WO2017141558A1 - 磁気記録媒体用スパッタリングターゲット及び磁性薄膜 - Google Patents
磁気記録媒体用スパッタリングターゲット及び磁性薄膜 Download PDFInfo
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- WO2017141558A1 WO2017141558A1 PCT/JP2017/000022 JP2017000022W WO2017141558A1 WO 2017141558 A1 WO2017141558 A1 WO 2017141558A1 JP 2017000022 W JP2017000022 W JP 2017000022W WO 2017141558 A1 WO2017141558 A1 WO 2017141558A1
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Images
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
- G11B5/65—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition
- G11B5/658—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition containing oxygen, e.g. molecular oxygen or magnetic oxide
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/851—Coating a support with a magnetic layer by sputtering
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
- H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
- H01F10/12—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
- H01F10/14—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel
Definitions
- the present invention relates to a sputtering target suitable for forming a magnetic thin film on a magnetic recording medium.
- the present invention relates to a sputtering target having a structure in which a nonmagnetic phase is dispersed in a magnetic phase mainly composed of Fe—Pt.
- the above magnetic crystal particles use a ferromagnetic alloy mainly composed of Fe—Pt, and the nonmagnetic material uses carbon and its compound, boron and its compound, metal oxide, and the like.
- a granular structure type magnetic thin film is produced by sputtering a sputtering target having a texture structure in which a nonmagnetic phase is dispersed in a magnetic phase onto a substrate using a magnetron sputtering apparatus.
- deposits on the thin film forming substrate called particles are a problem in the sputtering process. It is known that many of the particles generated during film formation are oxides in the target. It is considered that abnormal discharge occurs on the sputtering surface of the target during sputtering, and that carbon and its compounds, boron and its compounds, metal oxides, and the like fall off from the sputtering surface of the target.
- Patent Documents 1 to 5 etc. when mixing and pulverizing raw material powder with a ball mill or the like, a primary sintered body powder obtained by mixing, sintering, and pulverizing a part of the raw material powder in advance is mixed to oxidize. A method for reducing the generation of particles while minimizing the target structure by suppressing the aggregation of objects is disclosed.
- a nonmagnetic phase such as carbon and its compound, boron and its compound, and metal oxide
- components constituting the nonmagnetic phase may agglomerate. Aggregation sometimes caused particles during sputtering.
- the nonmagnetic phase composed of carbon and its compound, boron and its compound, metal oxide, etc. is finely dispersed in the magnetic phase composed of metal. It was done.
- an object of the present invention is to provide a sputtering target for a magnetic recording medium that can significantly reduce particles generated during sputtering. This makes it possible to form a high-quality magnetic recording layer and improve the yield of the magnetic recording medium.
- the present inventor has conducted intensive research, and as a result, by adding an oxide having a low viscosity, the magnetic phase composed of the metal in the target and carbon and its compound, boron and its compound, metal It has been found that adhesion to a nonmagnetic phase made of an oxide or the like is increased, the nonmagnetic phase is prevented from being separated during sputtering, and the generation of particles can be greatly reduced.
- One or more oxides selected from FeO, Fe 3 O 4 , K 2 O, Na 2 O, PbO, ZnO are 0.1 to 10 mol%, Pt is 5 to 70 mol%, and the remainder is Fe
- a sputtering target characterized by comprising: 2) The oxide containing one or more elements selected from Al, B, Si, and Ti, carbon, boron, boron nitride, and boron carbide in a total amount of 1 to 50 mol%, 1) The sputtering target as described.
- One or more selected from Au, Ag, Cu, Ga, Ge, Ir, Mn, Mo, Nb, Ni, Pd, Re, Rh, Ru, Sn, Ta, W, V, Zn are 1
- One or more oxides selected from FeO, Fe 3 O 4 , K 2 O, Na 2 O, PbO, ZnO are 0.1 to 10 mol%, Pt is 5 to 70 mol%, and the remainder is Fe A film characterized by 6)
- the sputtering target of the present invention has an excellent effect that the amount of particles generated during sputtering can be greatly reduced, and the yield during film formation can be remarkably improved.
- a grain boundary of a nonmagnetic phase is easily formed so as to surround the magnetic particles, so that improvement in device characteristics can be expected.
- a material (low viscosity oxide) capable of reducing the viscosity of the nonmagnetic phase is added.
- the material (low-viscosity oxide) for reducing the viscosity of the nonmagnetic phase may be any one or more oxides selected from FeO, Fe 3 O 4 , K 2 O, Na 2 O, PbO, and ZnO. preferable.
- the viscosities at 1000 ° C. of FeO, Fe 3 O 4 , K 2 O, Na 2 O, PbO, and ZnO are 1.8 ⁇ 10 ⁇ 1 , 3.0 ⁇ 10 ⁇ 1 , 4.7 ⁇ , respectively.
- the viscosity of CaO, MgO, NiO at 1000 ° C. is relatively high values of 2.1 ⁇ 10 1 , 1.6 ⁇ 10 1 , and 1.8 ⁇ 10 0 poise, respectively.
- any one or more oxides selected from FeO, Fe 3 O 4 , K 2 O, Na 2 O, PbO, and ZnO are contained in the sputtering target in a total amount of 0.1 mol% or more and 10 mol% or less. It is preferable to add such that. If it is less than 0.1 mol%, it is difficult to obtain the effect of improving adhesion, while if it exceeds 10 mol%, desired magnetic properties may not be obtained. In order to further improve the adhesion, it is more preferable that these oxides be 0.1 mol% or more and 5 mol% or less. Further, it is possible to further contain other oxides in order to improve the magnetic characteristics.
- a metal having a composition containing at least Fe and Pt can be used as a component of the magnetic phase in the sputtering target of the present invention.
- a metal having a composition in which Pt is 5 mol% or more and 70 mol% or less and the balance is Fe can be used.
- the composition range of the magnetic phase is a molar fraction with respect to the composition obtained by subtracting the composition of the nonmagnetic phase from the total composition of the sputtering target.
- the components of the magnetic phase can be appropriately adjusted in composition within the above range as long as sufficient characteristics as a magnetic thin film can be obtained.
- Impurities inevitably mixed in the sputtering target change significantly with respect to the adhesion between the magnetic phase composed of metal and the nonmagnetic phase composed of carbon and its compound, boron and its compound, metal oxide, etc. It will not cause. Therefore, whether or not the sputtering target satisfies the composition range of the present invention can be considered by excluding such inevitable impurities.
- the sputtering target of the present invention is a total of any one or more of carbon, boron, boron nitride, boron carbide, oxide containing any one or more of Al, B, Si, Ti as a nonmagnetic phase. 1 to 50 mol% is preferable.
- a general perpendicular magnetic recording film contains, as a non-magnetic phase material, an oxide containing at least one of carbon, boron, boron nitride, boron carbide, Al, B, Si, and Ti as a constituent component.
- a nonmagnetic phase grain boundary is formed so as to surround the magnetic particles, thereby exhibiting a function as a perpendicular magnetic recording film.
- the sputtering target of the present invention preferably contains a non-magnetic material in a volume ratio of 10% or more and less than 55%, including the oxides (including low viscosity oxides) and carbides.
- a non-magnetic material in a volume ratio of 10% or more and less than 55%, including the oxides (including low viscosity oxides) and carbides.
- the sputtering target of the present invention is selected from Au, Ag, Cu, Ga, Ge, Ir, Mn, Mo, Nb, Ni, Pd, Re, Rh, Ru, Sn, Ta, W, V, and Zn as the magnetic phase. Any one or more of the above can be contained in the sputtering target in an amount of 1 mol% or more and 30 mol% or less. Thereby, the magnetic characteristics of the magnetic thin film can be improved. These metals are mainly contained in the magnetic phase, but may be partially contained in the nonmagnetic phase by being oxidized during sintering.
- the average area of nonmagnetic particles in the metal magnetic phase (substrate) is preferably in the range of 0.1 to 2000 ⁇ m 2 .
- production of the particle resulting from an oxide at the time of a sputtering can be reduced.
- the nonmagnetic particles include not only low viscosity oxides but also other nonmagnetic phases such as carbides.
- the average area is larger than 2000 ⁇ m 2, since the starting point of arcing occurs when coarse metal oxide particles are sputtered, there is a risk of increase in particles, while the average area per particle is 0.1 ⁇ m.
- the average area of the non-magnetic particles is determined by observing five regions in the plane as shown in FIG. 1 in order to reduce variation depending on the observation location.
- the boundary between the two can be clearly identified by the difference in contrast with the nonmagnetic phase portion made of boron, a compound thereof, a metal oxide, or the like. Then, the average area of the nonmagnetic particles surrounded by the boundary is calculated by the attached software. Specifically, as shown in FIG. 1, five points in the plane of the sintered body (sputtering target) (one center, one arbitrary point 30 mm inside from the outer periphery, and 90 points with the center of the target as the center of rotation) A tissue image is observed with a field of view of 216 ⁇ m ⁇ 288 ⁇ m at three points rotated by 180 °, 180 °, and 270 °. Next, these tissue images are converted into binarized images.
- the threshold value at the time of binarization is set between a difference in color tone at the boundary between a magnetic phase portion made of a metal component and a nonmagnetic phase portion made of carbon or a compound thereof, boron or a compound thereof, a metal oxide, or the like.
- a laser microscope image in which nonmagnetic particles composed of carbon or a compound thereof, boron or a compound thereof, a metal oxide, or the like are dispersed in a magnetic phase (matrix) composed of a metal component, the color difference at the boundary between the two is usually clear.
- it is also possible to increase the separation accuracy between the two by using a process such as a discriminant analysis method and a differential histogram method.
- the non-magnetic particles that are in contact with the image edges in the binarized image of each tissue image are calculated on the software at this stage to prevent the average area of the non-magnetic particles in each tissue image from being undercalculated. Exclude from the target. Next, the average value of the areas of nonmagnetic particles in each tissue image is calculated. Then, about the area of the nonmagnetic particle in each obtained observation location, the average of 5 locations is taken and it is set as the average area per nonmagnetic particle.
- the magnetic thin film produced using the sputtering target of the present invention contains 0.1 to 10 mol of one or more oxides selected from FeO, Fe 3 O 4 , K 2 O, Na 2 O, PbO, and ZnO. %, Pt is contained in an amount of 5 to 70 mol%, and the balance is Fe.
- a total of 1 to 50 mol% of oxide, carbon, boron, boron nitride, and boron carbide composed of one or more elements of Al, B, Si, and Ti are contained. It is characterized by that.
- the component composition selected from Au, Ag, Cu, Ga, Ge, Ir, Mn, Mo, Nb, Ni, Pd, Re, Rh, Ru, Sn, Ta, W, V, Zn 1 to 30 mol% of any one or more of the above.
- the sputtering target of the present invention can be produced, for example, by the following method using a powder sintering method.
- metal powder metal powder such as Fe powder, Pt powder, and, if necessary, Au powder, Ag powder, Cu powder, and Ga powder is prepared.
- the metal powder not only a single element metal powder but also an alloy powder can be used.
- These metal powders preferably have a particle size in the range of 1 to 10 ⁇ m. When the particle size is 1 to 10 ⁇ m, more uniform mixing is possible, and segregation and coarse crystallization can be prevented. When the particle size of the metal powder is larger than 10 ⁇ m, the non-magnetic particles may not be uniformly dispersed.
- oxide powder FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder, PbO powder, ZnO powder, and the Al 2 O 3 powder, B 2 O 3 powder, SiO 2 powder, Prepare TiO 2 powder.
- C powder, B powder, BN powder, and B 4 C powder are prepared as necessary. It is desirable to use oxide powder having a particle size in the range of 1 to 30 ⁇ m. When the particle size is 1 to 30 ⁇ m, the oxide powders are less likely to aggregate when mixed with the metal powder described above, and can be uniformly dispersed.
- the oxide powder when the average particle size of the oxide powder is larger than 30 ⁇ m, coarse nonmagnetic particles may be formed after sintering, and when the average particle size is smaller than 1 ⁇ m, the oxide powder may be aggregated.
- the above particle size range is a preferable range, and that deviating from this range is not a condition for negating the present invention.
- the raw material powder is measured so that it may become a desired composition, and it mixes also using a well-known method, such as a ball mill, also as a grinding
- the mixed powder thus obtained is molded and sintered by a hot press method in a vacuum atmosphere or an inert gas atmosphere.
- various pressure sintering methods such as a plasma discharge sintering method can be used.
- the hot isostatic pressing is effective for improving the density of the sintered body.
- the holding temperature at the time of sintering depends on the components of the target, but in many cases, it is in the temperature range of 700 to 1500 ° C.
- Examples 1 to 6 nonmagnetic phase C, etc.
- Fe powder and Pt powder are prepared as magnetic materials
- C powder and low-viscosity oxide are prepared as non-magnetic materials.
- FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder, PbO powder, ZnO Powder was prepared. Then, these powders were weighed so that the composition ratios shown in Table 1 were obtained.
- weighed powders were sealed in a 10-liter ball mill pot together with zirconia balls as grinding media, and rotated and mixed for 24 hours.
- the mixed powder taken out from the ball mill was filled in a carbon mold having a diameter of 190 mm and sintered by hot pressing.
- the hot pressing conditions were a vacuum atmosphere, a heating rate of 300 ° C./hour, a holding temperature of 1050 ° C., and a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of heating to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
- each sintered body of Examples 1 to 6 was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe to produce a disk-shaped target. These were attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva) and subjected to sputtering. The sputtering conditions were an input power of 1 kW and an Ar gas pressure of 1.7 Pa. After performing 2 kWhr of pre-sputtering, a film was formed on a 4-inch diameter silicon substrate for 20 seconds. For each of Examples 1 to 6, the number of particles having a size of 0.25 to 3 ⁇ m adhered on the substrate was measured with a particle counter. As a result, as shown in Table 1, it was significantly reduced as compared with the comparative examples described later.
- Examples 7 to 12 nonmagnetic phase B, etc.
- Fe powder and Pt powder are prepared as magnetic materials
- B powder and low viscosity oxide are prepared as nonmagnetic materials
- FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder, PbO powder, ZnO Powders were prepared and these powders were weighed so that the composition ratios shown in Table 1 were obtained.
- sintered bodies were produced in the same manner as in Examples 1 to 6. The cross section of the obtained sintered body was observed with a microscope in the same manner as in Examples 1 to 6. As a result, a structure in which the nonmagnetic phase was dispersed in the magnetic phase was confirmed.
- Example 7 For each of Examples 7 to 12, the average area per nonmagnetic particle was calculated in the same manner as in Examples 1 to 6. The results are shown in Table 1. Next, the sintered bodies of Examples 7 to 12 were sputtered in the same manner as in Examples 1 to 6, and the number of particles was measured. As a result, as shown in Table 1, it was significantly reduced as compared with the comparative examples described later.
- Example 13-18 Nonmagnetic phase BN, etc.
- Fe powder and Pt powder are prepared as magnetic materials
- BN powder and low viscosity oxide are prepared as nonmagnetic materials
- FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder, PbO powder, ZnO Powder was prepared, and these powders were weighed so as to have the composition ratios described in Table 1.
- sintered bodies were produced in the same manner as in Examples 1 to 6. The cross section of the obtained sintered body was observed with a microscope in the same manner as in Examples 1 to 6. As a result, a structure in which the nonmagnetic phase was dispersed in the magnetic phase was confirmed.
- Example 13 to 18 For each of Examples 13 to 18, the average area per nonmagnetic particle was calculated in the same manner as in Examples 1 to 6. The results are shown in Table 1. Next, the sintered bodies of Examples 7 to 12 were sputtered in the same manner as in Examples 1 to 6, and the number of particles was measured. As a result, as shown in Table 1, it was significantly reduced as compared with the comparative examples described later.
- Examples 19-24 nonmagnetic phase B 4 C, etc.
- Fe powder and Pt powder are prepared as magnetic materials
- B 4 C powder and FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder and PbO powder are used as non-magnetic materials as B 4 C powder.
- ZnO powder was prepared, and these powders were weighed so as to have the composition ratios described in Table 1.
- a sintered body was produced by the same method as in Examples 1 to 6. The cross section of the obtained sintered body was observed with a microscope in the same manner as in Examples 1 to 6. As a result, a structure in which the nonmagnetic phase was dispersed in the magnetic phase was confirmed.
- Example 19 For each of Examples 19 to 24, the average area per nonmagnetic particle was calculated in the same manner as in Examples 1 to 6. The results are shown in Table 1. Next, the sintered bodies of Examples 19 to 24 were sputtered in the same manner as in Examples 1 to 6, and the number of particles was measured. As a result, as shown in Table 1, it was significantly reduced as compared with the comparative examples described later.
- Example 25-30 Nonmagnetic phase Al 2 O 3 , etc.
- Fe powder and Pt powder are prepared as magnetic materials, Al 2 O 3 powder as non-magnetic materials, FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder, PbO as low viscosity oxides.
- Powders and ZnO powders were prepared, and these powders were weighed so as to have the composition ratios described in Table 1. Then, for each of Examples 25 to 30, sintered bodies were produced by the same method as in Examples 1 to 6. The cross section of the obtained sintered body was observed with a microscope in the same manner as in Examples 1 to 6. As a result, a structure in which the nonmagnetic phase was dispersed in the magnetic phase was confirmed.
- Example 25 to 30 For each of Examples 25 to 30, the average area per nonmagnetic particle was calculated in the same manner as in Examples 1 to 6. The results are shown in Table 1. Next, the sintered bodies of Examples 25 to 30 were sputtered in the same manner as in Examples 1 to 6, and the number of particles was measured. As a result, as shown in Table 1, it was significantly reduced as compared with the comparative examples described later.
- Examples 31-36 nonmagnetic phase B 2 O 3 , etc.
- Fe powder and Pt powder are prepared as magnetic materials, B 2 O 3 powder as non-magnetic materials, FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder, PbO as low viscosity oxides.
- Powders and ZnO powders were prepared, and these powders were weighed so as to have the composition ratios described in Table 1.
- a sintered body was produced by the same method as in Examples 1 to 6. The cross section of the obtained sintered body was observed with a microscope in the same manner as in Examples 1 to 6. As a result, a structure in which the nonmagnetic phase was dispersed in the magnetic phase was confirmed.
- Example 31 to 36 For each of Examples 31 to 36, the average area per nonmagnetic particle was calculated in the same manner as in Examples 1 to 6. The results are shown in Table 1. Next, the sintered bodies of Examples 31 to 36 were sputtered in the same manner as in Examples 1 to 6, and the number of particles was measured. As a result, as shown in Table 1, it was significantly reduced as compared with the comparative examples described later.
- Example 37-42 nonmagnetic phase SiO 2 , etc.
- the magnetic material providing a Fe powder, Pt powder, a non-magnetic material, SiO 2 powder as a low viscosity oxide, FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder, PbO powder, ZnO powder was prepared, and these powders were weighed so that the composition ratios shown in Table 1 were obtained.
- a sintered body was produced by the same method as in Examples 1 to 6. The cross section of the obtained sintered body was observed with a microscope in the same manner as in Examples 1 to 6. As a result, a structure in which the nonmagnetic phase was dispersed in the magnetic phase was confirmed.
- Example 37 to 42 For each of Examples 37 to 42, the average area per nonmagnetic particle was calculated in the same manner as in Examples 1 to 6. The results are shown in Table 1. Next, the sintered bodies of Examples 37 to 42 were sputtered in the same manner as in Examples 1 to 6, and the number of particles was measured. As a result, as shown in Table 1, it was significantly reduced as compared with the comparative examples described later.
- Example 43 to 48 nonmagnetic phase TiO 2 , etc.
- Fe powder and Pt powder are prepared as magnetic materials
- TiO 2 powder and low viscosity oxide are prepared as non-magnetic materials
- FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder, PbO powder, ZnO powder was prepared, and these powders were weighed so that the composition ratios shown in Table 1 were obtained.
- a sintered body was produced by the same method as in Examples 1 to 6. The cross section of the obtained sintered body was observed with a microscope in the same manner as in Examples 1 to 6. As a result, a structure in which the nonmagnetic phase was dispersed in the magnetic phase was confirmed.
- Example 43 to 48 For each of Examples 43 to 48, the average area per nonmagnetic particle was calculated in the same manner as in Examples 1 to 6. The results are shown in Table 1. Next, the sintered bodies of Examples 43 to 48 were sputtered in the same manner as in Examples 1 to 6, and the number of particles was measured. As a result, as shown in Table 1, it was significantly reduced as compared with the comparative examples described later.
- Examples 49-53 addition of metal elements
- C powder, B powder, BN powder as nonmagnetic materials , B 4 C powder, Al 2 O 3 powder, and low-viscosity oxide, FeO powder, Fe 3 O 4 powder, K 2 O powder, Na 2 O powder, and PbO powder are prepared.
- sintered bodies were produced by the same method as in Examples 1 to 6. The cross section of the obtained sintered body was observed with a microscope in the same manner as in Examples 1 to 6.
- Comparative Example 1-4 Nonmagnetic phase C, no low viscosity oxide
- Fe powder and Pt powder are prepared as magnetic materials
- C powder, CaO powder, MgO powder and NiO powder are prepared as nonmagnetic materials, and these powders are weighed so as to have the composition ratios shown in Table 1.
- Table 1 For each of Comparative Examples 1 to 4, sintered bodies were produced by the same method as in Examples 1 to 6.
- the average area per nonmagnetic particle was calculated in the same manner as in Examples 1 to 6. The results are shown in Table 1.
- the sintered bodies of Comparative Examples 1 to 4 were sputtered in the same manner as in Examples 1 to 6, and the number of particles was measured. As a result, as shown in Table 1, it increased significantly compared to the Examples.
- Comparative Example 5-11 Non-magnetic phase B, BN, Al 2 O 3 etc., no low viscosity oxide
- Fe powder and Pt powder are prepared as magnetic materials
- B powder, BN powder, B 4 C powder, Al 2 O 3 powder, B 2 O 3 powder, SiO 2 powder, and TiO 2 powder are prepared as nonmagnetic materials. These powders were weighed so that the composition ratios shown in Table 1 were obtained.
- sintered bodies were produced by the same method as in Examples 1 to 6.
- the average area per nonmagnetic particle was calculated in the same manner as in Examples 1 to 6. The results are shown in Table 1.
- the sintered bodies of Comparative Examples 5 to 11 were sputtered in the same manner as in Examples 1 to 6, and the number of particles was measured. As a result, as shown in Table 1, it increased significantly compared to the Examples.
- the sputtering target of the present invention has an excellent effect that the amount of particles generated during sputtering can be reduced and the yield during film formation can be improved. Therefore, it is useful as a sputtering target for forming a magnetic thin film of a magnetic recording medium represented by a hard disk drive.
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Abstract
Description
1)FeO、Fe3O4、K2O、Na2O、PbO、ZnOから選択されるいずれか一種以上の酸化物が0.1~10mol%、Ptが5~70mol%、残余がFeからなることを特徴とするスパッタリングターゲット。
2)Al、B、Si、Tiから選択されるいずれか一種以上の元素の酸化物、炭素、ホウ素、窒化ホウ素、及び、炭化ホウ素を、合計で1~50mol%含有することを特徴とする上記1)記載のスパッタリングターゲット。
3)Au、Ag、Cu、Ga、Ge、Ir、Mn、Mo、Nb、Ni、Pd、Re、Rh、Ru、Sn、Ta、W、V、Znから選択されるいずれか一種以上を、1~30mol%含有することを特徴とする上記1)又は2)記載のスパッタリングターゲット。
4)非磁性粒子1個あたりの平均面積が0.1~2000μm2であることを特徴とする上記1)~3)のいずれか一に記載のスパッタリングターゲット。
5)FeO、Fe3O4、K2O、Na2O、PbO、ZnOから選択されるいずれか一種以上の酸化物が0.1~10mol%、Ptが5~70mol%、残余がFeからなることを特徴とする膜。
6)Al、B、Si、Tiから選択されるいずれか一種以上の元素の酸化物、炭素、ホウ素、窒化ホウ素、及び、炭化ホウ素を、合計で1~50mol%含有することを特徴とする上記5)記載の膜。
7)Au、Ag、Cu、Ga、Ge、Ir、Mn、Mo、Nb、Ni、Pd、Re、Rh、Ru、Sn、Ta、W、V、Znから選択されるいずれか一種以上を、1~30mol%含有することを特徴とする上記5)又は6)記載の膜。
70mol%以下、残余がFeからなる組成の金属を用いることができる。また、磁気特性向上のため、他の金属をさらに含有させることも可能である。なお、上記磁性相の組成範囲は、スパッタリングターゲットの全組成から非磁性相の組成を差し引いた組成に対するモル分率である。
(非磁性相の測定方法)
装置:キーエンス社製 カラー3Dレーザー顕微鏡VK-9700
ソフトウェア:VK Analyzer(装置付属)
(非磁性粒子の平均面積の求め方)
非磁性粒子の測定には、上記レーザー顕微鏡による拡大像を用いる。金属成分からなる磁性相中に炭素又はその化合物、ホウ素又はその化合物、金属酸化物、等からなる非磁性粒子が分散した組織のレーザー顕微鏡像は、金属成分からなる磁性相部分と炭素又はその化合物、ホウ素又はその化合物、金属酸化物、等からなる非磁性相部分との間のコントラスト差によって両者の境界を明確に識別することができる。そして、その境界によって囲まれる非磁性粒子の平均面積を、上記付属のソフトウェアで計算する。
具体的には、図1に示すように、焼結体(スパッタリングターゲット)の面内5箇所(中心1点、外周から30mm内側の任意1点、及び、ターゲット中央を回転中心としてその点を90°、180°、270°回転させた3点)について、216μm×288μmの視野で組織像を観察する。
次に、これらの組織像を二値化画像に変換する。二値化に際しての閾値は、金属成分からなる磁性相部分と、炭素又はその化合物、ホウ素又はその化合物、金属酸化物、等からなる非磁性相部分の境界の色調の差異の間で設定する。金属成分からなる磁性相(マトリックス)中に炭素又はその化合物、ホウ素又はその化合物、金属酸化物、等からなる非磁性粒子が分散したレーザー顕微鏡像において両者の境界の色調差は通常明確であるが、場合によっては判別分析法、微分ヒストグラム法等の処理を併用して両者の分離精度を高めることもできる。
各組織像の二値化画像において画像端部に接触している非磁性粒子は、各組織像における非磁性粒子の平均面積が過小計算されることを防ぐために、この段階でソフトウェア上にて計算対象から除外する。次に、各組織像における非磁性粒子の面積の平均値を計算する。その後、得られた各観察箇所における非磁性粒子の面積について、5箇所の平均をとって非磁性粒子1個あたりの平均面積とする。
酸化物粉は粒径が1~30μmの範囲のものを用いることが望ましい。粒径が1~30μmであると前述の金属粉と混合した際に、酸化物粉同士が凝集しにくくなり、均一に分散させることが可能になる。一方、酸化物粉の平均粒径が30μmより大きい場合には焼結後に粗大な非磁性粒子が生じることがあり、1μmより小さい場合には、酸化物粉同士の凝集が生じることがある。また、C粉、B粉、BN粉、B4C粉の原料粉については、1~100μmの範囲のものを用いることが望ましい。
但し、以上の粒径範囲はあくまで好ましい範囲であり、この範囲を逸脱することが本発明を否定する条件でないことは当然理解されるべきである。
次に、このようにして得られた混合粉末をホットプレス法で真空雰囲気、あるいは、不活性ガス雰囲気において成型・焼結させる。また、前記ホットプレス以外にも、プラズマ放電焼結法など様々な加圧焼結方法を使用することができる。特に、熱間静水圧焼結法は焼結体の密度向上に有効である。焼結時の保持温度は、ターゲットの構成成分にもよるが、多くの場合、700~1500℃の温度範囲とする。
このように得られた焼結体を旋盤で所望の形状に加工することにより、本発明のスパッタリングターゲットを作製することができる。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、C粉、低粘度酸化物として、FeO粉、Fe3O4粉、K2O粉、Na2O粉、PbO粉、ZnO粉、を用意した。そして、これらの粉末を、表1に記載する組成比となるように秤量した。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、B粉、低粘度酸化物として、FeO粉、Fe3O4粉、K2O粉、Na2O粉、PbO粉、ZnO粉を用意しこれらの粉末を表1に記載する組成比となるように秤量した。そして、実施例7~12のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。得られた焼結体の断面について、実施例1~6と同様に顕微鏡で観察したところ、非磁性相が磁性相中に分散している組織が確認された。また、実施例7~12のそれぞれについて、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、実施例7~12のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、後述する比較例に比べて大幅に減少した。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、BN粉、低粘度酸化物として、FeO粉、Fe3O4粉、K2O粉、Na2O粉、PbO粉、ZnO粉、を用意し、これらの粉末を表1に記載する組成比となるように秤量した。そして、実施例13~18のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。得られた焼結体の断面について、実施例1~6と同様に顕微鏡で観察したところ、非磁性相が磁性相中に分散している組織が確認された。また、実施例13~18のそれぞれについて、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、実施例7~12のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、後述する比較例に比べて大幅に減少した。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、B4C粉、低粘度酸化物として、FeO粉、Fe3O4粉、K2O粉、Na2O粉、PbO粉、ZnO粉、を用意し、これらの粉末を表1に記載する組成比となるように秤量した。そして、実施例19~24のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。得られた焼結体の断面について、実施例1~6と同様に顕微鏡で観察したところ、非磁性相が磁性相中に分散している組織が確認された。また、実施例19~24のそれぞれについて、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、実施例19~24のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、後述する比較例に比べて大幅に減少した。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、Al2O3粉、低粘度酸化物として、FeO粉、Fe3O4粉、K2O粉、Na2O粉、PbO粉、ZnO粉、を用意し、これらの粉末を表1に記載する組成比となるように秤量した。そして、実施例25~30のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。得られた焼結体の断面について、実施例1~6と同様に顕微鏡で観察したところ、非磁性相が磁性相中に分散している組織が確認された。また、実施例25~30のそれぞれについて、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、実施例25~30のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、後述する比較例に比べて大幅に減少した。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、B2O3粉、低粘度酸化物として、FeO粉、Fe3O4粉、K2O粉、Na2O粉、PbO粉、ZnO粉、を用意し、これらの粉末を表1に記載する組成比となるように秤量した。そして、実施例31~36のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。得られた焼結体の断面について、実施例1~6と同様に顕微鏡で観察したところ、非磁性相が磁性相中に分散している組織が確認された。また、実施例31~36のそれぞれについて、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、実施例31~36のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、後述する比較例に比べて大幅に減少した。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、SiO2粉、低粘度酸化物として、FeO粉、Fe3O4粉、K2O粉、Na2O粉、PbO粉、ZnO粉、を用意し、これらの粉末を表1に記載する組成比となるように秤量した。そして、実施例37~42のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。得られた焼結体の断面について、実施例1~6と同様に顕微鏡で観察したところ、非磁性相が磁性相中に分散している組織が確認された。また、実施例37~42のそれぞれについて、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、実施例37~42のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、後述する比較例に比べて大幅に減少した。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、TiO2粉、低粘度酸化物として、FeO粉、Fe3O4粉、K2O粉、Na2O粉、PbO粉、ZnO粉、を用意し、これらの粉末を表1に記載する組成比となるように秤量した。そして、実施例43~48のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。得られた焼結体の断面について、実施例1~6と同様に顕微鏡で観察したところ、非磁性相が磁性相中に分散している組織が確認された。また、実施例43~48のそれぞれについて、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、実施例43~48のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、後述する比較例に比べて大幅に減少した。
磁性材料として、Fe粉、Pt粉、さらに、添加成分として、Au粉、Ag粉、Cu粉、Ge粉、Pd粉、を用意し、また、非磁性材料として、C粉、B粉、BN粉、B4C粉、Al2O3粉、低粘度酸化物として、FeO粉、Fe3O4粉、K2O粉、Na2O粉、PbO粉、を用意し、これらの粉末を表1に記載する組成比となるように秤量した。そして、実施例49~53のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。得られた焼結体の断面について、実施例1~6と同様に顕微鏡で観察したところ、非磁性相が磁性相中に分散している組織が確認された。また、実施例49~53のそれぞれについて、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、実施例48~53のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、後述する比較例に比べて大幅に減少した。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、C粉、CaO粉、MgO粉、NiO粉、を用意し、これらの粉末を表1に記載する組成比となるように秤量した。そして、比較例1~4のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。比較例1~4の得られた焼結体について、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、比較例1~4のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、実施例に比べて大幅に増加した。
磁性材料として、Fe粉、Pt粉を用意し、非磁性材料として、B粉、BN粉、B4C粉、Al2O3粉、B2O3粉、SiO2粉、TiO2粉を用意し、これらの粉末を表1に記載する組成比となるように秤量した。そして、比較例5~11のそれぞれについて、実施例1~6と同様の方法により、焼結体を作製した。比較例5~11の得られた焼結体について、実施例1~6と同様に、非磁性粒子1個あたりの平均面積を計算した。その結果を表1に示す。次に、比較例5~11のそれぞれの焼結体を、実施例1~6と同様に、スパッタリングを実施して、パーティクルの個数を測定した。その結果、表1に示す通り、実施例に比べて大幅に増加した。
Claims (7)
- FeO、Fe3O4、K2O、Na2O、PbO、ZnOから選択されるいずれか一種以上からなる酸化物が0.1~10mol%、Ptが5~70mol%、残余がFeからなることを特徴とするスパッタリングターゲット。
- Al、B、Si、Tiから選択されるいずれか一種以上からなる酸化物、炭素、ホウ素、窒化ホウ素、及び、炭化ホウ素を、合計で1~50mol%含有することを特徴とする請求項1記載のスパッタリングターゲット。
- Au、Ag、Cu、Ga、Ge、Ir、Mn、Mo、Nb、Ni、Pd、Re、Rh、Ru、Sn、Ta、W、V、Znから選択されるいずれか一種以上を、1~30mol%含有することを特徴とする請求項1又は2記載のスパッタリングターゲット。
- 非磁性粒子1個あたりの平均面積が0.1~2000μm2であることを特徴とする請求項1~3のいずれか一項に記載のスパッタリングターゲット。
- FeO、Fe3O4、K2O、Na2O、PbO、ZnOから選択されるいずれか一種以上からなる酸化物が0.1~10mol%、Ptが5~70mol%、残余がFeからなることを特徴とする膜。
- Al、B、Si、Tiから選択されるいずれか一種以上からなる酸化物、炭素、ホウ素、窒化ホウ素、及び、炭化ホウ素を、合計で1~50mol%含有することを特徴とする請求項5記載の膜。
- Au、Ag、Cu、Ga、Ge、Ir、Mn、Mo、Nb、Ni、Pd、Re、Rh、Ru、Sn、Ta、W、V、Znから選択されるいずれか一種以上を、1~30mol%含有することを特徴とする請求項5又は6記載の膜。
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---|---|---|---|---|
WO2021085410A1 (ja) * | 2019-11-01 | 2021-05-06 | 田中貴金属工業株式会社 | 熱アシスト磁気記録媒体用スパッタリングターゲット |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012029498A1 (ja) * | 2010-08-31 | 2012-03-08 | Jx日鉱日石金属株式会社 | Fe-Pt系強磁性材スパッタリングターゲット |
WO2013094605A1 (ja) * | 2011-12-22 | 2013-06-27 | Jx日鉱日石金属株式会社 | C粒子が分散したFe-Pt系スパッタリングターゲット |
WO2014064995A1 (ja) * | 2012-10-25 | 2014-05-01 | Jx日鉱日石金属株式会社 | 非磁性物質分散型Fe-Pt系スパッタリングターゲット |
WO2014185266A1 (ja) * | 2013-05-13 | 2014-11-20 | Jx日鉱日石金属株式会社 | 磁性薄膜形成用スパッタリングターゲット |
Family Cites Families (27)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6680831B2 (en) * | 2000-09-11 | 2004-01-20 | Matsushita Electric Industrial Co., Ltd. | Magnetoresistive element, method for manufacturing the same, and method for forming a compound magnetic thin film |
US20080057350A1 (en) * | 2006-09-01 | 2008-03-06 | Heraeus, Inc. | Magnetic media and sputter targets with compositions of high anisotropy alloys and oxide compounds |
US20090053089A1 (en) | 2007-08-20 | 2009-02-26 | Heraeus Inc. | HOMOGENEOUS GRANULATED METAL BASED and METAL-CERAMIC BASED POWDERS |
CN101685776B (zh) * | 2008-09-27 | 2011-10-05 | 中国科学院半导体研究所 | 一种改善ZnO薄膜欧姆接触的方法 |
JP4870855B2 (ja) * | 2009-08-06 | 2012-02-08 | Jx日鉱日石金属株式会社 | 無機物粒子分散型スパッタリングターゲット |
JP5540948B2 (ja) * | 2010-07-07 | 2014-07-02 | 三菱マテリアル株式会社 | スパッタリングターゲット |
CN103210115B (zh) | 2010-07-29 | 2016-01-20 | 吉坤日矿日石金属株式会社 | 磁记录膜用溅射靶及其制造方法 |
CN103168328B (zh) | 2010-12-17 | 2016-10-26 | 吉坤日矿日石金属株式会社 | 磁记录膜用溅射靶及其制造方法 |
US9945026B2 (en) | 2010-12-20 | 2018-04-17 | Jx Nippon Mining & Metals Corporation | Fe-Pt-based sputtering target with dispersed C grains |
US20130292245A1 (en) | 2010-12-20 | 2013-11-07 | Jx Nippon Mining & Metals Corporation | FE-PT-Based Ferromagnetic Sputtering Target and Method for Producing Same |
CN103262166B (zh) * | 2010-12-21 | 2016-10-26 | 吉坤日矿日石金属株式会社 | 磁记录膜用溅射靶及其制造方法 |
US9683284B2 (en) | 2011-03-30 | 2017-06-20 | Jx Nippon Mining & Metals Corporation | Sputtering target for magnetic recording film |
WO2013046882A1 (ja) | 2011-09-26 | 2013-04-04 | Jx日鉱日石金属株式会社 | Fe-Pt-C系スパッタリングターゲット |
TWI504768B (zh) | 2012-01-13 | 2015-10-21 | Tanaka Precious Metal Ind | FePt sputtering target and its manufacturing method |
SG11201404314WA (en) | 2012-02-22 | 2014-10-30 | Jx Nippon Mining & Metals Corp | Magnetic material sputtering target and manufacturing method for same |
JP5876138B2 (ja) | 2012-03-15 | 2016-03-02 | Jx金属株式会社 | 磁性材スパッタリングターゲット及びその製造方法 |
JP5705993B2 (ja) | 2012-05-22 | 2015-04-22 | Jx日鉱日石金属株式会社 | C粒子が分散したFe−Pt−Ag−C系スパッタリングターゲット及びその製造方法 |
MY167825A (en) | 2012-06-18 | 2018-09-26 | Jx Nippon Mining & Metals Corp | Sputtering target for magnetic recording film |
SG11201404072YA (en) | 2012-07-20 | 2014-10-30 | Jx Nippon Mining & Metals Corp | Sputtering target for forming magnetic recording film and process for producing same |
WO2014034390A1 (ja) | 2012-08-31 | 2014-03-06 | Jx日鉱日石金属株式会社 | Fe系磁性材焼結体 |
US10755737B2 (en) | 2012-09-21 | 2020-08-25 | Jx Nippon Mining & Metals Corporation | Fe-Pt based magnetic material sintered compact |
SG11201500762SA (en) * | 2012-10-23 | 2015-05-28 | Jx Nippon Mining & Metals Corp | Fe-Pt-BASED SINTERED COMPACT SPUTTERING TARGET AND MANUFACTURING METHOD THEREFOR |
MY172839A (en) * | 2013-03-01 | 2019-12-12 | Tanaka Precious Metal Ind | Fept-c-based sputtering target and method for manufacturing same |
SG11201501365WA (en) | 2013-03-12 | 2015-05-28 | Jx Nippon Mining & Metals Corp | Sputtering target |
KR20180088491A (ko) | 2013-11-28 | 2018-08-03 | 제이엑스금속주식회사 | 자성재 스퍼터링 타깃 및 그 제조 방법 |
WO2016047236A1 (ja) | 2014-09-22 | 2016-03-31 | Jx金属株式会社 | 磁気記録膜形成用スパッタリングターゲット及びその製造方法 |
SG11201704465WA (en) | 2015-03-04 | 2017-06-29 | Jx Nippon Mining & Metals Corp | Magnetic material sputtering target and method for producing same |
-
2017
- 2017-01-04 MY MYPI2018702637A patent/MY184036A/en unknown
- 2017-01-04 SG SG11201806169UA patent/SG11201806169UA/en unknown
- 2017-01-04 US US16/077,663 patent/US11837450B2/en active Active
- 2017-01-04 CN CN201780011757.2A patent/CN108699677B/zh active Active
- 2017-01-04 JP JP2017567977A patent/JP6553755B2/ja active Active
- 2017-01-04 WO PCT/JP2017/000022 patent/WO2017141558A1/ja active Application Filing
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012029498A1 (ja) * | 2010-08-31 | 2012-03-08 | Jx日鉱日石金属株式会社 | Fe-Pt系強磁性材スパッタリングターゲット |
WO2013094605A1 (ja) * | 2011-12-22 | 2013-06-27 | Jx日鉱日石金属株式会社 | C粒子が分散したFe-Pt系スパッタリングターゲット |
WO2014064995A1 (ja) * | 2012-10-25 | 2014-05-01 | Jx日鉱日石金属株式会社 | 非磁性物質分散型Fe-Pt系スパッタリングターゲット |
WO2014185266A1 (ja) * | 2013-05-13 | 2014-11-20 | Jx日鉱日石金属株式会社 | 磁性薄膜形成用スパッタリングターゲット |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2021085410A1 (ja) * | 2019-11-01 | 2021-05-06 | 田中貴金属工業株式会社 | 熱アシスト磁気記録媒体用スパッタリングターゲット |
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