TWI616548B - Fe-Pt series sintered body sputtering target and manufacturing method thereof - Google Patents

Abstract

A sintered body sputtering target, which is a Fe-Pt based sintered body sputtering target containing BN, which is characterized in that it is opposite to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the horizontal plane of the sputtering plane. The intensity ratio of the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the cross section of the vertical sputtering surface is 2 or more. An object of the present invention is to provide a sputtering target which can produce a magnetic film of a heat-assisted magnetic recording medium and can reduce the amount of particles generated during sputtering.

Description

Fe-Pt-based sintered body sputtering target and manufacturing method thereof

The present invention relates to a Fe-Pt-based sintered body sputtering target for manufacturing a magnetic thin film in a heat-assisted magnetic recording medium and a method for manufacturing the same.

In the field of magnetic recording represented by hard disk drives, the material of the magnetic thin film in the magnetic recording medium has always been made of Co, Fe or Ni based on ferromagnetic metals. For example, for a magnetic film of a hard disk using a horizontal magnetic recording method, a Co-Cr-based or Co-Cr-Pt-based ferromagnetic alloy containing Co as a main component is used. In addition, for magnetic films of hard disks using a perpendicular magnetic recording method which has been practically used in recent years, a composite material composed of a Co-Cr-Pt-based ferromagnetic alloy containing Co as a main component and non-magnetic inorganic particles is often used. Furthermore, in terms of high productivity, the above-mentioned magnetic thin films are often produced by sputtering a sputtering target using the above-mentioned material as a component using a DC magnetron sputtering device.

Hard disk recording density increases rapidly year by year, think of the future from the current 600Gbit / in ² areal density of the reach 1Tbit / in ^2. If the recording density reaches 1Tbit / in ² , the size of the recording bit will be less than 10nm. It is expected that the superparamagnetization caused by thermal fluctuations will become a problem in this case, and it is expected that the magnetic recording medium used now For example, a material having Pt added to a Co—Cr-based alloy to improve crystal magnetic anisotropy is not sufficient. The reason is that magnetic particles with a size below 10 nm that stably operate with strong magnetism need to have higher crystalline magnetic anisotropy.

For the above reasons, the structure having L1 ₀ FePt phase ultrahigh-density recording medium as a material that attracts attention. Since the FePt phase is not only a high crystalline magnetic anisotropy, but also has excellent corrosion resistance and oxidation resistance, it is expected to be suitable as a material suitable for use as a magnetic recording medium. In the case where the FePt phase is used as a material for an ultra-high-density recording medium, it is required to develop a technique for making regular FePt magnetic particles uniform and dispersed in a direction as high as possible in a magnetically isolated state.

Therefore, a granular structure magnetic film in which FePt magnetic particles having the L1 ₀ structure are isolated by a non-magnetic material such as oxide or carbon has been proposed as a magnetic recording medium for a next-generation hard disk using a thermally-assisted magnetic recording method. use. This granular structure magnetic thin film has a structure in which magnetic particles are magnetically insulated from each other through a non-magnetic substance. Generally, a magnetic film with a granular structure having an Fe-Pt phase is formed by using a Fe-Pt-based sintered body sputtering target.

Regarding the sputtering target of a sintered body of a magnetic material of the Fe-Pt system, the present inventors have previously disclosed a technology regarding a sputtering target of a ferromagnetic material (Patent Document 1): The ferromagnetic material sputtering target is made of Fe A magnetic phase such as a -Pt alloy and a non-magnetic phase separating the same are used, and a metal oxide is used as one of the materials of the non-magnetic phase.

In addition, Patent Document 2 discloses a sputtering palladium for forming a magnetic recording medium film. The sputtering palladium for forming a magnetic recording medium film is composed of a sintered body having a structure in which a C layer is dispersed in an FePt alloy phase. Patent Document 3 discloses a sputtering target for forming a magnetic recording medium film including a SiO ₂ phase, an FePt alloy phase, and an interdiffusion phase. Also, Patent Document 4 discloses an Fe-Pt ferromagnetic material sputtering target composed of Pt, SiO ₂ , Sn, and the remainder is Fe; and Patent Document 5 discloses an X-ray A sputtering target for a magnetic recording film having a peak intensity ratio of the (011) plane of the quartz to the background intensity during diffraction of 1.40 or more.

Hexagonal BN (a compound of boron and nitrogen) as the above-mentioned non-magnetic material has excellent performance as a lubricant, but when it is used as a raw material for powder metallurgy, Poor bonding properties make it difficult to produce high density sintered bodies. In addition, when such a sintered body has a low density, when the sintered body is processed into a target, problems such as cracks or peeling are caused, and the yield is reduced. In addition, if the density is low, there will be a problem that a large number of voids will be generated in the target, and the voids will cause abnormal discharge, resulting in particles (sprayed on the substrate) during the sputtering process. Dust), resulting in reduced product yield.

Patent Document 1: International Publication No. WO2012 / 029498

Patent Document 2: Japanese Patent Application Publication No. 2012-102387

Patent Document 3: Japanese Patent Application Laid-Open No. 2011-208167

Patent Document 4: International Publication No. WO2012 / 086578

Patent Document 5: Japanese Patent No. 5009447

The object of the present invention is to provide a Fe-Pt-based sintered body, which can be used to make a magnetic film of a heat-assisted magnetic recording medium, and uses hexagonal BN as a non-magnetic material, and the present invention provides a method for reducing Particle size sputtering target.

In order to solve the above problems, the present inventors conducted diligent research and found that, because the hexagonal BN of a non-magnetic material has a two-dimensional crystal structure, if the crystal direction of the hexagonal BN in the sintered body is random, the Affects electrical conduction, and causes sputtering to become unstable due to abnormal discharge and the like.

Based on this knowledge, the present invention provides the following inventions: 1) A sintered body sputtering target, which is a Fe-Pt based sintered body sputtering target containing BN, which is characterized in that six of the planes are horizontal to the sputtering surface. X-ray diffraction peak intensity of the crystal BN (002) plane The ratio of the intensity to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the cross section of the vertical sputtering surface is 2 or more; 2) The sintered body sputtering target as described in 1) above, wherein vertical sputtering The average thickness of the hexagonal BN phase in the cross section of the surface is 30 μm or less; 3) The sintered body sputtering target as described in 1) or 2) above, wherein the Pt content is 5 mol% or more and 60 mol% or less; 4) as described in 1 above Sintered body sputtering target according to any one of the above) to 3), wherein the BN content is 1 mol% or more and 60 mol% or less; 5) The sintered body sputtering target according to any one of the above 1) to 4), which contains 0.5 mol% or more and 40.0 mol% or less of one or more elements selected from the group consisting of C, Ru, Ag, Au, Cu as an additive element; 6) A sintered body according to any one of 1) to 5) above Sputtering target, which contains one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides as an additive material; 7) A method for manufacturing a sputtering target, used for manufacturing the above 1) The sputtering target according to any one of 6 to 6), which is a method in which flake-shaped or plate-shaped raw material powders are mixed and formed, and the formed body is subjected to uniaxial Pressure sintering.

The Fe-Pt-based sintered body using BN as a non-magnetic material of the present invention has an excellent effect of suppressing abnormal discharge during sputtering and reducing the amount of particles produced by improving the orientation of hexagonal BN.

[Fig. 1] A microscope photograph of a target (a cross section horizontal to a sputtering surface and a vertical sputtering surface) in Example 1. [Fig.

[Fig. 2] A microscope photograph of a target (a cross section horizontal to a sputtering surface and a vertical sputtering surface) in Example 2. [Fig.

[Fig. 3] A microscope photograph of a target (a cross section horizontal to the sputtering surface and a cross section perpendicular to the sputtering surface) in Example 3. [Fig.

[Fig. 4] A microscope photograph of a target (a cross section horizontal to a sputtering surface and a vertical sputtering surface) of Comparative Example 1. [Fig.

[Fig. 5] An X-ray diffraction waveform chart (the uppermost stage) of the target (the surface that is horizontal to the sputtering surface) in Example 1. [Fig.

[Fig. 6] An X-ray diffraction waveform diagram (the uppermost stage) of the target (section of the vertical sputtering surface) in Example 1. [Fig.

[Fig. 7] An X-ray diffraction waveform chart (the uppermost stage) of the target (the surface that is horizontal to the sputtering surface) in Example 2. [Fig.

[Fig. 8] An X-ray diffraction waveform chart of the target (vertical sputtering surface cross section) of Example 2 (top stage).

[Fig. 9] An X-ray diffraction waveform chart (the uppermost stage) of the target (the surface that is horizontal to the sputtering surface) in Example 3. [Fig.

[Fig. 10] An X-ray diffraction waveform chart of the target (vertical sputtering surface cross section) of Example 3 (top stage).

[Fig. 11] An X-ray diffraction waveform chart (the uppermost stage) of the target (the surface horizontal to the sputtering surface) in Comparative Example 1. [Fig.

[Fig. 12] An X-ray diffraction waveform chart (the uppermost stage) of the target (vertical sputtering surface cross section) of Comparative Example 1. [Fig.

As the non-magnetic material of the hexagonal BN has a two-dimensional crystal structure, if the crystal direction of the hexagonal BN in the target is random, it will affect the electrical conduction and the sputtering will become unstable. Therefore, by aligning the crystal directions of the hexagonal BN, stable sputtering can be performed.

That is, the Fe-Pt-based sintered body sputtering target of the present invention contains hexagonal BN as a non-magnetic material, and X-ray diffraction peak intensity of the hexagonal BN (002) plane in a plane horizontal to the sputtering surface. The intensity ratio of the X-ray diffraction peak intensity with respect to the hexagonal BN (002) plane in the cross section of the vertical sputtering surface is set to 2 or more.

Further, in the Fe-Pt-based sintered body sputtering target of the present invention, it is preferable that the hexagonal BN phase is flaky or plate-shaped, and more preferably that the average thickness of the hexagonal BN phase in the cross section of the vertical sputtering surface is 30 μm or less. Thereby, the influence of electrical conduction caused by hexagonal BN can be reduced, and stable sputtering can be performed.

In the present invention, the Pt content is preferably set to 5 mol% or more and 60 mol% or less. By setting the Pt content to 5 mol% or more and 60 mol% or less, good magnetic properties can be obtained. The content of hexagonal BN is preferably 1 mol% or more and 60 mol% or less. By setting the BN content as a non-magnetic material to be 1 mol% or more and 60 mol% or less, magnetic insulation can be improved.

In addition, in the Fe-Pt-based sintered body sputtering target of the present invention, the remainder is Fe except Pt, hexagonal BN, an additive element or an additive material described later.

In the present invention, the total amount of addition is preferably 0.5 mol% or more and 40.0 mol% or less. One or more elements selected from the group consisting of C, Ru, Ag, Au, and Cu are added as an additional element. In addition, it is preferable to add one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides as an additive material. These added elements or materials are components effective for improving the magnetic properties of the film after sputtering.

The Fe-Pt-based magnetic material sintered body of the present invention can be produced, for example, by the following method.

First, each raw material powder (Fe powder, Pt powder, BN powder) is prepared. Moreover, as a raw material powder, an alloy powder (Fe-Pt powder) can also be used. Although it also depends on its composition, the alloy powder containing Pt can be effectively used to reduce the amount of oxygen in the raw material powder. Furthermore, each raw material powder of the added component disclosed above is prepared as needed.

Next, a metal powder (Fe powder, Pt powder) or an alloy powder (Fe-Pt alloy powder) is pulverized using a ball mill, a media stirring mill, or the like. Generally, the raw material powder of such a metal is spherical, lumpy, or any other shape. However, since hexagonal BN is formed into a plate shape or a flake shape, if these materials are mixed and sintered, it is difficult to form the sintered body. The direction of hexagonal BN is uniform. Therefore, by pulverizing the metal raw material powder and forming it into a plate shape or a sheet shape, a structure such as a metal raw material and hexagonal crystal BN stacked on each other can be formed, and the orientation of the hexagonal crystal BN can be made uniform.

The metal powder or alloy powder obtained by the pulverizing treatment in the above manner is mixed with hexagonal BN powder using a mortar, a media stirring mill, a sieve, or the like. Additives and materials can be added together with the raw material powder of the metal, or with the hexagonal BN powder, or at the stage of mixing the raw material powder of the metal with the hexagonal BN powder.

Then, this mixed powder is shaped and sintered by hot pressing. In addition to hot pressing, A plasma discharge sintering method and a hydrostatic sintering method are used. Although the holding temperature during sintering depends on the composition of the sputtering target, in most cases, it is in the temperature range of 800 to 1400 ° C.

Next, the hot-static pressing process is performed on the sintered body taken out from the auto-pressing. Hot equalizing can effectively increase the density of the sintered body. Although the holding temperature during hot equalizing processing also depends on the composition of the sintered body, in most cases, it is in the temperature range of 800 to 1200 ° C. And the pressure is set above 100MPa. Then, the sintered body obtained in the above manner is processed into a desired shape by a lathe, whereby a sputtering target can be produced.

By the above method, an Fe-Pt-based sintered body sputtering target having the following characteristics can be produced, which includes hexagonal BN and X-ray diffraction around the hexagonal BN (002) plane of the horizontal plane of the sputtering surface. The intensity ratio of the radiation peak intensity to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the cross section of the vertical sputtering surface is 2 or more.

For the evaluation of crystal orientation, the X-ray diffraction intensity of a cross section of a sintered body for a sputtering target with a horizontal surface and a vertical sputtering surface was measured using an X-ray diffraction device under the following measurement conditions. . Device: UltimaIV protectus, manufactured by Rigaku Co., Ltd., tube: Cu, tube voltage: 40kV, tube current: 30mA, scan range (2 θ): 10 ° to 90 °, measurement step width (2 θ): 0.01 ° Scan speed (2 θ): 1 ° per minute, scan mode 2 θ / θ. Furthermore, the diffraction peaks of the hexagonal BN (002) plane appear near (2 θ): 26.75 °.

Hereinafter, it demonstrates based on an Example and a comparative example. In addition, this embodiment is only an example, and is not limited by this example. That is, the present invention is limited only by the scope of the patent application, and includes various modifications other than the embodiments included in the present invention.

(Example 1)

Fe-Pt alloy powder and hexagonal BN powder (flaky) were prepared as raw material powders. These powders are weighed to 70 (50Fe-50Pt) -30BN (mol%).

Next, the Fe-Pt alloy powder and a zirconia ball of a pulverizing medium were put into a 5L medium agitating mill and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the medium stirring mill and the BN powder were mixed with a V-type mixer, and further mixed with a 150 μm mesh sieve, and the mixed powder was filled in a carbon mold and hot-pressed.

The conditions of the hot pressing were a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure of the Ar gas was gradually increased from the beginning of the temperature rise, and the pressure was maintained at 1100 ° C. at 150 MPa. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. The results are shown in Fig. 1. As can be seen from FIG. 1, in the cross-sectional direction of the vertical sputtering surface, a layered structure is formed and BN is oriented. In FIG. 1, the average thickness of the hexagonal BN phase is 3 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 657, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 54. The ratio is 12.2.

Next, this sintered body was cut into a shape of 180.0 mm in diameter and 5.0 mm in thickness by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by CANON ANELVA), and Perform sputtering. Set the sputtering conditions to 1 kW of input power and Ar gas. After a pre-sputtering of 2 kWhr was performed at a pressure of 1.7 Pa, a film was formed on a Si substrate having a diameter of 4 inches for 20 seconds. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 250, and good results were obtained.

(Example 2)

Fe-Pt alloy powder, BN powder (flaky), and SiO ₂ powder were prepared as raw material powders. These powders were weighed to 70 (50Fe-50Pt) -5SiO ₂ -25BN (mol%).

Next, the Fe-Pt alloy powder, the SiO ₂ powder, and the zirconia grinding ball of the crushing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the medium stirring mill and the BN powder were mixed with a V-type mixer, and further mixed with a 100 μm mesh sieve, and the mixed powder was filled in a carbon mold and hot-pressed.

The conditions of the hot pressing were set to a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours in the same manner as in Example 1. Pressurization was performed at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the holding was completed, observation was performed by using an in-furnace SEM. The results are shown in FIG. 2. As can be seen from FIG. 2, in the cross-sectional direction of the vertical sputtering surface, a layered structure is formed and BN is oriented. In FIG. 2, the average thickness of the hexagonal BN phase is 9 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of X-ray diffraction peaks on the BN (002) plane horizontal to the sputtering surface was 566, and the X-ray diffraction of the BN (002) plane on the cross-section of the vertical sputtering surface. The peak intensity is 45, and the intensity ratio is 12.6.

Next, this sintered body was cut into a shape of 180.0 mm in diameter and 5.0 mm in thickness by a lathe, and then installed in a magnetron sputtering device (C-3010 sputtering system manufactured by Canon Anahua). 1 Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 30, and good results were obtained.

(Example 3)

Fe-Pt alloy powder, BN powder (flaky), Ag powder, and C (flaked graphite) powder were prepared as raw material powders. These powders were weighed to 58 (35Fe-10Pt) -20Ag-20BN-2C (mol%).

Next, the Fe-Pt alloy powder and the zirconia grinding ball of the pulverizing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the medium stirring mill was mixed with a BN powder, a C powder, and an Ag powder with a V-type mixer, and further mixed with a mortar, and this was filled in a carbon mold and hot-pressed.

The conditions of the hot pressing were set in a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours in the same manner as in Example 1. The pressure was increased at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C / hour, the holding temperature was 950 ° C, and the holding time was 2 hours. The gas pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 950 ° C and 150MPa Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. The result Shown in Figure 3. As can be seen from FIG. 3, in the cross-sectional direction of the vertical sputtering surface, a layered structure is formed and BN is oriented. In FIG. 3, the average thickness of the hexagonal BN phase is 2.2 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 327, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 45. The ratio is 7.3.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 25, and good results were obtained.

(Example 4)

Fe-Pt alloy powder, BN powder (flaky), and Ag powder were prepared as raw material powders. These powders were weighed into 55 (45Fe-45Pt-10Ag) -45BN (mol%).

Next, the Fe-Pt alloy powder and the zirconia grinding ball of the pulverizing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the media stirring mill was mixed with a BN powder and an Ag powder with a V-type mixer, and then mixed with a 150 μm mesh sieve, and this was filled in a carbon mold and hot-pressed.

The conditions of the hot pressing were set in a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours in the same manner as in Example 1. The pressure was increased at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1, and the temperature rising rate was 300 ° C / hour, the holding temperature was 950 ° C, and After 2 hours, the pressure of the Ar gas was gradually increased from the start of the temperature rise, and the pressure was maintained at 950 ° C and 150 MPa. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that in the cross-sectional direction of the vertical sputtering surface, a layered structure was formed and BN was oriented. The average thickness of the hexagonal BN phase was 6 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 713, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 52. The ratio is 13.7.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 83, and good results were obtained.

(Example 5)

Fe-Pt alloy powder, BN powder (flaky), Ag powder, and SiO ₂ powder were prepared as raw material powders. These powders were weighed to 80 (50Fe-40Pt-10Ag) -5SiO ₂ -15BN (mol%).

Next, the Fe-Pt alloy powder and the zirconia grinding ball of the pulverizing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the media stirring mill was mixed with a BN powder, an Ag powder, and a SiO ₂ powder with a V-type mixer, and then mixed with a mortar, and then filled into a carbon mold and hot-pressed.

The conditions of the hot pressing were the same as in Example 1. The vacuum environment, the heating rate was 300 ° C / hour, the holding temperature was 950 ° C, and the holding time was 2 hours. Pressurize. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C / hour, the holding temperature was 950 ° C, and the holding time was 2 hours. The gas pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 950 ° C and 150MPa Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that in the cross-sectional direction of the vertical sputtering surface, a layered structure was formed and BN was oriented. The average thickness of the hexagonal BN phase was 2.4 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 158, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 46. The ratio is 3.4.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 25, and good results were obtained.

(Example 6)

Fe-Pt alloy powder, BN powder (flaky), and Cu powder were prepared as raw material powders. These powders were weighed into 80 (50Fe-45Pt-5Cu) -20BN (mol%).

Next, the Fe-Pt alloy powder and the zirconia grinding ball of the pulverizing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the medium stirring mill was mixed with a BN powder and a Cu powder in a V-type mixer, and then a 150 μm mesh was used. The sieve is mixed, filled in a carbon mold, and hot-pressed.

The conditions of the hot pressing were set in a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours in the same manner as in Example 1. The pressure was increased at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 950 ° C., and the holding time was 2 hours. The gas pressure of Ar gas was gradually increased from the start of heating, and the temperature was maintained at 950 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that in the cross-sectional direction of the vertical sputtering surface, a layered structure was formed and BN was oriented. The average thickness of the hexagonal BN phase was 3 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 498, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 43. The ratio is 11.6.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 126, and good results were obtained.

(Example 7)

Fe-Pt alloy powder, BN powder (flaky), and Au powder were prepared as raw material powders. These powders were weighed to 80 (50Fe-45Pt-5Au) -20BN (mol%).

Next, the Fe-Pt alloy powder and a zirconia grinding ball of a pulverizing medium are put into a capacity of 5 L. In a medium agitating mill, it was treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the medium stirring mill was mixed with the BN powder and the Au powder in a V-type mixer, and further mixed with a 150 μm mesh sieve, and this was filled in a carbon mold and hot-pressed.

The conditions of the hot pressing were set in a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours in the same manner as in Example 1. The pressure was increased at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C / hour, the holding temperature was 950 ° C, and the holding time was 2 hours. The gas pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 950 ° C and 150MPa Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that in the cross-sectional direction of the vertical sputtering surface, a layered structure was formed and BN was oriented. The average thickness of the hexagonal BN phase was 2.5 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane horizontal to the sputtering surface was 523, and the X-ray diffraction peak intensity of the BN (002) plane of the cross-section of the vertical sputtering surface was 46. The ratio is 11.4.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 174, and good results were obtained.

(Example 8)

Fe-Pt alloy powder, BN powder (flaky), Ru powder, SiO ₂ powder, and TiO ₂ powder were prepared as raw material powders. These powders were weighed to 74 (48Fe-48Pt-4Ru) -3SiO ₂ -3TiO ₂ -20BN (mol%).

Next, the Fe-Pt alloy powder and the zirconia grinding ball of the pulverizing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the medium agitating mill was mixed with BN powder, Ru powder, SiO ₂ powder, and TiO ₂ powder by a V-type mixer, and then mixed with a mortar to fill the carbon mold and Perform hot pressing.

The conditions of the hot pressing were set in a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours in the same manner as in Example 1. The pressure was increased at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 950 ° C., and the holding time was 2 hours. The gas pressure of Ar gas was gradually increased from the start of heating, and the temperature was maintained at 950 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that in the cross-sectional direction of the vertical sputtering surface, a layered structure was formed and BN was oriented. The average thickness of the hexagonal BN phase was 2.4 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane on the horizontal plane of the sputtering surface was 369, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering plane was 42. The ratio is 8.8.

Next, the sintered body was cut into a shape of 180.0 mm in diameter and 5.0 mm in thickness by a lathe. After that, it was mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Annelwa), and sputtering was performed under the same conditions as in Example 1. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 36, and good results were obtained.

(Example 9)

Preparing Fe-Pt alloy powder, BN powder (flake), Cr ₂ 0 ₃ powder as raw material powders. These powders were weighed to 75 (55Fe-45Pt) -5Cr ₂ 0 ₃ -20BN (mol%).

Next, the Fe-Pt alloy powder and the zirconia grinding ball of the pulverizing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, from the extracted medium stirring mill powder and BN powder and Cr ₂ 0 ₃ powder were mixed in a V-shaped mixer, mixing using a mortar, which was filled in a carbon mold and hot-pressed.

The conditions of the hot pressing were set in a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours in the same manner as in Example 1. The pressure was increased at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 950 ° C., and the holding time was 2 hours. The gas pressure of Ar gas was gradually increased from the start of heating, and the temperature was maintained at 950 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that in the cross-sectional direction of the vertical sputtering surface, a layered structure was formed and BN was oriented. The average thickness of the hexagonal BN phase was 3.2 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, X-rays of the BN (002) plane which is horizontal to the sputtering surface The diffraction peak intensity is 252, the X-ray diffraction peak intensity of the BN (002) plane of the cross section of the vertical sputtering surface is 48, and the intensity ratio is 5.3.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 76, and good results were obtained.

(Example 10)

Fe-Pt alloy powder, BN powder (flaky), Ag powder, and TiN powder were prepared as raw material powders. These powders were weighed to 75 (45Fe-55Pt-10Ag) -3TiN-22BN (mol%).

Next, the Fe-Pt alloy powder and the zirconia grinding ball of the pulverizing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the medium agitating mill was mixed with the BN powder and the TiN powder in a V-type mixer, and then mixed using a mortar. The carbon mold was filled and hot-pressed.

The conditions of the hot pressing were set in a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours in the same manner as in Example 1. The pressure was increased at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 950 ° C., and the holding time was 2 hours. The gas pressure of Ar gas was gradually increased from the start of heating, and the temperature was maintained at 950 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. the result, It was confirmed that in the cross-sectional direction of the vertical sputtering surface, a layered structure was formed and BN was oriented. The average thickness of the hexagonal BN phase was 5 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 289, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 43. The ratio is 6.7.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 129, and good results were obtained.

(Example 11)

Fe-Pt alloy powder, BN powder (flaky), Ag powder, and SiC powder were prepared as raw material powders. These powders were weighed to 75 (45Fe-55Pt-10Ag) -3SiC-22BN (mol%).

Next, the Fe-Pt alloy powder and the zirconia grinding ball of the pulverizing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the media stirring mill was mixed with the BN powder and the SiC powder with a V-type mixer, and then mixed with a mortar, and the carbon mold was filled and hot-pressed.

The conditions of the hot pressing were set in a vacuum environment, a heating rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours in the same manner as in Example 1. The pressure was increased at 30 MPa from the start of the heating to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1, and the temperature rising rate was 300 ° C / hour, the holding temperature was 950 ° C, and After 2 hours, the pressure of the Ar gas was gradually increased from the start of the temperature rise, and the pressure was maintained at 950 ° C and 150 MPa. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that in the cross-sectional direction of the vertical sputtering surface, a layered structure was formed and BN was oriented. The average thickness of the hexagonal BN phase was 4.2 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 304, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 49. The ratio is 6.2.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 137, and good results were obtained.

(Example 12)

Fe-Pt alloy powder and BN powder (flaky) were prepared as raw material powders. These powders were weighed into 40 (55Fe-45Pt) -60BN (mol%).

Next, the Fe-Pt alloy powder and the zirconia grinding ball of the pulverizing medium were put into a medium stirring grinder with a capacity of 5 L, and treated at a rotation number of 300 rpm for 2 hours. The average particle diameter of the treated Fe-Pt alloy powder was 10 μm. Then, the powder taken out from the medium stirring mill and the BN powder were mixed with a V-type mixer, and further mixed with a 150 μm mesh sieve, and this was filled in a carbon mold and hot-pressed.

The conditions of the hot pressing were the same as in Example 1. The vacuum environment, the heating rate was 300 ° C / hour, the holding temperature was 950 ° C, and the holding time was 2 hours. Pressurize. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C / hour, the holding temperature was 950 ° C, and the holding time was 2 hours. The gas pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 950 ° C and 150MPa Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that in the cross-sectional direction of the vertical sputtering surface, a layered structure was formed and BN was oriented. The average thickness of the hexagonal BN phase was 9.5 μm. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 810, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 53. The ratio is 15.3.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 358, and good results were obtained.

(Comparative example 1)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flaky), and C powder were prepared as raw material powders. These powders were weighed into 60 (30Fe-70Pt) -5BN-35C (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as those in Example 1. The conditions were a vacuum environment, a heating rate of 300 ° C / hour, The holding temperature was 1200 ° C, the holding time was 2 hours, and the pressure was increased from 30 MPa from the start of the temperature rise to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. The results are shown in FIG. 4. As can be seen from FIG. 4, the layered structure is not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 52, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 44. The ratio is 1.2.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 1100, which was significantly increased compared with the examples.

(Comparative example 2)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flaky), and Ag powder were prepared as raw material powders. These powders were weighed into 55 (45Fe-45Pt-10Ag) -45BN (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as those in Example 1. The conditions were a vacuum environment, a heating rate of 300 ° C / hour, The holding temperature was 1200 ° C, the holding time was 2 hours, and the pressure was increased from 30 MPa from the start of the temperature rise to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that the layered structure was not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak on the BN (002) plane that is horizontal to the sputtering surface is 67, and the intensity of the X-ray diffraction peak on the BN (002) plane that is perpendicular to the cross-section of the sputtering surface is 52. The ratio is 1.3.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 860, which was a significant increase compared to the examples.

(Comparative example 3)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flaky), Ag powder, and SiO ₂ powder were prepared as raw material powders. These powders were weighed to 80 (50Fe-40Pt-10Ag) -5Si0 ₂ -15BN (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as those in Example 1. The conditions were a vacuum environment, a heating rate of 300 ° C / hour, The holding temperature was 1200 ° C, the holding time was 2 hours, and the pressure was increased from 30 MPa from the start of the temperature rise to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that the layered structure was not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane on the plane horizontal to the sputtered surface was 58, and the X-ray diffraction peak intensity of the BN (002) plane of the cross-section of the vertical sputtering plane was 46. The ratio is 1.3.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 712, which was significantly increased compared to the examples.

(Comparative Example 4)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flaky), and Cu powder were prepared as raw material powders. These powders were weighed into 80 (50Fe-45Pt-5Cu) -20BN (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as those in Example 1. The conditions were a vacuum environment, a heating rate of 300 ° C / hour, The holding temperature was 1200 ° C, the holding time was 2 hours, and the pressure was increased from 30 MPa from the start of the temperature rise to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that the layered structure was not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 71, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 43. The ratio is 1.7.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 616, which was a significant increase compared to the examples.

(Comparative example 5)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flaky), and Au powder were prepared as raw material powders. These powders were weighed to 80 (50Fe-45Pt-5Au) -20BN (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as those in Example 1. The conditions were a vacuum environment, a heating rate of 300 ° C / hour, The holding temperature was 1200 ° C, the holding time was 2 hours, and the pressure was increased from 30 MPa from the start of the temperature rise to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that the layered structure was not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 64, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 46. The ratio is 1.4.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 732, which was significantly increased compared with the examples.

(Comparative Example 6)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flaky), Ru powder, TiO ₂ powder, and SiO ₂ powder were prepared as raw material powders. These powders were weighed to 74 (48Fe-48Pt-4Ru) -3Ti0 ₂ -3Si0 ₂ -20BN (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as those in Example 1. The conditions were a vacuum environment, a heating rate of 300 ° C / hour, The holding temperature was 1200 ° C, the holding time was 2 hours, and the pressure was increased from 30 MPa from the start of the temperature rise to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that the layered structure was not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 46, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 42. The ratio is 1.1.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 1047, which was significantly increased compared with the examples.

(Comparative Example 7)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flaky), and Cr ₂ 0 ₃ powder were prepared as raw material powders. These powders were weighed to 75 (55Fe-45Pt) -5Cr ₂ 0 ₃ -20BN (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as those in Example 1. The conditions were a vacuum environment, a heating rate of 300 ° C / hour, The holding temperature was 1200 ° C, the holding time was 2 hours, and the pressure was increased from 30 MPa from the start of the temperature rise to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that the layered structure was not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane on the plane horizontal to the sputtering surface was 52, and the X-ray diffraction peak intensity of the BN (002) plane on the cross-section of the vertical sputtering plane was 48. The ratio is 1.1.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 823, which was significantly increased compared with the examples.

(Comparative Example 8)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flaky), Ag powder, and TiN powder were prepared as raw material powders. These powders were weighed to 75 (45Fe-55Pt-10Ag) -3TiN-22BN (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as those in Example 1. The conditions were a vacuum environment, a heating rate of 300 ° C / hour, The holding temperature was 1200 ° C, the holding time was 2 hours, and the pressure was increased from 30 MPa from the start of the temperature rise to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that the layered structure was not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane on the plane horizontal to the sputtering surface was 53, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering plane was 43. The ratio is 1.2.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 1079, which was significantly increased compared with the examples.

(Comparative Example 9)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flaky), Ag powder, and SiC powder were prepared as raw material powders. These powders were weighed to 75 (45Fe-55Pt-10Ag) -3SiC-22BN (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as those in Example 1. The conditions were a vacuum environment, a heating rate of 300 ° C / hour, The holding temperature was 1200 ° C, the holding time was 2 hours, and the pressure was increased from 30 MPa from the start of the temperature rise to the end of the holding. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that the layered structure was not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 77, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 49. The ratio is 1.6.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 1055, which was significantly increased compared with the examples.

(Comparative Example 10)

Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, and BN powder (flaky) were prepared as raw material powders. These powders were weighed into 40 (55Fe-45Pt) -60BN (mol%).

Next, the weighed powder was mixed with a V-type mixer, and then mixed with a mortar, filled into a carbon mold, and hot-pressed.

The conditions of the hot pressing were the same as in Example 1. The conditions were vacuum environment, heating rate of 300 ° C / hour, holding temperature of 1200 ° C, and holding time of 2 hours. 行 压 压。 Line pressure. After the holding, the natural cooling is performed directly in the chamber.

Next, the sintered body taken out from the hot press mold was subjected to hot equalizing processing. The conditions of the hot equalizing process were the same as those in Example 1. The heating rate was 300 ° C./hour, the holding temperature was 1100 ° C., and the holding time was 2 hours. The pressure of the Ar gas was gradually increased from the start of the heating, and the temperature was maintained at 1100 ° C. and 150 MPa. Pressurize. After the end of the cooling, it is naturally cooled in the furnace.

The end of the sintered body obtained in this manner was cut, and its cross section was observed by SEM. As a result, it was confirmed that the layered structure was not formed in the cross-sectional direction of the vertical sputtering surface. Next, the cross section of the sintered body was measured using X-ray diffraction (XRD). As a result, the intensity of the X-ray diffraction peak of the BN (002) plane horizontal to the sputtering surface was 82, and the intensity of the X-ray diffraction peak of the BN (002) plane of the cross-section of the vertical sputtering surface was 53. The ratio is 1.5.

Next, the sintered body was cut into a shape with a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then mounted on a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anahua). Sputtering was performed under the same conditions. Then use a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 2530, which was significantly increased compared with the examples.

[Industrial availability]

The Fe-Pt-based sintered body using BN as a non-magnetic material according to the present invention has an excellent effect of providing a sputtering target capable of reducing the amount of particles generated during sputtering. Therefore, it is suitable as a sputtering target for a magnetic thin film for forming a granular structure.

Claims (12)

A sintered body sputtering target, which is a Fe-Pt based sintered body sputtering target containing BN, which is characterized in that it is opposite to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the horizontal plane of the sputtering plane. The intensity ratio of the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the cross section of the vertical sputtering surface is 2 or more. For example, the sintered body sputtering target of the first scope of the patent application, wherein the average thickness of the hexagonal BN phase in the cross section of the vertical sputtering surface is 30 μm or less. For example, the sputtering target for a magnetic recording film according to item 1 of the patent application scope, wherein the Pt content is 5 mol% or more and 60 mol% or less. For example, the sputtering target for a magnetic recording film according to item 2 of the patent application, wherein the Pt content is 5 mol% or more and 60 mol% or less. For example, the sputtering target for a magnetic recording film according to any one of claims 1 to 4, wherein the BN content is 1 mol% or more and 60 mol% or less. For example, the sputtering target for a magnetic recording film according to any one of claims 1 to 4 contains 0.5 mol% or more and 40.0 mol% or less selected from the group consisting of C, Ru, Ag, Au, and Cu. More than one element is used as the additive element. For example, a sputtering target for a magnetic recording film according to item 5 of the patent application, which contains at least one element selected from the group consisting of C, Ru, Ag, Au, and Cu in an amount of 0.5 mol% or more and 40.0 mol% or less as an additive. element. For example, the sputtering target for a magnetic recording film according to any one of claims 1 to 4 includes one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides as additives. material. For example, a sputtering target for a magnetic recording film according to item 5 of the application, which contains one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides as an additive material. For example, the sputtering target for a magnetic recording film according to item 6 of the patent application contains as an additive material one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides. For example, the sputtering target for a magnetic recording film according to item 7 of the patent application scope contains as an additive material one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides. A method for manufacturing a sputtering target for manufacturing a sputtering target according to any one of claims 1 to 11 in a patent application. The manufacturing method is to mix and shape a flake-shaped or plate-shaped raw material powder, and then The formed body is subjected to uniaxial pressure sintering.