CN114959599A - Sputtering target for forming magnetic recording film and method for producing same - Google Patents

Sputtering target for forming magnetic recording film and method for producing same Download PDF

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CN114959599A
CN114959599A CN202210426425.3A CN202210426425A CN114959599A CN 114959599 A CN114959599 A CN 114959599A CN 202210426425 A CN202210426425 A CN 202210426425A CN 114959599 A CN114959599 A CN 114959599A
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powder
sputtering target
sputtering
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alloy
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荻野真一
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JX Nippon Mining and Metals Corp
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C5/00Alloys based on noble metals
    • C22C5/04Alloys based on a platinum group metal
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • GPHYSICS
    • G11INFORMATION STORAGE
    • G11BINFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/84Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/851Coating a support with a magnetic layer by sputtering
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00Thin magnetic films, e.g. of one-domain structure
    • H01F10/08Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
    • H01F10/10Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
    • H01F10/12Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
    • H01F10/14Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/14Apparatus 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
    • H01F41/18Apparatus 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Physical Vapour Deposition (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Powder Metallurgy (AREA)
  • Magnetic Record Carriers (AREA)

Abstract

The present invention relates to a sputtering target for forming a magnetic recording film and a method for producing the same. A FePt-based sintered sputtering target containing C and/or BN, characterized in that the area ratio of AuCu alloy particles in a polished surface of a cross section perpendicular to the sputtering surface of the target is 0.5% or more and 15% or less. The present invention addresses the problem of providing a sputtering target which can reduce particles generated during sputtering and can efficiently form a magnetic thin film of a magnetic recording medium.

Description

Sputtering target for forming magnetic recording film and method for producing same
The application is a divisional application of Chinese patent application with application number 201580051739.8 and application date 2015, 9 and 18.
Technical Field
The present invention relates to a ferromagnetic material sputtering target used for forming a magnetic thin film of a magnetic recording medium, particularly for forming a magnetic recording layer of a thermally assisted magnetic recording medium, and relates to a FePt-based sintered body sputtering target which can obtain stable discharge and generates few particles when sputtered by a magnetron sputtering apparatus.
Background
In the field of magnetic recording media represented by HDDs (hard disk drives), materials based on Co, Fe, or Ni, which are ferromagnetic metals, are used as materials of magnetic thin films for recording. For example, a Co-Cr-based or Co-Cr-Pt-based ferromagnetic alloy containing Co as a main component has been used for a recording layer of a hard disk adopting an in-plane magnetic recording system. In addition, a composite material containing a Co — Cr — Pt-based ferromagnetic alloy containing Co as a main component and nonmagnetic inorganic particles is often used for a recording layer of a hard disk employing a perpendicular magnetic recording system which has been put into practical use in recent years. In addition, from the viewpoint of high productivity, a magnetic thin film of a magnetic recording medium such as a hard disk is often produced by sputtering using a ferromagnetic material sputtering target containing the above-described material as a component.
On the other hand, the recording density of magnetic recording media has been rapidly increasing year by year, and it is considered that the areal density of 100 gigabits (Gbit)/square inch will reach 1 trillion bits (Tbit)/square inch in the future. When the recording density reaches trillion bits per square inch, the size of the recording bits (bits) is less than 10nm, in which case the superparamagnetic formation caused by thermal fluctuation is expected to be a problem, and the magnetic recording medium currently used, such as a material in which the crystal magnetic anisotropy is improved by adding Pt to a Co — Cr-based alloy, or a medium in which the magnetic coupling between magnetic particles is weakened by further adding B thereto, is expected to be insufficient. This is because particles stably exhibiting ferromagnetic properties in a size of 10nm or less are required to have higher crystal magnetic anisotropy.
In view of the above, L1 is provided 0 The FePt phase having a structure has attracted attention as a material for an ultra-high density recording medium. Further, has L1 0 The structured FePt phase is excellent in corrosion resistance and oxidation resistance, and thereforeMaterials suitable for use as recording media are expected. The FePt phase has an order-disorder transition temperature of 1573K, and generally has L1 due to rapid ordering reaction even when the alloy is quenched from high temperature 0 And (5) structure. Further, when the FePt phase is used as a material for an ultra-high density recording medium, it is required to develop a technique for uniformly dispersing the ordered FePt phase in a magnetically isolated state at a density as high as possible and in a uniform orientation. In view of such circumstances, it has been proposed to use a nonmagnetic material to provide L1 0 A granular structure magnetic thin film obtained by magnetically separating a FePt magnetic phase of the structure is used as a magnetic recording medium for a next-generation hard disk using a heat-assisted magnetic recording system.
The granular structure magnetic film is formed into the following structure: the magnetic particles are magnetically insulated from each other by the insertion of the non-magnetic substance. The magnetic recording layer is composed of a magnetic phase such as FePt alloy and a nonmagnetic phase for separating the magnetic phases, and C, BN is known to be effective as a material of the nonmagnetic phase. In the case of forming such a magnetic thin film, a FePt alloy sputtering target containing C is generally used, instead of using a plurality of targets of a C target and a FePt alloy target (for example, patent documents 1 to 2). The present inventors have previously made inventions relating to a sputtering target for forming a FePt-based magnetic recording film containing C (patent document 3) and a sputtering target for forming a FePt-based magnetic recording film containing BN (patent document 4).
The FePt-based sputtering target containing C, BN is generally produced by a powder sintering method. However, since the thermal expansion coefficient of C, BN is too small compared to the FePt alloy, the compressive stress applied to C, BN increases as the sintering temperature increases, and as a result, C, BN may cause physical defects and cause generation of particles during sputtering. On the other hand, when the sintering temperature is too low, the density of the target becomes low, and there is a problem that this causes generation of particles.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 2012 and 102387
Patent document 2: japanese laid-open patent publication No. 2012 and 214874
Patent document 3: international publication WO2014/013920
Patent document 4: international publication WO2014/065201
Patent document 5: japanese patent No. 5041261
Patent document 6: japanese patent No. 5041262
Disclosure of Invention
Problems to be solved by the invention
The present invention provides a FePt-based sintered sputtering target for forming a magnetic recording layer, which sputtering target is composed of a magnetic phase such as a FePt-based alloy and a nonmagnetic phase for separating the magnetic phase, wherein C and/or BN is used as a material of the nonmagnetic phase.
Means for solving the problems
As a result of intensive studies to solve the above problems, the present inventors have found that by adding an AuCu alloy having a low melting point as a sintering aid to raw materials, the density of a target can be increased even at a sintering temperature lower than that of the conventional art, and as a result, the generation of particles during sputtering due to the defect of C, BN and the decrease in density can be reduced.
Based on such findings, the present invention provides:
1) a FePt-based sintered sputtering target containing C and/or BN, characterized in that the area ratio of AuCu alloy particles in a polished surface of a cross section perpendicular to the sputtering surface of the target is 0.5% or more and 15% or less.
2) The sputtering target according to 1) above, wherein the total content of Au and Cu is 1 to 20 mol% based on the composition of the entire sputtering target.
3) The sputtering target according to the above 2), wherein the content ratio of Cu to Au in the sputtering target is 20 to 80 mol%.
4) The sputtering target according to any one of the above 1) to 3), wherein the content of Pt is 30 to 70 mol% based on the composition of the entire sputtering target.
5) The sputtering target according to any one of the above 1) to 4), wherein the content of C is 5 to 50 mol% based on the composition of the entire sputtering target.
6) The sputtering target according to any one of the above 1) to 5), wherein the BN content is 5 to 40 mol% based on the composition of the entire sputtering target.
7) The sputtering target according to any one of the above 1) to 6), characterized by containing 0.1 to 20 mol% of one or more metal oxides selected from the group consisting of Y, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Fe, Co, Ni, Al, Ga and Si, based on the composition of the entire sputtering target.
8) The sputtering target according to any one of the above 1) to 7), wherein the density of the sputtering target is 95% or more.
Effects of the invention
The FePt-based sintered sputtering target containing C and/or BN according to the present invention has an excellent effect of significantly reducing the amount of particles generated during sputtering. Further, the magnetic thin film of the magnetic recording medium, particularly the granular magnetic recording layer, can be efficiently formed.
Drawings
Fig. 1 shows a laser microscope image and a binarized image of the sintered body of example 1.
FIG. 2 is an elemental distribution diagram of the sintered body of example 1 obtained by using FE-EPMA.
Detailed Description
In general, the lower the melting point of the metal material, the lower the softening temperature, so that by adding a material having a low melting point as a sintering aid, the density of the sintered body can be increased even at a low sintering temperature. As a metal of the sintering aid added to the FePt-based sintered compact sputtering target, it is known to add Au, Ag, or Cu separately.
The present inventors have focused on that an AuCu alloy containing Au (melting point: 1064.4 ℃ C.) and Cu (melting point: 1064.6 ℃ C.) has its melting point lowered to 910 ℃ due to eutectic reaction, and found that a sintered body of high density can be obtained even at a lower sintering temperature by using it as a sintering aid. In the present invention, the term "AuCu alloy" refers to an alloy having a composition range (Au: 20 to 80 atomic%) in which a liquid phase of the alloy appears at 910 ℃ in an Au-Cu binary phase diagram.
It has been known to add Ag, Cu, or the like to a FePt-based alloy sputtering target (for example, patent documents 3 to 6). However, these are not added as sintering aids for the purpose of improving magnetic properties, and are added by adding Ag or Cu alone, or an AgPt alloy or a CuPt alloy, but not by adding an AuCu alloy having a low melting point. In particular, patent documents 5 to 6 describe: by mixing pure Au powder, AuPt alloy powder having a high melting point of pure Cu powder, and CuPt alloy powder, the sintering temperature can be increased, and a high-density target can be obtained.
Based on the above findings, the present invention is characterized in that, in a FePt-based sintered compact sputtering target containing C and/or BN, the area ratio of AuCu alloy particles in a polished surface of a cross section perpendicular to the sputtering surface of the target is 0.5% or more and 15% or less. The FePt-based sintered sputtering target containing C and/or BN according to the present invention has a structure in which nonmagnetic material particles of C and/or BN are dispersed in a ferromagnetic material made of a FePt-based alloy. The reason why the structure in the vertical cross section is defined is that C, BN used as a raw material has a sheet-like form, and therefore, when hot pressing is performed by uniaxial pressing, the appearance of the structure differs between the vertical cross section and the horizontal cross section. In this case, the vertical cross section is defined because it looks like a layer of a characteristic stratum.
In the observation of the AuCu alloy particles, a cross section perpendicular to the sputtering surface of the sputtering target was mirror-polished until the AuCu alloy particles could be distinguished, and arbitrary 10 sites of the sputtering target were observed within a field of view of 60 μm × 80 μm using a laser microscope to determine their average area ratio. In addition, sandpaper of SiC abrasive grains is used for polishing. For the sandpaper, sandpaper having a grain size of #240, #400, #600, #1000(JIS R6010) was used for polishing in this order. Then, as a finish, wet polishing was performed using alumina abrasive grains having a grain size of 0.3 μm. The area ratio is calculated as follows.
First, a laser microscope (VK-9710, K.K., 20 times the objective lens and 1 time the digital zoom) was used to take a laser microscope image of a vertical cross section of the target (field: 60 μm in the vertical direction and 80 μm in the horizontal direction). Subsequently, elemental analysis was performed by FE-EPMA at the same site as the laser microscope image, and the AuCu alloy was identified. In this case, in the FE-EPMA image, particles detected at the same sites as Au and Cu were identified as AuCu alloy particles. Since the AuCu alloy particles (alloy phases) are imaged so as to be darker in color than the FePt-based alloy phase and brighter in color than the C phase and the BN phase, only the AuCu alloy phase can be binarized and digitally distinguished by utilizing the difference in contrast. In addition, in the case where an oxide is added, the oxide phase is imaged darker than the AuCu alloy particles, like the C phase and the BN phase, and therefore, in this case, it can be easily distinguished by a contrast difference. Thus, the area ratio of the AuCu alloy particles was calculated from the binarized data. In the case of binarization, since the probability of noise is high when the area is 100 pixels or less, the values thereof are not included in the binarized data.
In the sputtering target of the present invention, the total content of Au and Cu is preferably set to 1 to 20 mol% based on the entire composition of the sputtering target. When the total content of Au and Cu is less than 1 mol%, the effect as a sintering aid by the addition of the AuCu alloy cannot be sufficiently obtained, and therefore, the density of the sintered body (sputtering target) cannot be increased, and particles are likely to be generated, which is not preferable. On the other hand, if the total content of Au and Cu is more than 20 mol%, it is difficult to control the characteristics of the magnetic thin film formed by sputtering, which is not preferable.
In the sputtering target of the present invention, the content ratio of Cu to Au in the sputtering target is preferably set to 20 to 80 mol%. When the content ratio of Cu to Au is less than 20 mol% or more than 80 mol%, the effect of lowering the melting point of the AuCu alloy cannot be sufficiently obtained, the density of the sintered body (sputtering target) cannot be increased, and particles are likely to be generated, which is not preferable.
In the present invention, the Pt content is preferably set to 30 mol% or more and 70 mol% or less with respect to the composition of the entire sputtering target. By setting the Pt content to 30 mol% or more and 70 mol% or less, good magnetic properties can be obtained. Further, the magnetic insulation can be improved by setting the C content as the nonmagnetic material to 5 mol% or more and 50 mol% or less and the BN content to 5 mol% or more and 40 mol% or less with respect to the composition of the entire sputtering target. The total content of C and BN is preferably set to 3 vol% or more and 50 vol% or less. By setting these numerical ranges, magnetic insulation can be improved while suppressing particles during sputtering.
In the present invention, it is preferable that the sputtering target contains 0.1 to 20 mol% of each of at least one metal oxide selected from the group consisting of Y, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Fe, Co, Ni, Al, Ga, and Si with respect to the composition of the entire sputtering target. These oxides are effective components for improving the magnetic properties of the sputtered film. In the FePt-based sintered sputtering target of the present invention, the balance is Fe, in addition to Pt, C and/or BN, AuCu, and the above-described oxides. For these components, the respective contents can be determined by an ICP (inductively coupled plasma) -OES method.
The density of the sputtering target of the present invention is preferably 95% or more. This reduces the occurrence of abnormal discharge (arc discharge) during film formation, and enables the production of a uniform thin film. The relative density in the present invention is a value obtained by dividing the measured density of the target by the calculated density (also referred to as theoretical density). The calculated density is a density when the components of the target are assumed to be present in a mixed state without diffusing or reacting with each other, and is calculated by the following formula.
Formula (II): the calculated density ∑ (molecular weight of constituent component × atomic weight ratio of constituent component)/Σ (molecular weight of constituent component × atomic weight ratio of constituent component/literature value density of constituent component). Here, Σ means the sum over all the constituent components of the target.
The FePt-based sintered compact sputtering target of the present invention can be produced by the following method.
First, each raw material powder (Fe powder, Pt powder, C powder, BN powder, AuCu alloy powder) was prepared. As the raw material powder, alloy powder (Fe — Pt powder) obtained by alloying in advance by a heat treatment or an atomizing device can be used. The alloy powder containing Pt is effective for reducing the amount of oxygen in the raw material powder, although it depends on the composition thereof. In addition, instead of the AuCu alloy powder, Au powder and Cu powder may be used, respectively, and alloyed in sintering. Further, each raw material powder of the metal oxides listed above was prepared as necessary.
Next, the metal powder (Fe powder, Pt powder, Fe — Pt alloy powder) is pulverized by a ball mill, a media-stirring mill, or the like. In general, as the raw material powder of such a metal, a powder having a spherical shape, a block shape, or other indefinite shape can be used, but the shape can be made into a flake shape by pulverizing the powder using a ball mill or a media-stirring mill. By using such a flaky powder, a layered structure is formed in the vertical cross-sectional direction of the sintered body, and the crystal orientation of the Fe — Pt alloy phase is stabilized, contributing to stabilization of discharge. The average particle diameter of each of these raw material powders is preferably 10 to 100. mu.m.
Then, the raw material powders are weighed to obtain a desired composition, and the metal powder obtained by the pulverization treatment and the AuCu alloy powder, C powder, and/or BN powder are mixed using a mortar, a media-stirring mill, a sieve, or the like. The oxide as an additive component may be added together with the raw material powder of the metal, or may be added together with the C powder and the BN powder, or may be added at a stage of mixing the raw material powder of the metal with the C powder and the BN powder.
Then, the mixed powder is molded and sintered by hot pressing. In addition to hot pressing, a spark plasma sintering method or a hot isostatic sintering method may be used. The holding temperature during sintering is, in many cases, in the range of 850 ℃ to 900 ℃, although it depends on the composition of the sputtering target. Conventionally, sintering was carried out at a temperature ranging from 800 ℃ to 1400 ℃ in order to increase the density, but according to the present invention, a high density equivalent to that of the conventional one can be achieved at a relatively low sintering temperature.
Next, the sintered body taken out of the hot press is subjected to Hot Isostatic Pressing (HIP). Hot press working or the like is effective for increasing the density of the sintered body. The holding temperature during the pressing process such as heating depends on the composition of the sintered body, but is usually set to a temperature range of 850 to 900 ℃. Conventionally, in order to increase the density, press working such as heating is performed at a temperature range of 800 to 1200 ℃ in the same manner as hot pressing, but according to the present invention, a high density equivalent to that of the conventional art can be achieved at a relatively low sintering temperature.
The sintered body obtained in this manner is machined into a desired shape by a lathe or the like, whereby the sputtering target of the present invention can be produced. By the above method, a high-density (particularly, a density of 95% or more) sputtering target, which is a FePt-based sintered compact sputtering target containing C and/or BN, can be produced.
Examples
The following description will be made based on examples and comparative examples. It should be noted that the present embodiment is only an example, and the present invention is not limited to the example at all. That is, the present invention is limited only by the claims and includes various modifications other than the embodiments included in the present invention.
Example 1
FePt alloy powder, C powder, and AuCu alloy powder were prepared as raw material powders, and these powders were weighed so as to attain 60(45Fe-45Pt-5Au-5Cu) -40C (mol%).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder taken out of the media agitation mill, the AuCu alloy powder, and the C powder were mixed by a V-type mixer, and then mixed by a sieve of 150 μm mesh, and the mixed powder was filled into a carbon mold and hot-pressed.
The hot pressing conditions were set to vacuum atmosphere, heating rate 300 ℃/h, holding temperature 850 ℃, holding time 2 h, and pressurization was performed at 30MPa from the start of heating to the end of holding. After the holding is finished, the chamber is directly cooled naturally.
Next, the sintered body taken out of the die of the hot press is subjected to a pressing process such as heating. The conditions for the press working such as heat were set to a temperature raising rate of 300 ℃/h, a holding temperature of 850 ℃ and a holding time of 2 hours, and the pressure of Ar gas was gradually raised from the start of the temperature raising and the press working was carried out at 150MPa while the press working was held at 850 ℃. After the holding, the steel plate is directly cooled naturally in the furnace.
The end portion (corresponding to a cross section perpendicular to the sputtering surface) of the sintered body obtained in this manner was cut, mirror-polished, and then the polished surface was observed with a laser microscope. The microscope image thereof is shown in the left image of fig. 1. In this figure, the dark gray region corresponds to the AuCu alloy particles. Then, the area ratio (average) of the AuCu alloy particles was obtained by binarizing the result. The result was 10.8%. It was confirmed that these particles contained the AuCu alloy using the FE-EPMA image (see fig. 2). The density of the other end portion of the sintered body was measured by the archimedes method, and found to be 95.8%.
Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. Sputtering conditions were set to 1kW of input power and 1.7Pa of Ar gas pressure, 2kWh of pre-sputtering was performed, and then film formation was performed on a silicon substrate having a diameter of 4 inches for 20 seconds. Then, the number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter. The number of particles in this case was 65.
Figure BDA0003609803080000111
Comparative example 1
FePt alloy powder, C powder, and Au powder were prepared as raw material powders, and these powders were weighed to achieve 60(45Fe-45Pt-10Au) -40C (mol%).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder taken out of the medium stirring mill, the Au powder and the C powder were mixed by a V-type mixer, and then mixed by a sieve having a 150 μm mesh, and the mixed powder was filled in a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 93.2%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and the number of particles was increased to 184 as compared with the examples.
Comparative example 2
FePt alloy powder, C powder, and Cu powder were prepared as raw material powders, and these powders were weighed to achieve 60(45Fe-45Pt-10Cu) -40C (mol%).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder taken out of the media agitation mill, the Cu powder and the C powder were mixed by a V-shaped mixer, and then mixed by a sieve of 150 μm mesh, and the mixed powder was filled into a carbon mold and hot pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 93.5%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 179 compared with the example.
Comparative example 3
FePt alloy powder and C powder were prepared as raw material powders, and these powders were weighed so as to attain 60(50Fe-50Pt) -40C (mol%).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder taken out of the media-stirring mill and the C powder were mixed by a V-type mixer, and then mixed by a sieve having a 150 μm mesh, and the mixed powder was filled in a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 92.8%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 261 more than in the examples.
Example 2
Fe powder, Pt powder, BN powder, and AuCu alloy powder were prepared as raw material powders, and these powders were weighed so as to attain 66(54Fe-40Pt-3Au-3Cu) -34BN (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the media agitation mill, the AuCu alloy powder, and the BN powder were mixed by a V-type mixer, and then mixed by a sieve of 150 μm mesh, and the mixed powder was filled into a carbon mold and hot pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The sintered body thus obtained was cut at its end (corresponding to a cross section perpendicular to the sputtering surface), mirror-polished, and the polished surface was observed with a laser microscope, whereby the area ratio of the AuCu alloy particles was 2.4%. The density of the other end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 95.4%. Next, sputtering was performed using this sintered body under the same conditions as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was 94.
Comparative example 4
Fe powder, Pt powder, BN powder, and Au powder were prepared as raw material powders, and these powders were weighed so as to obtain 66(54Fe-40Pt-6Au) -34BN (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the media-stirring mill, the Ag powder and the BN powder were mixed by a V-type mixer, and then mixed by a sieve of 150 μm mesh, and the mixed powder was filled into a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 93.9%. The sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 256 particles as compared with example 2.
Example 3
Fe powder, Pt powder, C powder, Au powder, and Cu powder were prepared as raw material powders, and these powders were weighed so as to be 50(60Fe-30Pt-1.5Au-8.5Cu) -50C (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the media agitation mill, the Au powder, the Cu powder, and the C powder were mixed by a V-shaped mixer, and then mixed by a sieve of 150 μm mesh, and the mixed powder was filled into a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The sintered body thus obtained was cut at its end (corresponding to a cross section perpendicular to the sputtering surface), mirror-polished, and the polished surface was observed with a laser microscope, whereby the area ratio of the AuCu alloy particles was 4.8%. The density of the other end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 95.1%. Next, sputtering was performed using this sintered body under the same conditions as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was 82.
Comparative example 5
Fe powder, Pt powder, C powder, and Au powder were prepared as raw material powders, and these powders were weighed to 50(60Fe-30Pt-10Au) -50C (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the media agitation mill, the Au powder and the C powder were mixed by a V-shaped mixer, and then mixed by a sieve of 150 μm mesh, and the mixed powder was filled into a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 93.3%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 439 in comparison with example 3.
Example 4
As raw material powders, Fe powder, Pt powder, BN powder, Au powder, and Cu powder were prepared, and these powders were weighed so as to attain 80(20Fe-70Pt-9Au-1Cu) -20BN (mol%).
Subsequently, the Fe powder and Pt powder were charged into a 5L media-agitating mill together with pulverized media zirconium balls, and treated at a rotation speed of 300rpm for 2 hours. Then, the powder taken out of the media agitation mill, the Ag powder, the Cu powder, and the BN powder were mixed by a V-type mixer, and then mixed by a sieve of 150 μm mesh, and the mixed powder was filled into a carbon mold and hot pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The sintered body thus obtained was cut at its end (corresponding to a cross section perpendicular to the sputtering surface), mirror-polished, and the polished surface was observed with a laser microscope, whereby the area ratio of the AuCu alloy particles was 9.7%. The density of the other end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 96.0%. Next, sputtering was performed using this sintered body under the same conditions as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was 83.
Comparative example 6
As raw material powders, Fe powder, Pt powder, BN powder, and Cu powder were prepared, and these powders were weighed so as to attain 80(20Fe-70Pt-10Cu) -20BN (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the media agitation mill, the Cu powder, and the BN powder were mixed by a V-type mixer, and then mixed by a sieve having a 150 μm mesh, and the mixed powder was filled in a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 93.2%. Then, the sintered body was cut into a shape of 180.0mm in diameter and 5.0mm in thickness by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 307 particles as compared with example 4.
Example 5
As raw material powders, Fe powder, Pt powder, C powder, AuCu powder, and SiO powder were prepared 2 Powders weighed to achieve 77(35Fe-45Pt-10Au-10Cu) -8SiO 2 -15C (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the medium stirring mill, AuCu alloy powder, and SiO 2 The powder and the C powder were mixed by a V-type mixer, and then mixed by a sieve having a 150 μm mesh, and the mixed powder was filled in a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The sintered body thus obtained was cut at its end (corresponding to a cross section perpendicular to the sputtering surface), mirror-polished, and the polished surface was observed with a laser microscope, whereby the area ratio of the AuCu alloy particles was 14.3%. The density of the other end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 97.1%. Next, sputtering was performed using this sintered body under the same conditions as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, 47 particles were present.
Comparative example 7
As the raw material powder, Fe powder, Pt powder, C powder, Au powder, and SiO powder were prepared 2 Powders weighed to 77(35Fe-45Pt-20Au) -8SiO 2 15C (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the medium stirring mill, Au powder, SiO 2 The powder and the C powder were mixed by a V-type mixer, and then mixed by a sieve having a 150 μm mesh, and the mixed powder was filled in a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 93.6%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 142 as compared with example 5.
Example 6
As raw material powders, Fe powder, Pt powder, C powder, AuCu powder, TiO powder were prepared 2 Powder of Cr 2 O 3 Powders weighed to achieve 73(53Fe-45Pt-1Au-1Cu) -1TiO 2 -1Cr 2 O 3 -25C (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the medium stirring mill is subjected to,AuCu alloy powder, TiO 2 Powder of Cr 2 O 3 The powder and the C powder were mixed by a V-shaped mixer, and then mixed by a sieve having a 150 μm mesh, and the mixed powder was filled in a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The sintered body thus obtained was cut at its end (corresponding to a cross section perpendicular to the sputtering surface), mirror-polished, and the polished surface was observed with a laser microscope, whereby the area ratio of the AuCu alloy particles was 0.8%. Further, the other end portion of the sintered body obtained in this manner was measured for density by the archimedes' method, and found to be 96.2%. Next, sputtering was performed using this sintered body under the same conditions as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was 59.
Comparative example 8
Fe powder, Pt powder, C powder, Au powder, TiO powder, etc. were prepared as raw material powders 2 Powder of Cr 2 O 3 Powders weighed to achieve 73(53Fe-45Pt-2Au) -1TiO 2 -1Cr 2 O 3 -25C (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder, Ag powder, TiO powder taken out of the media-stirring mill 2 Powder of Cr 2 O 3 The powder and the C powder were mixed by a V-type mixer, and then mixed by a sieve having a 150 μm mesh, and the mixed powder was filled in a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 92.9%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 227 in comparison with example 6.
Example 7
FePt alloy powder, BN powder, Au powder, Cu powder, MnO powder, Ta powder were prepared as raw material powders 2 O 5 Powders weighed to achieve 78.5(45Fe-45Pt-4Au-6Cu) -0.5MnO-1Ta 2 O 5 -20BN (mol%).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder, Au powder, Cu powder, MnO powder, Ta powder, etc. taken out of the medium stirring mill are mixed 2 O 5 The powder and BN powder were mixed by a V-shaped mixer, and then mixed by a 150 μm mesh sieve, and the mixed powder was filled into a carbon mold and hot pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The sintered body thus obtained was cut at its end (corresponding to a cross section perpendicular to the sputtering surface), mirror-polished, and the polished surface was observed with a laser microscope, whereby the area ratio of the AuCu alloy particles was 6.1%. The density of the other end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 95.2%. Next, sputtering was performed using this sintered body under the same conditions as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and the number of particles was 97.
Comparative example 9
FePt alloy powder, BN powder, Cu powder, MnO powder, Ta powder were prepared as raw material powders 2 O 5 Powders weighed to achieve 78.5(45Fe-45Pt-10Cu)-0.5MnO-1Ta 2 O 5 -20BN (% by mole).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder taken out of the medium stirring mill, Cu powder, MnO powder, Ta powder 2 O 5 The powder and BN powder were mixed by a V-shaped mixer, and then mixed by a 150 μm mesh sieve, and the mixed powder was filled into a carbon mold and hot pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 94.0%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 398 pieces compared with example 7.
Example 8
FePt alloy powder, C powder, AuCu alloy powder, and SiO were prepared as raw material powders 2 Powders were weighed to achieve 80(45Fe-45Pt-5Au-5Cu) -15SiO 2 -5C (mol%).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder taken out of the medium stirring mill, AuCu alloy powder, and SiO 2 The powder and the C powder were mixed by a V-shaped mixer, and then mixed by a sieve having a 150 μm mesh, and the mixed powder was filled in a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The sintered body thus obtained was cut at its end (corresponding to a cross section perpendicular to the sputtering surface), mirror-polished, and the polished surface was observed with a laser microscope, whereby the area ratio of the AuCu alloy particles was 7.2%. The density of the other end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 97.3%. Next, sputtering was performed under the same conditions as in example 1 using this sintered body. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and the number of particles was 13.
Comparative example 10
FePt alloy powder, C powder, Au powder, and SiO powder were prepared as raw material powders 2 Powders weighed to achieve 80(45Fe-45Pt-10Au) -15SiO 2 -5C (mol%).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder, Au powder, and SiO powder taken out of the medium stirring mill were mixed 2 The powder and the C powder were mixed by a V-shaped mixer, and then mixed by a sieve having a 150 μm mesh, and the mixed powder was filled in a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 92.2%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle size of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 285 particles considerably as compared with example 8.
Example 9
FePt alloy powder, BN powder, Au powder, Cu powder, and SiO were prepared as raw material powders 2 Powders, which were weighed to reach 85(45 Fe)-45Pt-4Au-6Cu)-10SiO 2 -5BN (mol%).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder, Ag powder, Cu powder, SiO taken out of the medium stirring mill 2 The powder and BN powder were mixed by a V-shaped mixer, and then mixed by a 150 μm mesh sieve, and the mixed powder was filled into a carbon mold and hot pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The sintered body thus obtained was cut at its end (corresponding to a cross section perpendicular to the sputtering surface), mirror-polished, and the polished surface was observed with a laser microscope, whereby the area ratio of the AuCu alloy particles was 5.9%. The density of the other end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 97.0%. Next, sputtering was performed using this sintered body under the same conditions as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was 31.
Comparative example 11
FePt alloy powder, BN powder, Cu powder, and SiO powder were prepared as raw material powders 2 Powders weighed to achieve 85(45Fe-45Pt-10Cu) -10SiO 2 -5BN (mol%).
Next, the FePt alloy powder was charged into a 5L capacity media agitator mill together with crushed media zirconium balls and treated at 300rpm for 2 hours. Then, the powder taken out of the medium stirring mill, Cu powder, and SiO 2 The powder and BN powder were mixed by a V-shaped mixer, and then mixed by a 150 μm mesh sieve, and the mixed powder was filled into a carbon mold and hot pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 93.8%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 213 in comparison with example 9.
Example 10
As raw material powders, Fe powder, Pt powder, C powder, BN powder, and AuCu alloy powder were prepared, and these powders were weighed so as to attain 60(50Fe-40Pt-5Au-5Cu) -30C-10BN (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the media agitation mill, the AuCu alloy powder, the C powder, and the BN powder were mixed by a V-type mixer, and then mixed by a sieve of 150 μm mesh, and the mixed powder was filled into a carbon mold and hot-pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The sintered body thus obtained was cut at its end (corresponding to a cross section perpendicular to the sputtering surface), mirror-polished, and the polished surface was observed with a laser microscope, whereby the area ratio of the AuCu alloy particles was 5.5%. The density of the other end portion of the sintered body obtained in this manner was measured by the archimedes method, and found to be 95.9%. Next, sputtering was performed using this sintered body under the same conditions as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was 97.
Comparative example 12
Fe powder, Pt powder, C powder, BN powder, and Au powder were prepared as raw material powders, and these powders were weighed so as to attain 60(50Fe-40Pt-10Au) -30C-10BN (mol%).
Then, the Fe powder and Pt powder were put into a 5L media-agitating mill together with the pulverized media of zirconium balls, and treated at 300rpm for 2 hours. Then, the powder taken out of the media agitation mill, the Ag powder, the C powder, and the BN powder were mixed by a V-type mixer, and then mixed by a sieve of 150 μm mesh, and the mixed powder was filled into a carbon mold and hot pressed under the same conditions as in example 1. Next, the sintered body taken out of the die of the hot press was subjected to press working such as heating under the same conditions as in example 1.
The density of the end portion of the sintered body obtained in this manner was measured by the archimedes method, and the result was 92.7%. Then, the sintered body was cut into a shape having a diameter of 180.0mm and a thickness of 5.0mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA) to perform sputtering. The sputtering conditions were the same as in example 1. The number of particles having a particle diameter of 0.25 μm or more adhering to the substrate was measured by a particle counter, and as a result, the number of particles was increased to 421 more than in example 10.
Industrial applicability
The FePt-based sintered sputtering target containing C and/or BN according to the present invention has an excellent effect of reducing the amount of particles generated during sputtering. Therefore, the ferromagnetic material sputtering target is useful for forming a magnetic thin film of a magnetic recording medium, particularly a granular magnetic recording layer.

Claims (24)

1. A FePt-based sintered sputtering target containing C and/or BN, characterized in that the area ratio of AuCu alloy particles in a polished surface of a cross section perpendicular to the sputtering surface of the target is 0.5% or more and 15% or less.
2. The sputtering target of claim 1 wherein the AuCu alloy is in the composition range where the liquid phase of the alloy appears at 910 ℃ in the Au-Cu binary phase diagram, namely Au: 20 atomic% to 80 atomic% of an alloy.
3. The sputtering target according to claim 1 or 2, wherein the total content of Au and Cu is 1 to 20 mol% based on the composition of the entire sputtering target.
4. The sputtering target according to claim 3, wherein the content ratio of Cu to Au in the sputtering target is 20 to 80 mol%.
5. The sputtering target according to any one of claims 1 to 4, wherein the Pt content is 30 to 70 mol% based on the composition of the entire sputtering target.
6. The sputtering target according to any one of claims 1 to 5, wherein the C content is 5 to 50 mol% based on the composition of the entire sputtering target.
7. The sputtering target according to any one of claims 1 to 6, wherein the BN content is 5 to 40 mol% based on the composition of the entire sputtering target.
8. The sputtering target according to any one of claims 1 to 7, comprising 0.1 to 20 mol% of each of one or more metal oxides selected from the group consisting of Y, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Fe, Co, Ni, Al, Ga and Si based on the composition of the entire sputtering target.
9. The sputtering target according to any one of claims 1 to 8, which is produced by adding an AuCu alloy to a raw material or adding Au and Cu to a raw material and alloying them in sintering.
10. The sputtering target according to any one of claims 1 to 9, which is produced by sintering a raw material powder at 850 to 900 ℃, followed by subjecting the sintered body to a pressure process such as heating at 850 to 900 ℃.
11. The sputtering target according to any one of claims 1 to 10, wherein the density of the sputtering target is 95% or more.
12. The sputtering target according to any one of claims 1 to 11, wherein the density of the sputtering target is 97.0% or more.
13. A method for producing a FePt-based sintered sputtering target containing C and/or BN, characterized by adding an AuCu alloy to a raw material or adding Au and Cu to a raw material and alloying the mixture during sintering so that the area ratio of AuCu alloy particles in a polished surface of a cross section perpendicular to a sputtering surface of the target is 0.5% or more and 15% or less.
14. The production method according to claim 13, wherein the raw material powder is sintered at 850 to 900 ℃, and then the sintered body is subjected to a press working such as heating at 850 to 900 ℃.
15. The manufacturing method according to claim 13 or 14, wherein the AuCu alloy refers to a composition range in which a liquid phase of the alloy appears at 910 ℃ in a binary phase diagram of Au — Cu, that is, Au: 20 atomic% to 80 atomic% of an alloy.
16. The production method according to any one of claims 13 to 15, wherein the total content of Au and Cu is 1 to 20 mol% based on the composition of the entire sputtering target.
17. The manufacturing method according to claim 16, wherein the content ratio of Cu to Au in the sputtering target is 20 to 80 mol%.
18. The production method according to any one of claims 13 to 17, wherein the Pt content is 30 to 70 mol% based on the composition of the entire sputtering target.
19. The production method according to any one of claims 13 to 18, wherein the C content is 5 to 50 mol% based on the composition of the entire sputtering target.
20. The production method according to any one of claims 13 to 19, wherein the BN content is 5 to 40 mol% based on the composition of the entire sputtering target.
21. The production method according to any one of claims 13 to 20, wherein the sputtering target contains 0.1 to 20 mol% of one or more metal oxides selected from the group consisting of Y, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Fe, Co, Ni, Al, Ga, and Si, respectively, based on the composition of the entire sputtering target.
22. The production method according to any one of claims 13 to 21, wherein the density of the sputtering target is 95% or more.
23. The production method according to any one of claims 13 to 22, wherein the density of the sputtering target is 97.0% or more.
24. A method for reducing the amount of particles generated during sputtering, characterized in that sputtering is performed using the sputtering target according to any one of claims 1 to 12 or the sputtering target produced by the production method according to any one of claims 13 to 23.
CN202210426425.3A 2014-09-26 2015-09-18 Sputtering target for forming magnetic recording film and method for producing same Pending CN114959599A (en)

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