixer using a ball for 15 minutes) within a range where the particle size of the amorphous carbon was not substantially reduced. The mixture was further mixed with a ball mill after mixing (at 300 rpm for 30 minutes ⁇ cumulative rotation number 9,000 times), and the temperature at the time of producing the sintered body was set to 1100 ° C. Thus, a sintered body and a sputtering target were produced.
- FIG. 5 shows a metallographic micrograph of the sintered body of Example 3 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m).
- the dark gray circular portion is amorphous carbon
- the light gray portion is the FePt alloy phase.
- the C phase has a substantially spherical shape with a value obtained by dividing the major axis by the minor axis of 2 or less.
- Example 3 in addition to weak mixing with a tumbler mixer, mixing with a ball mill (30 minutes at 300 rpm ⁇ cumulative rotation number 9,000 times)
- the structure photograph of FIG. 5 shows the shape of the amorphous carbon although the number of voids is reduced compared to the structure photographs of FIGS. 1 and 4 of Examples 1 and 2 in which only weak mixing was performed with a tumbler mixer.
- amorphous carbon having an average particle diameter of 8 ⁇ m is hardly pulverized by mixing in a ball mill having a cumulative number of rotations of about 9,000.
- Example 3 similarly to Examples 1 and 2, sputtering was performed using the obtained sputtering target, and the number of generated particles was evaluated. The number of particles at each time point of the cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours was 701, 203, 135, and 113, respectively. The graph which plotted those values is shown in FIG. 2, FIG. 3 with the result in another Example, a comparative example, and a reference example.
- the number of particles generated in the third embodiment is less than or equal to that in the first and second embodiments. Also from this point, a ball mill with a cumulative number of rotations of about 9,000 times In this mixing, it is considered that the amorphous carbon having an average particle diameter of 8 ⁇ m is hardly pulverized.
- the target of the composition of the mixed powder, sintered body and target in Comparative Example 1 is 60.50 (50Fe-50Pt) -39.50C. That is, the target of the composition of the metal component is 50 at% Fe-50 at% Pt, and the target of the composition ratio between the FePt alloy and C (carbon) is 60.50 at% for the FePt alloy and 39.50 at% for C, The same as in Examples 1 to 3.
- the target of the composition of the mixed powder and target in Comparative Example 1 is (50Fe-50Pt) -30 vol% C.
- FePt alloy atomized powder was produced by a gas atomizing method.
- the average particle diameter (median diameter) of the obtained FePt alloy atomized powder was 45 ⁇ m.
- the obtained powder mixture for pressure sintering is hot-pressed under conditions of temperature: 1460 ° C., pressure: 26.2 MPa, time: 60 min, atmosphere: 5 ⁇ 10 ⁇ 2 Pa or less, and sintered body was made.
- FIG. 6 shows a metallographic micrograph of the sintered body of Comparative Example 1 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m).
- the structure of the sintered body of Comparative Example 1 is very dense compared to the structures of the sintered bodies of Examples 1 to 3 (FIGS. 1, 4, and 5), and has a high magnification.
- the portion C is only observed as a dark gray small point.
- the size of small dark gray dots is considered to be about 0.5 ⁇ m or more when viewed from the scale in the photograph.
- the average particle size (median diameter) of the primary particles of carbon black used as the raw material powder was used. ) Is about 20 to 50 nm, and C dispersed in the FePt alloy phase is considered to form secondary particles.
- Examples 1 to 3 there are some voids (voids) that are black portions (portions indicated by arrows in FIGS. 1, 4 and 5) existing between the circular C phases. Such voids (voids) are not observed in the structure of the sintered body of Comparative Example 1. It is considered that the FePt alloy atomized powder having a large average particle diameter (median diameter) of 45 ⁇ m is sufficiently refined by long-time mixing in a ball mill.
- the number of particles at each time point of the cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours was 3019, 3587, 5803, and 4807, respectively.
- a graph in which these values are plotted is shown in FIG. 2 together with the results in other examples, comparative examples, and reference examples.
- the number of particles generated when sputtering is performed using the sputtering target of Comparative Example 1 is much larger than that in Examples 1 to 3.
- the carbon raw material powder used is carbon black having an average primary particle size (median diameter) of about 20 to 50 nm, which is extremely small, forming secondary particles, and in the FePt alloy phase. It is thought that secondary particles are also formed in The C of the secondary particles is a state in which the C of the primary particles is compacted, and the primary particles of C inside the secondary particles are not covered with the FePt alloy. It is thought that it falls out of the target and becomes particles. For this reason, it is considered that the number of particles generated when sputtering is performed using the sputtering target of Comparative Example 1 is much larger than that in Examples 1 to 3.
- the carbon black used as the raw material powder for C was mixed with the FePt alloy atomized powder for a long time in a ball mill and considered to be refined.
- FIG. 6 which is a metallographic micrograph of the magnification (photo magnification at the time of photographing is 1000 times)
- the portion C is only observed as a small dark gray point.
- the size of small dark gray dots is considered to be about 0.5 ⁇ m or more when viewed from the scale on the photograph.
- the average particle size of the primary particles of carbon black used as the raw material powder is 20 to Since it is about 50 nm, carbon black, which is the raw material powder used, is considered to form secondary particles even after long-time mixing in a ball mill.
- Reference Example 1 The target of the composition of the mixed powder, sintered body, and target in Reference Example 1 is 50Fe-50Pt, does not contain C (carbon), consists of only metal components Fe and Pt, and C (carbon). This is different from Examples 1 to 3 and Comparative Example 1 in which
- the obtained powder mixture for pressure sintering was hot pressed under vacuum conditions of temperature: 1300 ° C., pressure: 26.2 MPa, time: 60 min, atmosphere: 5 ⁇ 10 ⁇ 2 Pa or less, and sintered body was made.
- a sputtering target was produced in the same manner as in Examples 1 to 3 and Comparative Example 1, and the number of particles generated during sputtering was evaluated in Examples 1 to 3 and Comparative Example 1. The same was done.
- the number of particles at each time point of the cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours was 23, 7, 1, and 8, respectively.
- the graph which plotted those values is shown in FIG. 2, FIG. 3 with the result in another Example, a comparative example, and a reference example.
- the number of particles generated when sputtering was performed using the target of Reference Example 1 was extremely small. This is probably because the raw material powder is only metal powder (Fe powder, Pt powder) and C powder is not used.
- Example 4 The target of the composition of the mixed powder, sintered body and target in Example 4 is (50Fe-50Pt) -16.71 mol% C-6.51 mol% SiO 2 . That is, the target of the composition of the metal component is 50 at% Fe-50 at% Pt, and the target of the composition ratio of Fe, Pt, C (carbon) and SiO 2 is 38.39 mol% for Fe and 38.39 mol% for Pt. , C is 16.71 mol%, and SiO 2 is 6.51 mol%. When the contents of C (carbon) and SiO 2 are expressed in vol% instead of mol%, the target of the composition of the mixed powder and target in Example 4 is (50Fe-50Pt) -10 vol% C-20 vol% SiO. 2 .
- FePt alloy atomized powder was produced by a gas atomizing method.
- the average particle diameter (median diameter) of the obtained FePt alloy atomized powder was 45 ⁇ m.
- amorphous carbon having an average particle size of 8 ⁇ m to 990.00 g of the first mixed powder thus produced, and perform weak mixing with a tumbler mixer within a range where the particle size of the amorphous carbon does not substantially decrease. (Mixing with a tumbler mixer using a ball for 15 minutes) to obtain a mixed powder for pressure sintering.
- the amorphous carbon used is the same as that used in Examples 1 to 3, and no secondary particles are formed.
- the obtained powder mixture for pressure sintering was hot pressed under vacuum conditions of temperature: 1300 ° C., pressure: 26.2 MPa, time: 60 min, atmosphere: 5 ⁇ 10 ⁇ 2 Pa or less, and sintered body was made.
- FIG. 7 shows a metallographic micrograph of the sintered body of Example 4 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m).
- the dark gray circular portion is amorphous carbon
- the light gray portion is the FePt alloy phase.
- the black parts are voids (voids). It is considered that the FePt alloy atomized powder having a large average particle diameter (median diameter) of 45 ⁇ m is sufficiently refined by long-time mixing in a ball mill.
- a sufficiently refined FePt alloy atomized powder is likely to cover the periphery of amorphous carbon having a large average particle diameter of 8 ⁇ m.
- the C phase was substantially spherical with a value obtained by dividing the major axis by the minor axis of 2 or less.
- a sputtering target was prepared in the same manner as in Examples 1 to 3, Comparative Example 1 and Reference Example 1, and the number of particles generated during sputtering was evaluated in Examples 1 to 3. It carried out similarly to the comparative example 1 and the reference example 1.
- the number of particles at each time point of the cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours was 351, 110, 60, and 38, respectively.
- the graph which plotted those values is shown in FIG. 8, FIG. 9 with the result in another Example, a comparative example, and a reference example. 8 and 9, the horizontal axis represents the cumulative sputtering duration (h), and the vertical axis represents the number of particles (number).
- 8 and FIG. 9 are different in the step of the scale on the vertical axis, FIG. 8 has a large step of the scale on the vertical axis, and FIG. 9 has a small step of the scale on the vertical axis.
- Comparative Example 2 The target of the composition of the mixed powder, sintered body, and target in Comparative Example 2 is (50Fe-50Pt) -16.71 mol% C-6.51 mol% SiO 2, which is the same as Example 4. However, in Example 4, FePt alloy atomized powder and SiO 2 powder are first mixed to produce a first mixed powder, and then amorphous carbon is added to and mixed with the produced first mixed powder. In this comparative example 2, as will be described later, the FePt alloy atomized powder, carbon black, and SiO 2 powder are mixed at a time and mixed for pressure sintering. The point which produces the powder is a big difference.
- Example 4 As in Example 4, first, an FePt alloy atomized powder was prepared by the gas atomization method. The average particle diameter (median diameter) of the obtained FePt alloy atomized powder was 45 ⁇ m.
- the obtained powder mixture for pressure sintering was hot pressed under the conditions of a temperature of 1320 ° C., a pressure of 26.2 MPa, a time of 60 min, and an atmosphere of 5 ⁇ 10 ⁇ 2 Pa or less to obtain a sintered body.
- a temperature of 1320 ° C. a pressure of 26.2 MPa
- a time of 60 min a time of 60 min
- an atmosphere of 5 ⁇ 10 ⁇ 2 Pa or less was made.
- FIG. 10 shows a metallographic micrograph of the sintered body of Comparative Example 2 (photo magnification at the time of photographing is 1000 times, scale scale in the photo is 50 ⁇ m).
- the structure of the sintered body of Comparative Example 2 is very dense compared to the structure of the sintered body of Example 4 (FIG. 7).
- FIG. 10 which is a 1000 ⁇ magnification metal microscope photograph, the portion C is only observed as a dark gray small point.
- the size of the small dark gray dots is considered to be about 1 ⁇ m when viewed from the scale on the photograph, and the average particle size of the carbon black primary particles used is about 20 to 50 nm.
- C dispersed in the FePt alloy phase is considered to form secondary particles.
- Example 4 there are a small number of voids (voids) that are black portions (portions indicated by arrows in FIG. 7) existing between the circular C phases. Such voids (voids) are not observed in the tissue.
- a sputtering target was prepared in the same manner as in Examples 1 to 4, Comparative Example 1, and Reference Example 1, and the number of particles generated during sputtering was evaluated in Examples 1 to 4. It carried out similarly to the comparative example 1 and the reference example 1.
- the number of particles at the respective points of time for the cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours was 17584, 14466, 13377, and 14167, respectively.
- a graph in which these values are plotted is shown in FIG. 8 together with the results in other examples, comparative examples, and reference examples.
- the number of particles generated in this comparative example 2 is extremely larger than that in the fourth embodiment.
- the number of particles generated when sputtering is performed using the sputtering target of the present comparative example 2 is much larger than that of the fourth embodiment.
- the carbon raw material powder used is carbon black having an average primary particle size (median diameter) of as small as about 20 to 50 nm, forming secondary particles, and in the FePt alloy phase. It is thought that secondary particles are also formed in The C of the secondary particles is a state in which the C of the primary particles is compacted, and the primary particles of C inside the secondary particles are not covered with the FePt alloy. It is thought that it falls out of the target and becomes particles. For this reason, it is considered that the number of particles generated when sputtering is performed using the sputtering target of Comparative Example 2 is much larger than that in Example 4.
- Comparative Example 3 In this Comparative Example 3, the carbon raw material used in Comparative Example 2 was changed from 21.25 g of carbon black to 21.25 g of amorphous carbon, and the temperature at the time of producing the sintered body was changed to 1340 ° C. In the same manner as in Comparative Example 2, a sintered body and a sputtering target were produced.
- the amorphous carbon used is the same as that used in Examples 1 to 4, and no secondary particles are formed.
- FIG. 11 shows a metallographic micrograph of the sintered body of Comparative Example 3 (photo magnification at the time of photographing is 1000 times, and the scale scale in the photograph is 50 ⁇ m).
- the structure of the sintered body of Comparative Example 3 is very dense as compared with the structure of the sintered body of Example 4 (FIG. 7), similar to the sintered body of Comparative Example 2.
- FIG. 11 which is a metallographic micrograph of high magnification (photo magnification at the time of photographing is 1000 times)
- the portion C is only observed as a dark gray small point.
- Example 4 there are a small number of voids (voids) that are black portions (portions indicated by arrows in FIG. 7) that exist between the circular C phases. Such voids (voids) are not observed in the tissue.
- the structure (FIG. 11) of the sintered body of Comparative Example 3 is the same as the structure (FIG. 10) of the sintered body of Comparative Example 2, and the average particle diameter (median diameter) of primary particles as a carbon raw material. It was found that the structure of the sintered body obtained was the same whether carbon black of 20 to 50 nm or amorphous carbon having an average particle diameter of 8 ⁇ m was used. Even if amorphous carbon having an average particle size of 8 ⁇ m is used, it is considered that it is sufficiently mixed with the FePt alloy atomized powder and the SiO 2 powder for a long time by a ball mill and sufficiently pulverized.
- a sputtering target was prepared in the same manner as in Examples 1 to 4, Comparative Examples 1 and 2, and Reference Example 1, and the number of particles generated during sputtering was evaluated in Examples 1 to 4. 4. The same procedure as in Comparative Examples 1 and 2 and Reference Example 1 was performed.
- the number of particles at each time point of the cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours was 14266, 14562, 13681, and 13404, respectively.
- a graph in which these values are plotted is shown in FIG. 8 together with the results in other examples, comparative examples, and reference examples.
- Example 4 compared with Example 4 in which amorphous carbon was mixed within a range in which the particle size was not substantially reduced, this Comparative Example 3 in which the carbon raw material was sufficiently mixed by a ball mill. It was found that the number of particles generated during sputtering was very large. Even when the same carbon raw material as in Example 4 (amorphous carbon having an average particle diameter of 8 ⁇ m) with a small number of particles generated during sputtering is used, if it is sufficiently mixed by a ball mill, it will be crushed and the average particle diameter will be reduced. Are originally small carbon black (average particle size (median diameter) of primary particles is about 20 to 50 nm) and form secondary particles. The number of occurrences is thought to increase.
- the target of the composition of the mixed powder, sintered body, and target in Reference Example 2 is (50Fe-50Pt) -8.99 mol% SiO 2 . That is, the target of the composition of the metal component is 50 at% Fe-50 at% Pt, which is the same as in Example 4 and Comparative Examples 2 and 3, but does not contain C, and as a component other than metal Contains only SiO 2 . Incidentally, when the content of SiO 2 is displayed in mol% instead vol%, the target of the composition of the mixed powder and the target in the present reference example 2 is (50Fe-50Pt) -25vol% SiO 2.
- FePt alloy atomized powder was produced by a gas atomizing method.
- the average particle diameter (median diameter) of the obtained FePt alloy atomized powder was 45 ⁇ m.
- the obtained powder mixture for pressure sintering was hot pressed under the conditions of temperature: 1000 ° C., pressure: 26.2 MPa, time: 60 min, atmosphere: 5 ⁇ 10 ⁇ 2 Pa or less, and sintered body was made.
- FIG. 12 shows a metallographic micrograph of the sintered body of Reference Example 2 (photo magnification at the time of photographing is 1000 times, scale scale in the photograph is 50 ⁇ m).
- the structure of the sintered body of Reference Example 2 is very dense compared to the structure of the sintered body of Example 4 (FIG. 7), and the high magnification (photo magnification at the time of photographing is
- FIG. 12 which is a 1000 ⁇ magnification metal micrograph
- the SiO 2 site is only observed as a small dark gray point.
- Example 4 there are a few voids (voids) which are black portions (portions indicated by arrows in FIG. 7) existing between the circular C phases, but the sintered body of Reference Example 2 Such voids (voids) are not observed in the tissue.
- a sputtering target was prepared in the same manner as in Examples 1 to 4, Comparative Examples 1 to 3, and Reference Example 1, and the number of particles generated during sputtering was evaluated. 4. Performed in the same manner as Comparative Examples 1 to 3 and Reference Example 1.
- the number of particles at each time point of cumulative sputtering duration of 15 minutes, 30 minutes, 1 hour, and 2 hours was 48, 51, 27, and 35, respectively.
- the graph which plotted those values is shown in FIG. 8, FIG. 9 with the result in another Example, a comparative example, and a reference example.
- Examples 1 to 3 Comparative Example 1 and Reference Example 1 are cases in which no metal oxide (SiO 2 ) is contained.
- Examples 4, Comparative Examples 2, 3 and Reference Example 2 are metal oxides (SiO 2). 2 ) is included.
- the composition of the target is 60.50 (50Fe-50Pt) -39.50C, and the primary particles C dispersed in the FePt alloy phase constitute secondary particles.
- the primary particles C since it has a structure in which the primary particles C are not in contact with each other, they are included in the scope of the present invention.
- the target composition is 60.50 (50Fe-50Pt) -39.50C as in Examples 1 to 3, but the primary particles dispersed in the FePt alloy phase are secondary. Since the particles are composed of primary particles C in contact with each other, they are not included in the scope of the present invention.
- Examples 1 to 3 included in the scope of the present invention have a small number of particles generated at 113 to 814 when the cumulative sputtering duration is 2 hours, and the present invention Compared with the number of particles generated 4807 at the same time in Comparative Example 1 not included in the range of 1/40 to 1/6.
- the primary particles C dispersed in the FePt alloy phase do not constitute secondary particles, and the primary particles C contact each other. Therefore, it is considered that the primary particles C dispersed in the FePt alloy phase are almost entirely covered with the FePt alloy, and the primary particles C are formed into FePt during sputtering. It is considered that particles are difficult to fall off from the alloy phase and are difficult to generate.
- the carbon raw material powder used is carbon black having a very small average particle size (median diameter) of primary particles of about 20 to 50 nm. It is considered that secondary particles are also formed in the FePt alloy phase.
- the secondary particle C is in a state in which the primary particle C is compacted, and the C primary particle inside the secondary particle is not easily covered with the FePt alloy. It is thought that it is easy to fall off from the target in the state of a lump and easily becomes particles.
- Example 4 containing metal oxide (SiO 2 ), the composition of the target was 76.78 mol% (50Fe-50Pt) -16.71 mol% C-6.51 mol% SiO 2 , and the FePt alloy Since the primary particles C dispersed in the phase do not constitute secondary particles and the primary particles C are not in contact with each other, they are included in the scope of the present invention.
- Example 4 FePt alloy atomized powder having a large average particle size of 45 ⁇ m is used, but by mixing for a long time in the first stage (mixing before addition of C powder) in a ball mill after addition of SiO 2 , It is considered that the FePt alloy atomized powder is sufficiently refined, and it is considered that the FePt alloy atomized powder sufficiently covers the periphery of the primary particle C by the weak mixing after the addition of the C powder. For this reason, in the obtained target, it is considered that C of the primary particles are not in contact with each other but dispersed in the FePt alloy phase. In Example 4, at the time of the cumulative sputtering duration of 2 hours. It is considered that the number of particles generated was extremely reduced to 38.
- Comparative Examples 2 and 3 containing a metal oxide (SiO 2 ) the target composition was 76.78 mol% (50Fe-50Pt) -16.71 mol% C-6.51 mol as in Example 4. Although it is% SiO 2 , primary particles dispersed in the FePt alloy phase constitute secondary particles, and C of the primary particles are in contact with each other, and are not included in the scope of the present invention.
- amorphous carbon having an average particle diameter of 8 ⁇ m is used as the carbon raw material powder as in Example 4, but pulverized because it is sufficiently mixed with FePt atomized powder and SiO 2 powder in a ball mill.
- the average particle size becomes the same as that of carbon black whose average particle size is originally small (average particle size (median diameter) of primary particles is about 20 to 50 nm), and secondary particles are formed. Therefore, the FePt alloy atomized powder cannot sufficiently cover the periphery of C of the primary particles, and it is considered that C of the primary particles are in contact with each other in the obtained target. For this reason, it is considered that the number of particles generated during sputtering has increased.
- Reference Example 2 which does not contain C and contains only SiO 2 as a component other than the metal component has a very small number of particles generated during sputtering. This is presumably because SiO 2 has a higher adhesion strength to the metal than C, and the bond of atoms in SiO 2 is stronger than the bond of atoms in C 2 .
- the target according to the present invention can be suitably used as an FePt—C-based sputtering target.
- the manufacturing method according to the present invention can be suitably used as a method for manufacturing an FePt—C-based sputtering target.
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Abstract
Description
1-1.スパッタリングターゲットの構成成分および構造
本発明の第1実施形態に係るFePt-C系スパッタリングターゲットは、Fe、PtおよびCを含有するFePt-C系スパッタリングターゲットであって、Ptを33at%以上60at%以下含有して残部がFeおよび不可避的不純物からなるFePt系合金相中に、不可避的不純物を含む1次粒子のC同士がお互いに接触しないように分散した構造を有することを特徴とする。なお、本明細書では、数値範囲を表す際に「α以上β以下」のことを「α~β」と記すことがある。
FePt系合金は高温(例えば600℃以上)で熱処理をすることにより、高い結晶磁気異方性を持ったfct構造を備えることができるため、磁気記録媒体の記録層となる役割を有し、本発明の実施形態に係るFePt-C系スパッタリングターゲットにおいて主成分となる。
C(炭素)は、スパッタリングにより得られるFePtC系層中において、磁性粒子であるFePt系合金粒子同士を仕切る隔壁となり、FePtC系層中におけるFePt系合金粒子を小さく均一にする役割を有し、本第1実施形態に係るFePt-C系スパッタリングターゲットにおいて主成分の1つとなる。
本発明の第1実施形態に係るFePt-C系スパッタリングターゲットの構造は、Ptを33~60at%含有して残部がFeおよび不可避的不純物からなるFePt系合金相中に、不可避的不純物を含む1次粒子のC(炭素)同士がお互いに接触しないように分散した構造であり、1次粒子のC(炭素)は2次粒子を構成していない。
本第1実施形態に係るFePt-C系スパッタリングターゲットは、金属元素としてFeおよびPtのみ含んでいるが、FePt系合金相にFeおよびPt以外の金属元素を含ませてもよい(第1実施形態の変形例)。
本第1実施形態に係るFePt-C系スパッタリングターゲットは、Ptを33at%以上60at%以下含有して残部がFeおよび不可避的不純物からなる平均粒径20μm以下のFePt系合金粉末に、不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を添加して、該C粉末の1次粒子径が実質的に小さくならない範囲内(得られたターゲットを用いてスパッタリングを行った際に発生するパーティクル数が増加しない範囲内)で混合して加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することにより製造することができる。
本第1実施形態に係るFePt-C系スパッタリングターゲットにおいては、2次粒子を構成していない1次粒子のC(炭素)をFePt系合金相中に分散させて、1次粒子であるC(炭素)の周囲がFePt系合金で覆われやすくなるようにしているので、スパッタリング時にC(炭素)が塊の状態でターゲットから抜け落ちてパーティクルとなることが防止されており、パーティクルの発生の少ない良好なスパッタリングを実現することができる。
2-1.スパッタリングターゲットの構成成分および構造
第1実施形態に係るFePt-C系スパッタリングターゲットでは、合金成分としてFe、Ptを含有し、合金成分(Fe、Pt)以外にはC(炭素)を含有していたが、本発明の第2実施形態に係るFePt-C系スパッタリングターゲットでは、合金成分としてFe、Ptを含有し、合金成分(Fe、Pt)以外にはC(炭素)の他に酸化物を含有しており、この点が第1実施形態に係るFePt-C系スパッタリングターゲットとは異なる。即ち、本発明の第2実施形態に係るFePt-C系スパッタリングターゲットは、Ptを33at%以上60at%以下含有して残部がFeおよび不可避的不純物からなるFePt系合金相中に、不可避的不純物を含む1次粒子のCおよび不可避的不純物を含む金属酸化物が分散した構造を有し、前記1次粒子のCはお互いに接触していないことを特徴とする。
本第2実施形態におけるFePt系合金について説明すべき内容は、第1実施形態の「1-1-1.FePt合金について」で説明した内容と同様であるので、説明は省略する。
Cおよび金属酸化物は、スパッタリングによって得られる、FePt系合金ならびにCおよび金属酸化物を含有してなる層(以下、FePt-C-金属酸化物層と記すことがある。)中において、磁性粒子であるFePt系合金粒子同士を仕切る隔壁となり、FePt-C-金属酸化物層中におけるFePt系合金粒子を小さく均一にする役割を有し、本第2実施形態に係るFePt-C系スパッタリングターゲットにおいて主成分となる。
本発明の第2実施形態に係るFePt-C系スパッタリングターゲットの構造は、Ptを33~60at%含有して残部がFeおよび不可避的不純物からなるFePt系合金相中に、不可避的不純物を含む1次粒子のC(炭素)と不可避的不純物を含む金属酸化物とが分散した構造であり、1次粒子のC(炭素)はお互いに接触しておらず、2次粒子を構成していない。
本第2実施形態に係るFePt-C系スパッタリングターゲットは、金属元素としてFeおよびPtのみ含んでいるが、第1実施形態に係るFePt-C系スパッタリングターゲットと同様に、FePt系合金相にFeおよびPt以外の金属元素を含ませてもよい(第2実施形態の変形例)。
本第2実施形態に係るFePt-C系スパッタリングターゲットを製造する際には、まず、Ptを33~60at%含有して残部がFeおよび不可避的不純物からなるFePt系合金粉末と金属酸化物粉末とを十分に混合(メカニカルアロイが生じる程度まで混合)させることにより、FePt系合金粉末の平均粒径を十分に小さくした第1の混合粉末を作製する。FePt系合金粉末をアトマイズ法で作製すると、多くの場合、平均粒径が30μm以上となるが、このように平均粒径の大きいFePt系合金粉末であっても、金属酸化物粉末と十分に混合(メカニカルアロイが生じる程度まで混合)させることにより、平均粒径を十分に小さくすることができる。
本第2実施形態に係るFePt-C系スパッタリングターゲットにおいては、2次粒子を構成していない1次粒子のC(炭素)をFePt系合金相中に分散させて、1次粒子のC(炭素)同士が接触しないようにしており、1次粒子であるC(炭素)の周囲をFePt系合金で覆われやすくなるようにしているので、スパッタリング時にC(炭素)が塊の状態でターゲットから抜け落ちてパーティクルとなることが防止されており、パーティクルの発生の少ない良好なスパッタリングを実現することができる。
本実施例1における混合粉末、焼結体およびターゲットの組成の目標は60.50(50Fe-50Pt)-39.50Cである。即ち、金属成分の組成の目標は50at%Fe-50at%Ptであり、FePt合金とC(炭素)の組成比の目標は、FePt合金が60.50at%、Cが39.50at%である。なお、C(炭素)の含有量をat%ではなくvol%で表示すると、本実施例1における混合粉末およびターゲットの組成の目標は(50Fe-50Pt)-30vol%Cである。
本実施例2では、実施例1で用いたFeアトマイズ粉末107.19gに替えて、平均粒径10μmのFe粉107.19gを用いた以外は実施例1と同様にして、焼結体およびスパッタリングターゲットを作製した。
本実施例3では、加圧焼結用混合粉末作製時に、非晶質カーボンの粒径が実質的に小さくならない範囲内でタンブラーミキサーでの弱混合(ボールを用いたタンブラーミキサーでの15分間の混合)をした後にさらにボールミルで混合(300rpmで30min→累積回転回数9,000回)したこと、および焼結体作製時の温度を1100℃にしたこと以外は、実施例1、2と同様にして、焼結体およびスパッタリングターゲットを作製した。
本比較例1における混合粉末、焼結体およびターゲットの組成の目標は60.50(50Fe-50Pt)-39.50Cである。即ち、金属成分の組成の目標は50at%Fe-50at%Ptであり、FePt合金とC(炭素)の組成比の目標は、FePt合金が60.50at%、Cが39.50at%であり、実施例1~3と同様である。なお、C(炭素)の含有量をat%ではなくvol%で表示すると、本比較例1における混合粉末およびターゲットの組成の目標は(50Fe-50Pt)-30vol%Cである。
本参考例1における混合粉末、焼結体およびターゲットの組成の目標は50Fe-50Ptであり、C(炭素)は含有されておらず、金属成分であるFeおよびPtのみからなり、C(炭素)が含有されていた実施例1~3、比較例1とは異なる。
本実施例4における混合粉末、焼結体およびターゲットの組成の目標は(50Fe-50Pt)-16.71mol%C-6.51mol%SiO2である。即ち、金属成分の組成の目標は50at%Fe-50at%Ptであり、Fe、Pt、C(炭素)、SiO2の組成比の目標は、Feが38.39mol%、Ptが38.39mol%、Cが16.71mol%、SiO2が6.51mol%である。なお、C(炭素)およびSiO2の含有量をmol%ではなくvol%で表示すると、本実施例4における混合粉末およびターゲットの組成の目標は(50Fe-50Pt)-10vol%C-20vol%SiO2である。
本比較例2における混合粉末、焼結体およびターゲットの組成の目標は(50Fe-50Pt)-16.71mol%C-6.51mol%SiO2であり、実施例4と同様である。ただし、実施例4では、FePt合金アトマイズ粉末とSiO2粉末とをまず混合して第1の混合粉末を作製し、次に、作製した第1の混合粉末に非晶質カーボンを添加、混合して加圧焼結用混合粉末を作製していたが、本比較例2では、後述するように、FePt合金アトマイズ粉末とカーボンブラックとSiO2粉末とを一度で混合して加圧焼結用混合粉末を作製している点が、大きな相違点となっている。
本比較例3では、比較例2で用いたカーボン原材料をカーボンブラック21.25gから非晶質カーボン21.25gに替えたこと、および焼結体作製時の温度を1340℃にしたこと以外は、比較例2と同様にして、焼結体およびスパッタリングターゲットを作製した。なお、用いた非晶質カーボンは実施例1~4で用いたものと同一であり、2次粒子を形成していない。
本参考例2における混合粉末、焼結体およびターゲットの組成の目標は(50Fe-50Pt)-8.99mol%SiO2である。即ち、金属成分の組成の目標は50at%Fe-50at%Ptであり、この点は実施例4、比較例2、3と同様であるが、Cが含まれておらず、金属以外の成分としてはSiO2しか含まれていない。なお、SiO2の含有量をmol%ではなくvol%で表示すると、本参考例2における混合粉末およびターゲットの組成の目標は(50Fe-50Pt)-25vol%SiO2である。
実施例1~4、比較例1~3、参考例1、2についての主要なデータを次の表1にまとめて示す。
Claims (28)
- Fe、PtおよびCを含有するFePt-C系スパッタリングターゲットであって、
Ptを33at%以上60at%以下含有して残部がFeおよび不可避的不純物からなるFePt系合金相中に、不可避的不純物を含む1次粒子のC同士がお互いに接触しないように分散した構造を有することを特徴とするFePt-C系スパッタリングターゲット。 - Fe、PtおよびCを含有し、さらにFe、Pt以外の1種以上の金属元素を含有するFePt-C系スパッタリングターゲットであって、
Ptを33at%以上60at%未満、Fe、Pt以外の前記1種以上の金属元素を0at%よりも多く20at%以下含有し、かつ、Ptと前記1種以上の金属元素の合計が60at%以下であり、残部がFeおよび不可避的不純物からなるFePt系合金相中に、不可避的不純物を含む1次粒子のC同士がお互いに接触しないように分散した構造を有することを特徴とするFePt-C系スパッタリングターゲット。 - Fe、Pt以外の前記1種以上の金属元素は、Cu、Ag、Mn、Ni、Co、Pd、Cr、V、Bのうちの1種以上であることを特徴とする請求項2に記載のFePt-C系スパッタリングターゲット。
- 前記1次粒子の平均粒径は、1μm以上30μm以下であることを特徴とする請求項1~3のいずれかに記載のFePt-C系スパッタリングターゲット。
- 前記Cの結晶構造は、非晶質構造もしくはダイヤモンド構造であることを特徴とする請求項1~4のいずれかに記載のFePt-C系スパッタリングターゲット。
- 前記Cのターゲット全体に対する体積分率が5vol%以上60vol%以下であることを特徴とする請求項1~5のいずれかに記載のFePt-C系スパッタリングターゲット。
- 前記Cの全表面積のうち前記FePt系合金相に覆われている表面積は前記Cの全表面積の80%以上であることを特徴とする請求項1~6のいずれかに記載のFePt-C系スパッタリングターゲット。
- 前記FePt系合金相中にさらに酸化物相が分散していることを特徴とする請求項1~7のいずれかに記載のFePt-C系スパッタリングターゲット。
- 前記Cのターゲット全体に対する体積分率が5vol%以上60vol%未満であり、前記酸化物相のターゲット全体に対する体積分率が3vol%以上55vol%未満であり、かつ、前記Cと前記酸化物相との合計のターゲット全体に対する体積分率が8vol%以上60vol%以下であることを特徴とする請求項8に記載のFePt-C系スパッタリングターゲット。
- 前記酸化物相は、SiO2、TiO2、Ti2O3、Ta2O5、Cr2O3、CoO、Co3O4、B2O3、Fe2O3、CuO、Cu2O、Y2O3、MgO、Al2O3、ZrO2、Nb2O5、MoO3、CeO2、Sm2O3、Gd2O3、WO2、WO3、HfO2、NiO2のうちの少なくとも1種を含んでなることを特徴とする請求項8または9に記載のFePt-C系スパッタリングターゲット。
- 前記Cは、長径を短径で除した値が2以下の略球形であることを特徴とする請求項1~10のいずれかに記載のFePt-C系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1~11のいずれかに記載のFePt-C系スパッタリングターゲット。
- Ptを33at%以上60at%以下含有して残部がFeおよび不可避的不純物からなる平均粒径20μm以下のFePt系合金粉末に、不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を添加して、該C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- 不可避的不純物を含み平均粒径が20μm以下のPt粉末と、不可避的不純物を含み平均粒径が20μm以下のFe粉末を、PtとFeの合計に対するPtの含有割合が33at%以上60at%以下となるように秤量し、秤量した前記Pt粉末、秤量した前記Fe粉末、および不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を、前記C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- Ptを33at%以上60at%未満、Fe、Pt以外の1種以上の金属元素を0at%よりも多く20at%以下含有し、かつ、Ptと前記1種以上の金属元素の合計が60at%以下であり、残部がFeおよび不可避的不純物からなる平均粒径20μm以下のFePt系合金粉末に、不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を添加して該C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- Pt、Feおよび不可避的不純物からなる平均粒径20μm以下のFePt系合金粉末と、不可避的不純物を含みFe、Pt以外の1種以上の金属元素からなる平均粒径20μm以下の金属粉末を、前記Pt、前記Fe、前記1種以上の金属元素の総合計に対する前記Ptの割合が33at%以上60at%未満、前記総合計に対する前記1種以上の金属元素の割合が0at%よりも多く20at%以下、前記総合計に対する前記Ptと前記1種以上の金属元素の合計の割合が60at%以下となるように秤量し、秤量した前記FePt系合金粉末、秤量した前記1種以上の金属元素からなる金属粉末、および不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を、前記C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- 不可避的不純物を含み平均粒径が20μm以下のPt粉末と、不可避的不純物を含み平均粒径が20μm以下のFe粉末と、不可避的不純物を含み平均粒径が20μm以下のFe、Pt以外の1種以上の金属元素からなる金属粉末を、前記Pt、前記Fe、前記1種以上の金属元素の総合計に対するPtの割合が33at%以上60at%未満、前記総合計に対する前記1種以上の金属元素の割合が0at%よりも多く20at%以下、前記総合計に対するPtと前記1種以上の金属元素の合計の割合が60at%以下となるように秤量し、秤量した前記Pt粉末、秤量した前記Fe粉末、秤量した前記1種以上の金属元素からなる金属粉末、および不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を、前記C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- 前記C粉末の前記加圧焼結用混合粉末全体に対する体積分率が5vol%以上60vol%以下であることを特徴とする請求項13~17のいずれかに記載のFePt-C系スパッタリングターゲットの製造方法。
- Ptを33at%以上60at%以下含有して残部がFeおよび不可避的不純物からなるFePt系合金粉末に、不可避的不純物を含む酸化物粉末を添加してメカニカルアロイが生じる程度まで混合して第1の混合粉末を作製し、作製した該第1の混合粉末に不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を添加して、該C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- 不可避的不純物を含むPt粉末と、不可避的不純物を含むFe粉末を、PtとFeの合計に対するPtの含有割合が33at%以上60at%以下となるように秤量し、秤量した前記Pt粉末、秤量した前記Fe粉末、および不可避的不純物を含む酸化物粉末を混ぜ合わせ、メカニカルアロイが生じる程度まで混合して第1の混合粉末を作製し、作製した該第1の混合粉末に不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を添加して、該C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- Ptを33at%以上60at%未満、Fe、Pt以外の1種以上の金属元素を0at%よりも多く20at%以下含有し、かつ、Ptと前記1種以上の金属元素の合計が60at%以下であり、残部がFeおよび不可避的不純物からなるFePt系合金粉末に、不可避的不純物を含む酸化物粉末を添加してメカニカルアロイが生じる程度まで混合して第1の混合粉末を作製し、作製した該第1の混合粉末に不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を添加して、該C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- Pt、Feおよび不可避的不純物からなるFePt系合金粉末と、不可避的不純物を含みFe、Pt以外の1種以上の金属元素からなる金属粉末を、前記Pt、前記Fe、前記1種以上の金属元素の総合計に対する前記Ptの割合が33at%以上60at%未満、前記総合計に対する前記1種以上の金属元素の割合が0at%よりも多く20at%以下、前記総合計に対する前記Ptと前記1種以上の金属元素の合計の割合が60at%以下となるように秤量し、秤量した前記FePt系合金粉末、秤量した前記1種以上の金属元素からなる金属粉末、および不可避的不純物を含む酸化物粉末を混ぜ合わせ、メカニカルアロイが生じる程度まで混合して第1の混合粉末を作製し、作製した該第1の混合粉末に不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を添加して、該C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- 不可避的不純物を含むPt粉末、不可避的不純物を含むFe粉末、不可避的不純物を含みFe、Pt以外の1種以上の金属元素からなる金属粉末を、前記Pt、前記Fe、前記1種以上の金属元素の総合計に対する前記Ptの割合が33at%以上60at%未満、前記総合計に対する前記1種以上の金属元素の割合が0at%よりも多く20at%以下、前記総合計に対する前記Ptと前記1種以上の金属元素の合計の割合が60at%以下となるように秤量し、秤量した前記Pt粉末、秤量した前記Fe粉末、秤量した前記1種以上の金属元素からなる金属粉末、および不可避的不純物を含む酸化物粉末を混ぜ合わせ、メカニカルアロイが生じる程度まで混合して第1の混合粉末を作製し、作製した該第1の混合粉末に不可避的不純物を含む1次粒子からなり2次粒子を構成していないC粉末を添加して、該C粉末の1次粒子径が実質的に小さくならない範囲内で混合し、加圧焼結用混合粉末を作製した後、作製した該加圧焼結用混合粉末を加圧下で加熱して成形することを特徴とするFePt-C系スパッタリングターゲットの製造方法。
- 前記C粉末の前記加圧焼結用混合粉末全体に対する体積分率が5vol%以上60vol%未満であり、前記酸化物粉末の前記加圧焼結用混合粉末全体に対する体積分率が3vol%以上55vol%未満であり、かつ、前記C粉末と前記酸化物粉末との合計の前記加圧焼結用混合粉末全体に対する体積分率が8vol%以上60vol%以下であることを特徴とする請求項19~23のいずれかに記載のFePt-C系スパッタリングターゲットの製造方法。
- Fe、Pt以外の前記1種以上の金属元素は、Cu、Ag、Mn、Ni、Co、Pd、Cr、V、Bのうちの1種以上であることを特徴とする請求項15、16、17、21、22、23のいずれかに記載のFePt-C系スパッタリングターゲットの製造方法。
- 前記酸化物粉末は、SiO2、TiO2、Ti2O3、Ta2O5、Cr2O3、CoO、Co3O4、B2O3、Fe2O3、CuO、Cu2O、Y2O3、MgO、Al2O3、ZrO2、Nb2O5、MoO3、CeO2、Sm2O3、Gd2O3、WO2、WO3、HfO2、NiO2のうちの少なくとも1種を含んでなることを特徴とする請求項19~24のいずれかに記載のFePt-C系スパッタリングターゲットの製造方法。
- 前記C粉末の1次粒子の平均粒径は、1μm以上30μm以下であることを特徴とする請求項13~26のいずれかに記載のFePt-C系スパッタリングターゲットの製造方法。
- 前記C粉末の結晶構造は、非晶質構造もしくはダイヤモンド構造であることを特徴とする請求項13~27のいずれかに記載のFePt-C系スパッタリングターゲットの製造方法。
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| WO2013190943A1 (ja) * | 2012-06-18 | 2013-12-27 | Jx日鉱日石金属株式会社 | 磁気記録膜用スパッタリングターゲット |
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| US20070189916A1 (en) | 2002-07-23 | 2007-08-16 | Heraeus Incorporated | Sputtering targets and methods for fabricating sputtering targets having multiple materials |
| KR100470151B1 (ko) | 2002-10-29 | 2005-02-05 | 한국과학기술원 | FePtC 박막을 이용한 고밀도 자기기록매체 및 그제조방법 |
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| JP5590322B2 (ja) * | 2010-11-12 | 2014-09-17 | 三菱マテリアル株式会社 | 磁気記録媒体膜形成用スパッタリングターゲットおよびその製造方法 |
| WO2012073882A1 (ja) | 2010-11-29 | 2012-06-07 | 三井金属鉱業株式会社 | スパッタリングターゲット |
| CN103270554B (zh) | 2010-12-20 | 2016-09-28 | 吉坤日矿日石金属株式会社 | 分散有C粒子的Fe-Pt型溅射靶 |
| JP5041262B2 (ja) | 2011-01-31 | 2012-10-03 | 三菱マテリアル株式会社 | 磁気記録媒体膜形成用スパッタリングターゲットおよびその製造方法 |
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| MY166492A (en) * | 2012-07-20 | 2018-06-27 | Jx Nippon Mining & Metals Corp | Sputtering target for forming magnetic recording film and process for producing same |
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| US10787732B2 (en) | 2016-03-07 | 2020-09-29 | Tanaka Kikinzoku Kogyo K.K. | FePt-C-based sputtering target |
| JP7005647B2 (ja) | 2018-03-27 | 2022-02-14 | Jx金属株式会社 | スパッタリングターゲット及びその製造方法、並びに磁気記録媒体の製造方法 |
| WO2019187243A1 (ja) * | 2018-03-27 | 2019-10-03 | Jx金属株式会社 | スパッタリングターゲット及びその製造方法、並びに磁気記録媒体の製造方法 |
| JPWO2019187243A1 (ja) * | 2018-03-27 | 2021-01-07 | Jx金属株式会社 | スパッタリングターゲット及びその製造方法、並びに磁気記録媒体の製造方法 |
| WO2019208463A1 (ja) * | 2018-04-27 | 2019-10-31 | 田中貴金属工業株式会社 | C含有スパッタリングターゲット及びその製造方法 |
| JP2019189923A (ja) * | 2018-04-27 | 2019-10-31 | 田中貴金属工業株式会社 | C含有スパッタリングターゲット及びその製造方法 |
| WO2019220675A1 (ja) * | 2018-05-14 | 2019-11-21 | 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 |
| 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 |
| WO2021010019A1 (ja) * | 2019-07-12 | 2021-01-21 | 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 |
| JPWO2021010019A1 (ja) * | 2019-07-12 | 2021-01-21 | ||
| JP7267425B2 (ja) | 2019-07-12 | 2023-05-01 | 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 |
| 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 |
|---|---|
| JPWO2014132746A1 (ja) | 2017-02-02 |
| SG11201506426TA (en) | 2015-09-29 |
| JP5965539B2 (ja) | 2016-08-10 |
| US10186404B2 (en) | 2019-01-22 |
| US20160013033A1 (en) | 2016-01-14 |
| TWI507549B (zh) | 2015-11-11 |
| CN105026610B (zh) | 2017-10-24 |
| MY172839A (en) | 2019-12-12 |
| CN105026610A (zh) | 2015-11-04 |
| TW201500563A (zh) | 2015-01-01 |
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