WO2011070850A1 - Co若しくはCo合金相に酸化物相を分散させたスパッタリングターゲット、Co若しくはCo合金相と酸化物相とからなる磁性体薄膜及び同磁性体薄膜を用いた磁気記録媒体 - Google Patents
Co若しくはCo合金相に酸化物相を分散させたスパッタリングターゲット、Co若しくはCo合金相と酸化物相とからなる磁性体薄膜及び同磁性体薄膜を用いた磁気記録媒体 Download PDFInfo
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 33
- 229910000531 Co alloy Inorganic materials 0.000 title claims abstract description 22
- 230000005291 magnetic effect Effects 0.000 title claims description 41
- 239000000696 magnetic material Substances 0.000 title claims description 28
- 239000010409 thin film Substances 0.000 title claims description 21
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- 239000002245 particle Substances 0.000 claims abstract description 96
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- 229910045601 alloy Inorganic materials 0.000 claims description 20
- 239000000956 alloy Substances 0.000 claims description 20
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- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 9
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 8
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- 229910052681 coesite Inorganic materials 0.000 abstract 1
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- 239000000843 powder Substances 0.000 description 74
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Images
Classifications
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/851—Coating a support with a magnetic layer by sputtering
-
- C—CHEMISTRY; METALLURGY
- 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
-
- 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
- H01F10/16—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing cobalt
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
- H01F41/183—Sputtering targets therefor
Definitions
- the present invention relates to a sputtering target in which an oxide phase is dispersed in a Co or Co alloy phase used for forming a magnetic thin film of a magnetic recording medium, particularly a granular magnetic recording film of a hard disk adopting a perpendicular magnetic recording method.
- the present invention relates to the magnetic recording medium used.
- a technique for improving magnetic characteristics by finely dispersing a nonmagnetic material in a magnetic thin film has been developed.
- a hard disk recording medium employing a perpendicular magnetic recording system employs a granular film in which the magnetic interaction between the magnetic particles in the magnetic recording film is blocked or weakened by a non-magnetic material. Has improved various characteristics.
- the Co-Cr-Pt-SiO 2 in granular film as one of the best materials are known, granular film of the Co-Cr-Pt-SiO 2 is generally ferromagnetic mainly composed of Co It is produced by sputtering a non-magnetic material particle-dispersed magnetic material target in which SiO 2 as a non-magnetic material is uniformly finely dispersed in a Co—Cr—Pt alloy substrate.
- Such a non-magnetic material particle-dispersed magnetic material sputtering target cannot be uniformly and finely dispersed in the magnetic alloy substrate by the melting method, so that it can be manufactured by a powder metallurgy method.
- a powder metallurgy method Widely known.
- an alloy powder having an alloy phase produced by a rapid solidification method and a powder constituting the ceramic phase are mechanically alloyed, and the powder constituting the ceramic phase is uniformly dispersed in the alloy powder, and then molded by hot pressing and magnetically generated.
- Patent Document 1 A method for obtaining a sputtering target for a recording medium has been proposed (Patent Document 1).
- nonmagnetic material particle-dispersed magnetic material sputtering target can be produced by mixing by the above method and molding and sintering the mixed powder by hot pressing.
- magnetron sputtering apparatuses are widely used in the above-described formation of magnetic recording films because of their high productivity.
- a substrate serving as a positive electrode and a target serving as a negative electrode are opposed to each other, and an electric field is generated by applying a high voltage between the substrate and the target in an inert gas atmosphere.
- the inert gas is ionized and a plasma composed of electrons and cations is formed.
- the cations in the plasma collide with the surface of the target (negative electrode)
- atoms constituting the target are knocked out.
- the projected atoms adhere to the opposing substrate surface to form a film.
- the principle that the material constituting the target is formed on the substrate by such a series of operations is used.
- the magnetron sputtering device has a magnet on the back side of the target, and magnetic flux leaking from the magnet to the target surface (leakage magnetic flux) causes electrons to cycloidly move in the vicinity of the target surface to efficiently generate plasma. It is possible to generate.
- Co, Cr when a magnetic material target containing an oxide of a metal and SiO 2 such as Pt, since there is no conductivity oxide such as SiO 2, the area of each particle of oxide phase is exposed to the target surface If the thickness is large, there is a problem that the generation of particles increases during sputtering, and in order to solve the problem, it is necessary to reduce the area of each particle of the oxide phase as much as possible.
- Patent Document 2 describes that Cr is contained in the oxide phase, thereby suppressing the grain growth of the oxide phase and uniformly dispersing it, and obtaining a high-density target.
- it is important to suppress the grain growth of the oxide phase by using an electric current sintering method in addition to containing chromium.
- the chromium oxide content is as high as 1.2 to 12.0 mol%, and such a large amount of addition is a non-magnetic material particle-dispersed magnetic thin film and a magnetic recording medium using the same dispersed magnetic thin film. This is a problem because it will greatly change the characteristics.
- the silicon oxide raw material powder having an average particle size of 0.5 ⁇ m is used, the particle size of the obtained oxide phase is about 2 to 2.5 ⁇ m, and the particle size is sufficiently refined. There is a problem that it cannot be said.
- Patent Document 3 proposes that particle generation is suppressed by adding Cr oxide to the oxide phase.
- Patent Literature 4 Patent Literature 5 and the like are cited, and it is described that the generation of particles cannot be suppressed only by miniaturization of the silica phase and cannot be solved as “adhesion between the alloy phase and the silica phase is bad”.
- the quoted silica phase is 10 ⁇ m or less as “fine”, and the particle size of the raw material powder SiO 2 is 20 ⁇ m or less, and in the examples, 3 ⁇ m.
- the physical phase is a structure having a particle size larger than that.
- An object of the present invention is to provide a non-magnetic material particle-dispersed magnetic material sputtering target with reduced arcing, stable discharge obtained by a magnetron sputtering apparatus, and high density and fewer particles generated during sputtering. .
- the present inventors have conducted intensive research and found that a target capable of reducing arcing can be obtained by adjusting the target structure. Further, the present inventors have found that the density can be sufficiently increased and particles generated during sputtering can be reduced. Based on such knowledge, the present invention provides the following inventions.
- oxide phase a metal matrix phase containing Co and an oxide phase containing 6 to 14 mol% of SiO 2 that is dispersed in the form of particles (hereinafter referred to as “oxide phase”). It is a sputtering target and contains not less than 0.3 mol% and less than 1.0 mol% of Cr oxide scattered in or on the surface of the oxide phase in addition to the components constituting the metal matrix phase and the oxide phase.
- the metal matrix phase is Co metal alone or Cr: 6 to 40 mol%, and the balance is a Co-based alloy made of Co, or Cr: 6 to 40 mol%, Pt: 8 to 20 mol%
- These are typical Co-based nonmagnetic material particle-dispersed magnetic materials, and the present invention is suitable for these.
- the present invention is characterized in that the oxide phase particles can be miniaturized and the relative density can be improved.
- Nonmagnetic material particles comprising a metal matrix phase containing Co, an oxide phase containing 6 to 14 mol% of SiO 2 and a Cr oxide of 0.3 mol% or more and less than 1.0 mol% Dispersed magnetic thin film.
- the non-magnetic material particle-dispersed magnetic thin film of the present invention is obtained by forming a film using the above sputtering target, but the component composition of the thin film formed by sputtering reflects the component composition of the target. Therefore, it has the same component composition.
- the metal matrix phase is Co metal alone, Cr: 6 to 40 mol%, the balance is a Co-based alloy made of Co, or Cr: 6 to 40 mol%, Pt: 8 to 20 mol%
- the sputtering target in which the oxide phase is dispersed in the Co or Co alloy phase of the present invention desirably has a relative density of 98% or more as described above.
- the relative density is a value obtained by dividing the actually measured density of the target by the calculated density.
- the calculation density is a density when it is assumed that the constituent components of the target are mixed without diffusing or reacting with each other, and is calculated by the following equation.
- a target in which fine SiO 2, which is a nonmagnetic material, is uniformly dispersed in a base material of Co or an alloy containing Co as a main component can be obtained. That is, in addition to the components constituting the metal matrix phase and the oxide phase, 0.3 mol% or more and less than 1.0 mol% of Cr oxide scattered in the oxide phase or on the surface thereof are contained, and the oxide phase A sputtering target in which an oxide phase is dispersed in a Co or Co alloy phase having an average area of each particle of 2.0 ⁇ m 2 or less can be provided.
- the generation amount of particles can be greatly reduced by making the oxide particles of SiO 2 finer and densified. Furthermore, since it becomes a target with less arcing, stable discharge can be obtained, and there is an advantage that a magnetic thin film can be manufactured at low cost.
- tissue image when the target surface of Example 1 is observed with a scanning electron microscope (SEM). It is a structure
- the sputtering target in which the oxide phase is dispersed in the Co or Co alloy phase of the present invention comprises a magnetic metal matrix phase containing Co and 6 to 14 mol% of SiO 2 that is dispersed in the form of particles. It is a sputtering target composed of an oxide phase (hereinafter referred to as “oxide phase”). In addition to the components constituting the metal matrix phase and the oxide phase, it contains 0.3 mol% or more and less than 1.0 mol% of Cr oxide scattered in or on the surface of the oxide phase, The average area of each particle is 2.0 ⁇ m 2 or less. As described above, the present invention can be applied to Co or an alloy based on Co.
- Co-based non-magnetic material particle-dispersed magnetic material Cr is 6 to 40 mol%, and the balance is Co-based alloy composed of Co, or Cr: 6 to 40 mol%, Pt: 8 to 20 mol%.
- the balance is a Co-based alloy made of Co.
- the present invention is suitable for these.
- the conventional manufacturing method is on this extended line, and even when chromium oxide is added, sintering is performed at a high temperature for a long time for the purpose of improving the density, and as a result, per SiO 2 grain.
- the average area is 3 ⁇ m 2 or more. This cannot be said to be the refinement of SiO 2 grains, and it can be said that the abnormal discharge (arcing) and the generation of particles during the sputtering were tolerated. Further, although attempts such as Patent Document 2 and Patent Document 3 aiming at particle reduction have been made, the oxide phase has not been sufficiently miniaturized without affecting the characteristics of the magnetic material.
- the present invention solves this problem. That is, as a means for solving this problem, high-melting oxide fine particles having a much lower diffusion rate at the same temperature are interposed on the surface of the oxide containing SiO 2 or the gap between the oxide particles during sintering. It is proposed to suppress aggregation of oxides containing SiO 2 .
- the oxide phase containing SiO 2 means an oxide phase in which the oxide is only SiO 2 or a combination of SiO 2 and another oxide.
- the oxide may contain an oxide other than SiO 2 , for example, TiO 2 having similar characteristics, but means that the presence of the oxide is strongly influenced by SiO 2 .
- the oxide containing SiO 2 is sintered while maintaining the same particle size as the raw material powder. As a result, the area of each particle of the oxide phase can be reduced, and the sintering conditions can be reduced. Although it depends, it became possible to suppress to 2.0 ⁇ m 2 or less.
- the surface energy tends to agglomerate more easily as the particle size becomes smaller.
- This particle size cannot be made the particle size of the raw material powder.
- 0.3 mol% or more and less than 1.0 mol% of a high melting point oxide of Cr oxide is added. Further, the sintering conditions are moderately suppressed, and the growth of oxide particles containing SiO 2 is suppressed.
- the added amount of the Cr oxide is less than 0.3 mol%, the SiO 2 particles are aggregated and an average particle area of SiO 2 of 2.0 ⁇ m 2 or less cannot be achieved. As a result, the generation of particles cannot be reduced.
- the amount of Cr oxide added is 1.0 mol% or more, the magnetic characteristics change, and it becomes difficult to produce a magnetic film having predetermined characteristics. Further, to increase the density by adding 1.0 mol% or more, the sintering conditions become higher and longer, and diffusion / aggregation / growth during the sintering of SiO 2 is accelerated, which cannot be suppressed.
- SiO 2 is an insulator, the conductivity as a sintered body can be lowered to a specific resistance of 3.5 ⁇ 10 16 ⁇ ⁇ cm or less by adding a Cr oxide. Even when Cr oxide is not added intentionally, when Cr is contained in the matrix phase, it may be oxidized during sintering, and Cr oxide (Cr 2 O 3 ) may be formed in an amount of about 0.1 to 0.2 mol%. is there.
- the oxide-dispersed Co alloy sputtering target that has been conventionally produced would have been those containing Cr oxides about 0.1 ⁇ 0.2 mol% naturally this case, SiO 2 particle is It is coarse and no effect on the specific resistance and dielectric constant of the oxide phase can be obtained. This is an effect that remarkably appears when the content of Cr oxide is 0.3 mol% or more.
- the magnetic metal for example, Co powder with an average particle diameter of 1 ⁇ m, Cr powder with an average particle diameter of 2 ⁇ m, Pt powder with an average particle diameter of 2 ⁇ m A SiO 2 powder having an average particle size of 1 ⁇ m is prepared, and this and Cr 2 O 3 powder are mixed with a mixer.
- the average particle size of Cr 2 O 3 powder is preferably 0.6 ⁇ m or less.
- the average particle diameter of the raw material SiO 2 is 1 ⁇ m or less.
- the powder thus obtained is molded and sintered using a vacuum hot press apparatus, and is cut into a desired shape, whereby the oxide phase is dispersed in the Co or Co alloy phase of the present invention. Create a target. Molding / sintering is not limited to hot pressing, and plasma discharge sintering and hot isostatic pressing can also be used.
- the holding temperature at the time of sintering is preferably set to the lowest temperature in a temperature range where the target is sufficiently densified. Depending on the composition of the target, it is often in the temperature range of 900 to 1200 ° C.
- the average area per one SiO 2 particle can be obtained by image processing of a microscope observation image.
- the density is best measured by the Archimedes method, but may be calculated from dimensional measurement and weight measurement.
- the relative density can be calculated by using the calculated density obtained by calculating the absolute density measured in this manner assuming that each molecule is mixed in the composition ratio.
- the addition of Cr oxide can be obtained by uniformly mixing Cr 2 O 3 with mixed powder constituting each element powder or alloy powder such as Co—Cr—Pt—SiO 2 .
- Cr powder, Co—Cr powder and Co—Cr—Pt powder are appropriately naturally oxidized in the pulverization / mixing process, etc., and as a result, a part of Cr existing as a metal is changed to Cr oxide. It is also possible to add Cr oxide.
- Example 1 Co powder having an average particle diameter of 1 ⁇ m, Cr powder having an average particle diameter of 2 ⁇ m, SiO 2 powder having an average particle diameter of 1 ⁇ m, and Cr 2 O 3 powder having an average particle diameter of 0.6 ⁇ m were prepared as raw material powders. . These powders are the target composition 12.00Cr-7.58SiO 2 -0.75Cr 2 O 3 - so that the balance Co (mol%), Co powder 79.73wt%, Cr powder 10.60wt%, SiO 2 powders 7.73 wt% and Cr 2 O 3 powder 1.94 wt% were weighed respectively.
- Co powder, Cr powder, SiO 2 powder, and Cr 2 O 3 powder were enclosed in a ball mill pot having a capacity of 10 liters together with zirconia balls as a grinding medium, and rotated and mixed for 20 hours.
- This mixed powder was filled in a carbon mold and hot-pressed in a vacuum atmosphere under conditions of a temperature of 1150 ° C., a holding time of 90 minutes, and a pressure of 30 MPa to obtain a sintered body. Further, this was cut with a lathe to obtain a disk-shaped target having a diameter of 180 mm and a thickness of 7 mm.
- Example 1 a high-density target having a relative density exceeding 99% was obtained.
- a structure image when the polished surface of the target of Example 1 is observed with a scanning electron microscope (SEM) is shown in FIG.
- the characteristic feature of Example 1 is that the SiO 2 particles are finely dispersed in the matrix alloy phase.
- SiO 2 particles are finely dispersed.
- the average area of each particle of the oxide phase was 1.6 ⁇ m 2 .
- Table 1 shows the average area of each particle of the oxide phase and the analysis results of the components constituting the target.
- Comparative Example 1 Co powder having an average particle diameter of 1 ⁇ m, Cr powder having an average particle diameter of 2 ⁇ m, and SiO 2 powder having an average particle diameter of 1 ⁇ m were prepared as raw material powders. These powders were composed of 81.45 wt% Co powder, 10.72 wt% Cr powder, 7.83 wt% SiO 2 powder so that the target composition would be 12.00 Cr-7.58 SiO 2 -balance Co (mol%). Each was weighed by weight ratio. The difference from Example 1 is that Cr 2 O 3 powder is not added.
- this mixed powder was filled into a carbon mold and hot pressed under the conditions of a vacuum atmosphere, a temperature of 1150 ° C., a holding time of 90 minutes, and a pressure of 30 MPa. As a result, a sintered body was obtained. Further, this was cut with a lathe to obtain a disk-shaped target having a diameter of 180 mm and a thickness of 7 mm.
- Comparative Example 1 the relative density exceeded 99%, which was a high-density target as in Example 1.
- SEM scanning electron microscope
- the structural image of FIG. 2 it can be seen that in Comparative Example 1, the SiO 2 particles in the matrix alloy phase are coarser than in Example 1 described above.
- the average area of each particle of the oxide phase was 2.4 ⁇ m 2 .
- Table 1 shows the average area of each particle of the oxide phase and the analysis results of the components constituting the target.
- Example 2 In Example 2, as raw material powder, Co powder having an average particle diameter of 1 ⁇ m, Cr powder having an average particle diameter of 2 ⁇ m, Pt powder having an average particle diameter of 2 ⁇ m, Ru powder having an average particle diameter of 2 ⁇ m, Ta 2 O 5 having an average particle diameter of 2 ⁇ m. Powder, SiO 2 powder having an average particle diameter of 1 ⁇ m, and Cr 2 O 3 powder having an average particle diameter of 0.6 ⁇ m were prepared. Next, these powders were weighed so that the composition of the target was 16Cr-18Pt-4Ru-1Ta 2 O5-6SiO 2 -0.75Cr 2 O 3 balance Co (mol%).
- Co powder, Cr powder, Pt powder, Ru powder, SiO 2 powder, Ta 2 O 5 powder, and Cr 2 O 3 powder are enclosed in a ball mill pot with a capacity of 10 liters together with zirconia balls as a grinding medium for 20 hours.
- This mixed powder was filled in a carbon mold and hot-pressed in a vacuum atmosphere under conditions of a temperature of 1150 ° C., a holding time of 2 hours, and a pressure of 30 MPa to obtain a sintered body. Further, this was processed into a disk-shaped target having a diameter of 180.0 mm and a thickness of 7.0 mm using a lathe.
- Example 2 a high-density target having a relative density exceeding 99% was obtained.
- a structure image when the polished surface of the target of Example 2 is observed with a scanning electron microscope (SEM) is shown in FIG.
- the characteristic feature of Example 1 is that Ta 2 O 5 particles and SiO 2 particles are finely dispersed in the matrix alloy phase.
- Ta 2 O 5 particles and SiO 2 particles are finely dispersed.
- the average area of each particle of the oxide phase was 2.0 ⁇ m 2 .
- Table 1 shows the average area of each particle of the oxide phase and the analysis results of the components constituting the target.
- Comparative Example 2 In Comparative Example 2, as in Example 2, the raw material powder was Co powder having an average particle diameter of 1 ⁇ m, Cr powder having an average particle diameter of 2 ⁇ m, Pt powder having an average particle diameter of 2 ⁇ m, Ru powder having an average particle diameter of 2 ⁇ m, and average particles. A Ta 2 O 5 powder having a diameter of 2 ⁇ m and a SiO 2 powder having an average particle diameter of 1 ⁇ m were prepared. Each target was weighed so that the composition of the target was 16Cr-18Pt-4Ru-1Ta 2 O 5 -6SiO 2 -balance Co (mol%). The difference from Example 2 is that Cr 2 O 3 powder is not added.
- this mixed powder was filled in a carbon mold and hot pressed under the conditions of a vacuum atmosphere, a temperature of 1150 ° C., a holding time of 90 minutes, and a pressure of 30 MPa. As a result, a sintered body was obtained. Further, this was cut with a lathe to obtain a disk-shaped target having a diameter of 180 mm and a thickness of 7 mm.
- FIG. 4 shows a tissue image when the polished surface of the target of Comparative Example 3 was observed with a scanning electron microscope (SEM). As shown in the structure image of FIG. 4, it can be seen that in Comparative Example 2, Ta 2 O 5 grains and SiO 2 grains in the matrix alloy phase are coarser than in Example 2 described above. The average area of each particle of the oxide phase was 2.7 ⁇ m 2 . Table 1 shows the average area of each particle of the oxide phase and the analysis results of the components constituting the target.
- the present invention is composed of a metal matrix phase containing Co and an oxide phase containing 6 to 14 mol% of SiO 2 that is dispersed in the form of particles (hereinafter referred to as “oxide phase”).
- the sputtering target is 0.3 mol% or more and less than 1.0 mol% of Cr oxide scattered in or on the surface of the oxide phase.
- a sputtering target in which an oxide phase is dispersed in a Co or Co alloy phase, wherein the average area of each particle of the oxide phase is 2.0 ⁇ m 2 or less, and an oxidation containing SiO 2 The generation amount of particles can be greatly reduced by miniaturization and densification of physical particles.
- a sputtering target in which an oxide phase is dispersed in a Co or Co alloy phase by a magnetron sputtering apparatus can be realized. Furthermore, it becomes a target that can reduce arcing, and when used in a magnetron sputtering apparatus, the ionization promotion of inert gas proceeds efficiently, stable discharge is obtained, and it has an excellent effect of producing a magnetic thin film at low cost Therefore, it is useful as a sputtering target in which an oxide phase is dispersed in a Co or Co alloy phase used for forming a magnetic thin film of a magnetic recording medium, particularly a granular magnetic recording film of a hard disk adopting a perpendicular magnetic recording method. .
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Abstract
Description
このグラニュラー膜に最適な材料の一つとしてCo-Cr-Pt-SiO2が知られており、このCo-Cr-Pt-SiO2のグラニュラー膜は、一般に、Coを主成分とした強磁性のCo-Cr-Pt合金の素地中に非磁性材料であるSiO2が均一に微細分散した非磁性材粒子分散型磁性材ターゲットをスパッタリングして作製される。
例えば、急冷凝固法で作製した合金相を持つ合金粉末とセラミックス相を構成する粉末とをメカニカルアロイングし、セラミックス相を構成する粉末を合金粉末中に均一に分散させ、ホットプレスにより成形し磁気記録媒体用スパッタリングターゲットを得る方法が提案されている(特許文献1)。
また焼結後に密度の高い素材が得られれば、スパッタ時に問題となるパーティクルの発生量が少ないことが一般的に知られている。
スパッタリング法とは、正の電極となる基板と負の電極となるターゲットを対向させ、不活性ガス雰囲気下で、該基板とターゲット間に高電圧を印加して電場を発生させるものである。
この時、不活性ガスが電離し、電子と陽イオンからなるプラズマが形成されるが、このプラズマ中の陽イオンがターゲット(負の電極)の表面に衝突するとターゲットを構成する原子が叩き出されるが、この飛び出した原子が対向する基板表面に付着して膜が形成される。このような一連の動作により、ターゲットを構成する材料が基板上に成膜されるという原理を用いたものである。
Co、Cr、Ptなどの金属とSiO2などの酸化物を含有する磁性材ターゲットの場合、SiO2などの酸化物に導電性がないので、ターゲット表面に露出する酸化物相の各粒子の面積が大きいと、スパッタリング時にパーティクル発生が増加するという問題があり、それを解決するために、酸化物相の各粒子の面積を出来るだけ小さくする必要があった。
しかし、酸化クロム含有量が1.2~12.0mol%と多く、このような多量の添加は、非磁性材粒子分散型磁性体薄膜及び同分散型磁性体薄膜を用いた磁気記録媒体としての特性を大きく変えることになるので、問題である。また、平均粒径0.5μmの酸化ケイ素原料粉末を用いているにもかかわらず、得られた酸化物相の粒径が2~2.5μm程度であり、粒径が十分微細化されているとは言えないという問題がある。
この問題を解決するには、SiO2を均一に分散させることが有効である。
本発明は、アーキングを低減し、マグネトロンスパッタ装置で安定した放電が得られ、かつ、高密度でスパッタ時に発生するパーティクルの少ない非磁性材粒子分散型磁性材スパッタリングターゲットを提供することを課題とする。
このような知見に基づき、本発明は、次の発明を提供する。
より好ましい酸化物相の各粒子の平均面積は1.5μm2以下である。
これらは、代表的なCo系非磁性材粒子分散型磁性材であり、本願発明は、これらに好適である。
4)相対密度を98%以上であることを特徴とする上記1)~3)のいずれかに記載のCo若しくはCo合金相に酸化物相を分散させたスパッタリングターゲット。
本願発明は、酸化物相の粒子の微細化が可能であると共に、相対密度を向上させることができるという特徴を備えている。
本発明の非磁性材粒子分散型磁性体薄膜は、上記スパッタリングターゲットを用いて成膜することにより得られるものであるが、スパッタリングにより形成さられる薄膜の成分組成は、ターゲットの成分組成が反映されるので、同様の成分組成を備えている。
7)酸化物相の比抵抗が3.5×1016Ω・cm以下であることを特徴とする上記5)又は6)記載の非磁性材粒子分散型磁性体薄膜。
8)上記5)~7)のいずれかに記載の非磁性材粒子分散型磁性体薄膜を用いた磁気記録媒体。
ここでの相対密度とは、ターゲットの実測密度を計算密度で割り返して求めた値である。計算密度とはターゲットの構成成分が互いに拡散あるいは反応せずに混在していると仮定したときの密度で、次式で計算される。
式:計算密度=Σ(構成成分の分子量×構成成分のモル比)/Σ(構成成分の分子量×構成成分のモル比/構成成分の文献値密度)
ここでΣは、ターゲットの構成成分の全てについて、和をとることを意味する。
このように、SiO2の酸化物粒子の微細化と高密度化により、パーティクルの発生量を大きく低減させることができる。さらに、アーキングの少ないターゲットとなることから安定した放電が得られ、低コストで磁性体薄膜を製造できるというメリットがある。
前記金属マトリックス相及び酸化物相を構成する成分以外に、前記酸化物相内又はその表面に点在する0.3mol%以上、1.0mol%未満のCr酸化物を含有し、酸化物相の各粒子の平均面積が2.0μm2以下であることを特徴とする。
本願発明は、上記の通り、Co又はCoを基とする合金に適用できる。代表的なCo系非磁性材粒子分散型磁性材としては、Cr:6~40mol%であり、残部がCoからなるCo基合金、又はCr:6~40mol%、Pt:8~20mol%であり、残部がCoからなるCo基合金である。本願発明はこれらに好適である。
ここで「SiO2を含有する酸化物相」とは、酸化物がSiO2のみの場合及びSiO2と他の酸化物とを組合せた酸化物相を意味する。酸化物としてはSiO2以外の酸化物、例えば類似する特性のTiO2を含有する場合もあるが、酸化物の存在がSiO2の影響を強く受ける場合を意味するものである。
これにより、SiO2を含有する酸化物は原料粉体と同程度の粒子径を維持して焼結され、その結果、酸化物相の各粒子の面積を小さくすることができ、焼結条件にもよるが、2.0μm2以下に抑えることが可能となった。
以上を実現する手段として、Cr酸化物の高融点酸化物を0.3mol%以上、1.0mol%未満添加する。また、焼結条件を適度に抑制し、SiO2を含有する酸化物粒子の成長を抑制するものである。上記Cr酸化物の添加量が0.3mol%未満であると、SiO2の粒子が凝集し、SiO2の平均粒子面積2.0μm2以下を達成することができない。その結果パーティクルの発生が低減できない。
SiO2は絶縁体であるが、Cr酸化物を添加することにより、焼結体としての導電性を比抵抗3.5×1016Ω・cm以下に低くすることができる。
Cr酸化物を敢えて添加しない場合でも、マトリックス相にCrを含んでいる場合、焼結時に酸化し、Cr酸化物(Cr2O3)を0.1~0.2mol%程度形成される場合がある。
本発明のCo若しくはCo合金相に酸化物相を分散させたスパッタリングターゲットの製造に際し、磁性金属として、例えば平均粒径1μmのCo粉末、平均粒径2μmのCr粉末、平均粒径2μmのPt粉末、平均粒径1μmのSiO2粉末を用意し、これとCr2O3粉末をミキサーで混合する。
このようにして得られた粉末を、真空ホットプレス装置を用いて成型・焼結し、所望の形状へ切削加工することで、本発明のCo若しくはCo合金相に酸化物相を分散させたスパッタリングターゲットを作製する。
成型・焼結は、ホットプレスに限らず、プラズマ放電焼結法、熱間静水圧焼結法を使用することもできる。焼結時の保持温度はターゲットが十分緻密化する温度域のうち最も低い温度に設定するのが好ましい。ターゲットの組成にもよるが、多くの場合、900~1200°Cの温度範囲にある。
Cr酸化物の添加は、例えばCo-Cr-Pt-SiO2等の、各要素粉末、あるいは合金粉末を構成する混合粉末にCr2O3を均一に混合することにより得ることができる。また、粉砕・混合工程などで、Cr粉、Co-Cr粉やCo-Cr-Pt粉を適度に自然酸化させることで、結果として、金属として存在していたCrの一部をCr酸化物とすることによってもCr酸化物の添加は可能である。
実施例1では、原料粉末として、平均粒径1μmのCo粉末、平均粒径2μmのCr粉、平均粒径1μmのSiO2粉末、平均粒径を0.6μmのCr2O3粉末を用意した。
これらの粉末をターゲットの組成が12.00Cr-7.58SiO2-0.75Cr2O3-残部Co(mol%)となるように、Co粉末79.73wt%、Cr粉末10.60wt%、SiO2粉末7.73wt%、Cr2O3粉末1.94wt%、の重量比率でそれぞれ秤量した。
比較例1では、実施例1と同様に、原料粉末として、平均粒径1μmのCo粉末、平均粒径2μmのCr粉、平均粒径1μmのSiO2粉末を用意した。
これらの粉末をターゲットの組成が12.00Cr-7.58SiO2-残部Co(mol%)となるように、Co粉末81.45wt%、Cr粉末10.72wt%、SiO2粉末7.83wt%の重量比率でそれぞれ秤量した。実施例1との差異点は、Cr2O3粉末を添加していない点である。
実施例2では、原料粉末として、平均粒径1μmのCo粉末、平均粒径2μmのCr粉末、平均粒径2μmのPt粉末、平均粒径2μmのRu粉末、平均粒径2μmのTa2O5粉末、平均粒径1μmのSiO2粉末、平均粒径を0.6μmのCr2O3粉末を用意した。
次に、これらの粉末をターゲットの組成が16Cr-18Pt-4Ru-1Ta2O5-6SiO2-0.75Cr2O3残部Co(mol%)となるように、それぞれ秤量した。
この混合粉をカーボン製の型に充填し、真空雰囲気中、温度1150°C、保持時間2時間、加圧力30MPaの条件のもとホットプレスして焼結体を得た。さらにこれを旋盤で直径が180.0mm、厚さが7.0mmの円盤状のターゲットへ加工した。
比較例2では、実施例2と同様に、原料粉末として、平均粒径1μmのCo粉末、平均粒径2μmのCr粉末、平均粒径2μmのPt粉末、平均粒径2μmのRu粉末、平均粒径2μmのTa2O5粉末、平均粒径1μmのSiO2粉末を用意した。ターゲットの組成が16Cr-18Pt-4Ru-1Ta2O5-6SiO2-残部Co(mol%)となるようにそれぞれ秤量した。実施例2との差異点は、Cr2O3粉末を添加していない点である。
これらの粉末を実施例2と同様に混合した後、この混合粉をカーボン製の型に充填し、真空雰囲気中、温度1150°C、保持時間90分、加圧力30MPaの条件のもとホットプレスして、焼結体を得た。さらにこれを旋盤で切削加工して直径が180mm、厚さが7mmの円盤状のターゲットを得た。
Claims (8)
- Coを含有する金属マトリックス相と、SiO2を含有し、粒子を形成して分散して存在する6~14mol%の酸化物の相(以下、「酸化物相」という。)から構成されるスパッタリングターゲットであって、前記金属マトリックス相及び酸化物相を構成する成分以外に、前記酸化物相内又はその表面に点在する0.3mol%以上、1.0mol%未満のCr酸化物を含有し、酸化物相の各粒子の平均面積が2.0μm2以下であることを特徴とするCo若しくはCo合金相に酸化物相を分散させたスパッタリングターゲット。
- 前記金属マトリックス相が、Co金属単独であるか、Cr:6~40mol%であり、残部がCoからなるCo基合金であるか、又はCr:6~40mol%、Pt:8~20mol%であり、残部がCoからなるCo基合金であることを特徴とする請求項1記載のCo若しくはCo合金相に酸化物相を分散させたスパッタリングターゲット。
- 比抵抗が3.5×1016Ω・cm以下であることを特徴とする請求項1又は2記載のCo若しくはCo合金相に酸化物相を分散させたスパッタリングターゲット。
- 相対密度を98%以上であることを特徴とする請求項1~3のいずれか一項に記載のCo若しくはCo合金相に酸化物相を分散させたスパッタリングターゲット。
- Coを含有する金属マトリックス相、6~14mol%のSiO2を含有する酸化物相及び0.3mol%以上、1.0mol%未満のCr酸化物からなることを特徴とする非磁性材粒子分散型磁性体薄膜。
- 前記金属マトリックス相が、Co金属単独であるか、Cr:6~40mol%であり、残部がCoからなるCo基合金であるか、又はCr:6~40mol%、Pt:8~20mol%であり、残部がCoからなるCo基合金であることを特徴とする請求項5記載の非磁性材粒子分散型磁性体薄膜。
- 比抵抗が3.5×1016Ω・cm以下であることを特徴とする請求項5又は6記載の非磁性材粒子分散型磁性体薄膜。
- 請求項5~7のいずれか一項に記載の非磁性材粒子分散型磁性体薄膜を用いた磁気記録媒体。
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US13/513,898 US20120241317A1 (en) | 2009-12-11 | 2010-10-13 | Sputtering Target Comprising Oxide Phase Dispersed in Co or Co Alloy Phase, Magnetic Thin Film Made of Co or Co Alloy Phase and Oxide Phase, and Magnetic Recording Medium Using the Said Thin Film |
CN201080056252.6A CN102656290B (zh) | 2009-12-11 | 2010-10-13 | 在Co或Co合金相中分散有氧化物相的溅射靶、包含Co或Co合金相和氧化物相的磁性体薄膜及使用该磁性体薄膜的磁记录介质 |
JP2011513558A JP4837801B2 (ja) | 2009-12-11 | 2010-10-13 | Co若しくはCo合金相に酸化物相を分散させたスパッタリングターゲット |
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CN104145042A (zh) * | 2012-02-22 | 2014-11-12 | 吉坤日矿日石金属株式会社 | 磁性材料溅射靶及其制造方法 |
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JPWO2013136962A1 (ja) * | 2012-03-15 | 2015-08-03 | Jx日鉱日石金属株式会社 | 磁性材スパッタリングターゲット及びその製造方法 |
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WO2020044573A1 (ja) * | 2018-08-31 | 2020-03-05 | Jx金属株式会社 | 安定的に放電可能なスパッタリングターゲット |
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Also Published As
Publication number | Publication date |
---|---|
US20120241317A1 (en) | 2012-09-27 |
JPWO2011070850A1 (ja) | 2013-04-22 |
JP4837801B2 (ja) | 2011-12-14 |
CN102656290B (zh) | 2014-11-26 |
TWI496905B (zh) | 2015-08-21 |
TW201125993A (en) | 2011-08-01 |
MY149640A (en) | 2013-09-13 |
CN102656290A (zh) | 2012-09-05 |
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