WO2014065201A1 - Fe-Pt SINTERED COMPACT SPUTTERING TARGET AND MANUFACTURING METHOD THEREFOR - Google Patents

Abstract

An Fe-Pt sintered compact sputtering target containing BN characterized in that the intensity ratio of the X-ray diffraction peak intensity of a hexagonal BN (002) plane in a plane level with the sputtering surface with respect to the X-ray diffraction peak intensity of a hexagonal BN (002) plane in a cross-section perpendicular to the sputtering surface is 2 or more. The present invention addresses the problem of providing a sputtering target with which manufacture of a magnetic film in thermally assisted magnetic recording media is possible and particles that are generated during sputtering are reduced.

Description

Fe—Pt sintered compact sputtering target and method for producing the same

The present invention relates to an Fe—Pt-based sintered sputtering target used for manufacturing a magnetic thin film in a heat-assisted magnetic recording medium and a manufacturing method thereof.

In the field of magnetic recording typified by hard disk drives, materials based on Co, Fe, or Ni, which are ferromagnetic metals, are used as materials for magnetic thin films in magnetic recording media. For example, in a magnetic thin film of a hard disk employing the in-plane magnetic recording method, a Co—Cr-based or Co—Cr—Pt-based ferromagnetic alloy containing Co as a main component has been used. In addition, hard magnetic thin films employing perpendicular magnetic recording that have been put into practical use in recent years often use a composite material composed of Co—Cr—Pt-based ferromagnetic alloy mainly composed of Co and non-magnetic inorganic particles. It has been. And since the said magnetic thin film is high in productivity, it is often produced by sputtering the sputtering target which uses the said material as a component with a DC magnetron sputtering apparatus.

The recording density of hard disks is rapidly increasing year by year, and it is considered that the future will reach 1 Tbit / in ² from the current surface density of 600 Gbit / in ² . When the recording density reaches 1 Tbit / in ² , the size of the recording bit becomes less than 10 nm. In that case, superparamagnetization due to thermal fluctuation is expected to be a problem. It is expected that a material such as a material in which Pt is added to a Co—Cr base alloy to increase the magnetocrystalline anisotropy is not sufficient. This is because magnetic particles that behave stably as ferromagnetism with a size of 10 nm or less need to have higher crystal magnetic anisotropy.

For the above reasons, FePt phase having an L1 ₀ structure is attracting attention as a material for an ultra-high density recording medium. The FePt phase is expected to be a material suitable for application as a magnetic recording medium because it has high crystal magnetic anisotropy and excellent corrosion resistance and oxidation resistance. When the FePt phase is used as a material for an ultra-high density recording medium, it is necessary to develop a technique that aligns and disperses ordered FePt magnetic particles with as high a density as possible in a magnetically isolated state. It has been.

For this reason, a granular structure magnetic thin film of FePt magnetic particles are isolated by a non-magnetic material such oxides or carbon having an L1 ₀ structure, as for a magnetic recording medium of the next generation hard disk employing a thermally assisted magnetic recording method ,Proposed. This granular structure magnetic thin film has a structure in which magnetic particles are magnetically insulated by interposition of a nonmagnetic substance. Generally, a granular magnetic thin film having an Fe—Pt phase is formed using an Fe—Pt sintered sputtering target.

Regarding the Fe—Pt magnetic material sintered sputtering target, the present inventors have previously been composed of a magnetic phase such as an Fe—Pt alloy and a nonmagnetic phase separating the magnetic phase. As one of them, a technique related to a ferromagnetic sputtering target using a metal oxide has been disclosed (Patent Document 1).
In addition, Patent Document 2 discloses a sputtering target for forming a magnetic recording medium film made of a sintered body having a structure in which a C layer is dispersed in an FePt alloy phase. _A sputtering target for forming a magnetic recording medium film comprising _two phases, an FePt alloy phase, and an interdiffusion phase is disclosed. Patent Document 4 discloses a Fe—Pt ferromagnetic sputtering target composed of Pt, SiO ₂ , Sn, and the balance Fe, and Patent Document 5 discloses quartz with respect to background intensity in X-ray diffraction. Discloses a sputtering target for a magnetic recording film having a (011) plane peak intensity ratio of 1.40 or more.

Hexagonal BN (a compound of boron and nitrogen) as the nonmagnetic material exhibits excellent performance as a lubricant, but when used as a raw material for powder metallurgy, it has a high density due to poor sinterability. It is difficult to produce a sintered body. And when the density of such a sintered compact is low, when processing a sintered compact into a target, defects, such as a crack and chipping, raise | generate a problem of reducing a yield. In addition, when the density is low, a large number of holes are generated in the target, and these holes cause abnormal discharge, generating particles (dust adhering to the substrate) during sputtering and reducing the product yield. There was a problem.

International Publication No. WO2012 / 029498 JP 2012-102387 A JP 2011-208167 A International Publication No. WO2012 / 085578 Patent No. 5009447

The present invention provides an Fe—Pt-based sintered body using hexagonal BN as a nonmagnetic material, which makes it possible to produce a magnetic thin film of a heat-assisted magnetic recording medium. It is an object to provide a sputtering target with a reduced amount.

In order to solve the above problems, the present inventors have conducted intensive research. As a result, the hexagonal BN, which is a nonmagnetic material, has a two-dimensional crystal structure. It has been found that if the crystal orientation of the crystalline BN is random, the electric conduction is affected and abnormal discharge is generated, which causes the sputtering to become unstable.

Based on such knowledge, the present invention
1) A Fe—Pt sintered sputtering target containing BN, which is hexagonal in a cross section perpendicular to the sputtering surface with respect to the X-ray diffraction peak intensity of the hexagonal BN (002) surface in the horizontal plane with respect to the sputtering surface. A sintered body sputtering target, wherein the intensity ratio of the X-ray diffraction peak intensity of the crystal BN (002) plane is 2 or more,
2) The sintered sputtering target according to 1) above, wherein the average thickness of the hexagonal BN phase in a cross section perpendicular to the sputtering surface is 30 μm or less,
3) The sintered sputtering target according to 1) or 2) above, wherein the Pt content is 5 mol% or more and 60 mol% or less. 4) The BN content is 1 mol% or more and 60 mol% or less. The sintered sputtering target according to any one of 1) to 3) above,
5) The additive according to any one of 1) to 4) above, wherein the additive element contains one or more elements selected from the group consisting of C, Ru, Ag, Au, and Cu in an amount of 0.5 mol% to 40.0 mol%. The sintered compact sputtering target according to any one of the above,
6) The firing according to any one of 1) to 5) above, wherein the additive contains one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides. Conjugate sputtering target,
7) The sputtering target according to any one of 1) to 6) above, wherein flaky or plate-like raw material powders are mixed, molded, and then the compact is uniaxially pressed and sintered. A method for producing a sputtering target is provided.

The Fe—Pt-based sintered body using BN as the nonmagnetic material of the present invention can suppress abnormal discharge during sputtering by improving the orientation of hexagonal BN and reduce the amount of generated particles. It has an excellent effect of being able to.

It is a microscope picture of the target of Example 1 (a horizontal plane with respect to a sputtering surface and a vertical cross section with respect to a sputtering surface). It is a microscope picture of the target (a horizontal surface with respect to a sputtering surface, and a perpendicular cross section with respect to a sputtering surface) of Example 2. It is a microscope picture of the target of Example 3 (a horizontal surface with respect to a sputtering surface, and a perpendicular cross section with respect to a sputtering surface). It is a microscope picture of the target of Comparative Example 1 (horizontal plane with respect to the sputtering surface and vertical cross section with respect to the sputtering surface). It is an X-ray diffraction profile of the target of Example 1 (horizontal plane with respect to the sputtering surface) (uppermost stage). It is an X-ray diffraction profile of the target of Example 1 (a step surface perpendicular to the sputtering surface) (the uppermost step). It is an X-ray-diffraction profile of the target of Example 2 (horizontal surface with respect to a sputtering surface) (top stage). It is a X-ray-diffraction profile of the target of Example 2 (perpendicular | vertical cross section with respect to a sputtering surface) (top stage). It is an X-ray-diffraction profile of the target of Example 3 (horizontal surface with respect to a sputtering surface) (top stage). It is an X-ray-diffraction profile of the target of Example 3 (perpendicular | vertical cross section with respect to a sputtering surface) (top stage). It is an X-ray-diffraction profile of the target (the horizontal surface with respect to a sputtering surface) of the comparative example 1 (uppermost stage). It is an X-ray-diffraction profile of the target of Comparative Example 1 (perpendicular cross section with respect to the sputtering surface) (uppermost stage).

Since hexagonal BN, which is a nonmagnetic material, has a two-dimensional crystal structure, if the orientation of this hexagonal BN crystal is random in the target, it will affect electrical conduction, Sputtering may become unstable. Therefore, stable sputtering can be achieved by aligning the hexagonal BN crystal in one direction.

That is, the Fe—Pt-based sintered sputtering target of the present invention contains hexagonal BN as a nonmagnetic material, and has a sputter strength against the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the horizontal plane with respect to the sputtering plane. The intensity ratio of the X-ray diffraction peak intensity of the hexagonal BN (002) plane in a cross section perpendicular to the plane is set to 2 or more.

In the Fe—Pt sintered sputtering target of the present invention, the hexagonal BN phase is preferably flaky or plate-like, and more preferably the average of the hexagonal BN phase in a cross section perpendicular to the sputtering surface. The thickness is 30 μm or less. Thereby, the influence of the electrical conduction resulting from hexagonal BN can be reduced, and stable sputtering can be performed.

In the present invention, the Pt content is preferably 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. Further, the content of hexagonal BN is preferably 1 mol% or more and 60 mol% or less. Magnetic insulation can be improved by making BN content as a nonmagnetic material into 1 mol% or more and 60 mol% or less.
In the Fe—Pt-based sintered sputtering target of the present invention, the balance is Fe, except for Pt, hexagonal BN, and additional elements and additives described later.

In the present invention, it is preferable to add one or more elements selected from the group consisting of C, Ru, Ag, Au, and Cu as additive elements in a total amount of 0.5 mol% or more and 40.0 mol% or less. Further, as the additive, it is preferable to add one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides. These additive elements and additives are effective components for improving the magnetic properties of the sputtered film.

The Fe—Pt 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, alloy powder (Fe—Pt powder) may be used as the raw material powder. The alloy powder containing Pt is effective for reducing the amount of oxygen in the raw material powder, although it depends on its composition. Furthermore, each raw material powder which is an additional component hung up above is prepared as needed.

Next, the metal powder (Fe powder, Pt powder) or the alloy powder (Fe—Pt alloy powder) is pulverized using a ball mill, a medium stirring mill or the like. Usually, such a raw material powder of metal is used in a spherical shape, a lump shape, or other irregular shape, but since hexagonal BN has a plate shape or a flake shape, when these are mixed and sintered, It becomes difficult to align the directions of hexagonal BN in the sintered body. Therefore, by making the metal raw material powder into a plate shape or a flake shape by grinding, the metal raw material and the hexagonal BN can be stacked on each other, and the orientation of the hexagonal BN can be made uniform. Become.

The metal powder or alloy powder obtained by pulverization in this way and the hexagonal BN powder are mixed using a mortar, a medium stirring mill, a sieve or the like. Additive components and additives should be added together with the metal raw material powder, added together with the hexagonal BN powder, or mixed at the stage where the metal raw material powder and the hexagonal BN powder are mixed. Can do.
Thereafter, this mixed powder is molded and sintered by hot pressing. In addition to hot pressing, a plasma discharge sintering method or a hot isostatic pressing method can also be used. The holding temperature at the time of sintering depends on the composition of the sputtering target, but in most cases, it is in the temperature range of 800 ° C. to 1400 ° C.

Next, hot isostatic pressing is performed on the sintered body taken out from the hot press. Hot isostatic pressing is effective in improving the density of the sintered body. The holding temperature during hot isostatic pressing depends on the composition of the sintered body, but in many cases is in the temperature range of 800 ° C to 1200 ° C. The pressing force is set to 100 MPa or more. And a sputtering target is producible by processing the sintered compact obtained in this way into a desired shape with a lathe.
As described above, the X-ray of the hexagonal BN (002) plane in the cross section perpendicular to the sputter plane with respect to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the horizontal plane with respect to the sputter plane is contained. An Fe—Pt-based sintered sputtering target having a diffraction peak intensity ratio of 2 or more can be produced.
For the evaluation of crystal orientation, an X-ray diffractometer was used to measure the X-ray diffraction intensity of the horizontal plane and the cross section perpendicular to the sputtering surface with respect to the sputtering surface of the sintered body for sputtering target under the following measurement conditions. . Apparatus: manufactured by Rigaku Corporation (Ultima IV protectus), tube bulb: Cu, tube voltage: 40 kV, tube current: 30 mA, scanning range (2θ): 10 ° to 90 °, measurement step (2θ): 0.01 °, Scan speed (2θ): 1 ° per minute, scan mode 2θ / θ. The diffraction peak of the hexagonal BN (002) plane appears in the vicinity of (2θ): 26.75 °.

Hereinafter, description will be made based on examples and comparative examples. In addition, a present Example is an example to the last, and is not restrict | limited at all by this example. In other words, the present invention is limited only by the scope of the claims, and includes various modifications other than the examples included in the present invention.

(Example 1)
Fe—Pt alloy powder and hexagonal BN powder (flakes) were prepared as raw material powders, and these powders were weighed so as to be 70 (50Fe-50Pt) -30BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment 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 using a 150 μm sieve, and this mixed powder was filled into a carbon mold and hot pressed.
The hot pressing conditions were a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurization was performed at 30 MPa from the start of temperature rising to the end of holding. After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., a holding time of 2 hours, and gradually increasing the Ar gas pressure from the start of the temperature increase to 1100 ° While being held at C, it was pressurized at 150 MPa. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. The result is shown in FIG. From FIG. 1, it can be seen that the layer has a layered structure in the direction perpendicular to the sputtering surface, and BN is oriented. Further, from FIG. 1, the average thickness of the hexagonal BN phase was 3 μm. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 657, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 54, The intensity ratio was 12.2.
Next, this sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm by a lathe, and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva) and subjected to sputtering. The sputtering conditions were an input power of 1 kW and an Ar gas pressure of 1.7 Pa. After performing pre-sputtering of 2 kWhr, a film was formed on a 4-inch diameter Si substrate for 20 seconds. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 250 and good results were obtained.

(Example 2)
Fe—Pt alloy powder, BN powder (flakes), and SiO ₂ powder were prepared as raw material powders. These powders were weighed so as to be 70 (50Fe-50Pt) -5SiO ₂ -25BN (mol%).
Next, the Fe—Pt alloy powder and the SiO ₂ powder were put together with a zirconia ball as a grinding medium into a medium stirring mill having a capacity of 5 L and treated at a rotational speed of 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment 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 using a 100 μm sieve, and the mixed powder was filled into a carbon mold and hot pressed.
The hot pressing conditions were the same as in Example 1, with a vacuum atmosphere, a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours, and the pressure was increased from 30 MPa to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After the completion of holding, observation was performed by in-furnace SEM. The result is shown in FIG. From FIG. 2, it can be seen that BN is oriented with a layered structure in the direction perpendicular to the sputtering surface. Further, from FIG. 2, the average thickness of the hexagonal BN phase was 9 μm. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 566, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 45, The intensity ratio was 12.6.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 30 and good results were obtained.

(Example 3)
Fe—Pt alloy powder, BN powder (flaky), Ag powder, and C (flaky graphite) powder were prepared as raw material powders. These powders were weighed so as to be 58 (35Fe-10Pt) -20Ag-20BN-2C (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. The powder taken out from the medium stirring mill, BN powder, C powder and Ag powder were mixed with a V-type mixer, mixed in a mortar, filled into a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. The result is shown in FIG. From FIG. 3, it can be seen that BN is oriented with a layered structure in the direction perpendicular to the sputtering surface. Moreover, from FIG. 3, the average thickness of the hexagonal BN phase was 2.2 μm. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 327, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 45, The intensity ratio was 7.3.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, good results were obtained with 25 particles.

Example 4
Fe—Pt alloy powder, BN powder (flakes), and Ag powder were prepared as raw material powders. These powders were weighed so as to be 55 (45Fe-45Pt-10Ag) -45BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. The powder taken out from the medium agitation mill, BN powder and Ag powder were mixed with a V-type mixer, then mixed using a 150 μm sieve, filled into a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface 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 an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 713, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 52, The intensity ratio was 13.7.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 83 particles.

(Example 5)
Fe—Pt alloy powder, BN powder (flakes), Ag powder, and SiO ₂ powder were prepared as raw material powders. These powders were weighed so as to be 80 (50Fe-40Pt-10Ag) -5SiO ₂ -15BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. The powder taken out from the medium stirring mill, BN powder, Ag powder, and SiO ₂ were mixed with a V-type mixer, mixed in a mortar, filled into a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface 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 an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 158, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 46, The intensity ratio was 3.4.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, good results were obtained with 25 particles.

(Example 6)
Fe-Pt alloy powder, BN powder (flakes), and Cu powder were prepared as raw material powders. These powders were weighed so as to be 80 (50Fe-45Pt-5Cu) -20BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. The powder taken out from the medium agitating mill, BN powder and Cu powder were mixed with a V-type mixer, and further mixed using a 150 μm sieve, filled into a carbon mold and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface 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 an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 498, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 43, The intensity ratio was 11.6.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. Good results were obtained with 126 particles at this time.

(Example 7)
Fe—Pt alloy powder, BN powder (flakes), and Au powder were prepared as raw material powders. These powders were weighed so as to be 80 (50Fe-45Pt-5Au) -20BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. The powder taken out from the medium agitating mill, BN powder and Au powder were mixed with a V-type mixer, and further mixed using a 150 μm sieve, filled into a carbon mold and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface 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 an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 523, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 46, The intensity ratio was 11.4.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 174 particles.

(Example 8)
Fe—Pt alloy powder, BN powder (flakes), Ru powder, SiO ₂ powder, and TiO ₂ powder were prepared as raw material powders. These powders were weighed so as to be 74 (48Fe-48Pt-4Ru) -3SiO ₂ -3TiO ₂ -20BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. Then, the powder taken out from the medium stirring mill, BN powder, Ru powder, SiO ₂ powder and TiO ₂ powder were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold and hot pressed. .
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface 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 an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 369, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 42, The intensity ratio was 8.8.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 36 particles.

Example 9
Fe—Pt alloy powder, BN powder (flakes), and Cr ₂ O ₃ powder were prepared as raw material powders. These powders were weighed so as to be 75 (55Fe-45Pt) -5Cr ₂ O ₃ -20BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. The powder taken out from the medium agitating mill, BN powder and Cr ₂ O ₃ powder were mixed with a V-type mixer, then mixed in a mortar, filled into a carbon mold and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface 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 an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 252 and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 48, The intensity ratio was 5.3.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 76 particles.

(Example 10)
Fe—Pt alloy powder, BN powder (flakes), Ag powder, and TiN powder were prepared as raw material powders. These powders were weighed to be 75 (45Fe-55Pt-10Ag) -3TiN-22BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. The powder taken out from the medium stirring mill, BN powder and TiN powder were mixed with a V-type mixer, then mixed in a mortar, filled in a carbon mold and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface 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 an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 289, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 43, The intensity ratio was 6.7.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 129 and good results were obtained.

(Example 11)
Fe—Pt alloy powder, BN powder (flakes), Ag powder, and SiC powder were prepared as raw material powders. These powders were weighed to be 75 (45Fe-55Pt-10Ag) -3TiN-22BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. The powder taken out from the medium agitation mill, BN powder and SiC powder were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface 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 an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 304, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 49, The intensity ratio was 6.2.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. A good result was obtained with 137 particles.

Example 12
Fe—Pt alloy powder and BN powder (flakes) were prepared as raw material powders. These powders were weighed so as to be 40 (55Fe-45Pt) -60BN (mol%).
Next, the Fe—Pt alloy powder was put into a medium stirring mill having a capacity of 5 L together with zirconia balls as a grinding medium, and treated at 300 rpm for 2 hours. The average particle size of the Fe—Pt alloy powder after the treatment was 10 μm. The powder taken out from the medium stirring mill and the BN powder were mixed with a V-type mixer, and further mixed using a 150 μm sieve, filled into a carbon mold and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 950 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 950 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that the film had a layered structure in the direction perpendicular to the sputtering surface 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 an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 810, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 53, The intensity ratio was 15.3.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, a good result was obtained with 358 particles.

(Comparative Example 1)
As raw material powder, Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, BN powder (flakes), and C powder were prepared. These powders were weighed so as to be 60 (30Fe-70Pt) -5BN-35C (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. The result is shown in FIG. From FIG. 4, it was found that the layered structure was not formed in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 52, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 44, The intensity ratio was 1.2.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 1100, which was significantly increased as compared with the example.

(Comparative Example 2)
As raw material powder, 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. These powders were weighed so as to be 55 (45Fe-45Pt-10Ag) -45BN (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 67, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 52, The intensity ratio was 1.3.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 860, which was significantly increased as compared with the example.

(Comparative Example 3)
As raw material powder, Fe powder with an average particle diameter of 5 μm, Pt powder with an average particle diameter of 6 μm, BN powder (flakes), Ag powder, and SiO ₂ powder were prepared. These powders were weighed so as to be 80 (50Fe-40Pt-10Ag) -5SiO ₂ -15BN (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 58, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane relative to the sputtering plane is 46, The intensity ratio was 1.3.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 712, which was significantly increased as compared with the example.

(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 so as to be 80 (50Fe-45Pt-5Cu) -20BN (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 71, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 43, The intensity ratio was 1.7.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 616, which was remarkably increased as compared with the example.

(Comparative Example 5)
As raw material powder, Fe powder with an average particle diameter of 5 μm, Pt powder with an average particle diameter of 6 μm, BN powder (flakes), and Au powder were prepared. These powders were weighed so as to be 80 (50Fe-45Pt-5Au) -20BN (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 64, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 46, The intensity ratio was 1.4.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 732, which was significantly increased as compared with the example.

(Comparative Example 6)
As raw material powder, 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. These powders were weighed so as to be 74 (48Fe-48Pt-4Ru) -3TiO ₂ -3SiO ₂ -20BN (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 46, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 42, The intensity ratio was 1.1.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 1047, which was significantly increased as compared with the example.

(Comparative Example 7)
As raw material powder, 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 O ₃ powder were prepared. These powders were weighed so as to be 75 (55Fe-45Pt) -5Cr ₂ O ₃ -20BN (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 52, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 48, The intensity ratio was 1.1.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 823, which was remarkably increased as compared with the example.

(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 be 75 (45Fe-55Pt-10Ag) -3TiN-22BN (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 53, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 43, The intensity ratio was 1.2.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. The number of particles at this time was 1079, which was significantly increased as compared with the example.

(Comparative Example 9)
As raw material powder, Fe powder with an average particle diameter of 5 μm, Pt powder with an average particle diameter of 6 μm, BN powder (flaky), Ag powder, and SiC powder were prepared. These powders were weighed so as to be 75 (45Fe-55Pt-10Ag) -3SiC-22BN (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 77, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 49, The intensity ratio was 1.6.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 1055, which was remarkably increased as compared with the example.

(Comparative Example 10)
As raw material powder, Fe powder having an average particle diameter of 5 μm, Pt powder having an average particle diameter of 6 μm, and BN powder (flaky shape) were prepared. These powders were weighed so as to be 40 (55Fe-45Pt) -60BN (mol%).
Next, the weighed powders were mixed in a V-type mixer, then mixed in a mortar, filled in a carbon mold, and hot pressed.
The hot press conditions were the same as in Example 1, with a vacuum atmosphere, a temperature rising rate of 300 ° C./hour, a holding temperature of 1200 ° C., and a holding time of 2 hours, and pressurized at 30 MPa from the start of temperature rising to the end of holding. . After completion of the holding, it was naturally cooled in the chamber.
Next, hot isostatic pressing was performed on the sintered body taken out from the hot press mold. The conditions for hot isostatic pressing were the same as in Example 1, with a temperature increase rate of 300 ° C./hour, a holding temperature of 1100 ° C., and a holding time of 2 hours. The pressure was gradually increased and the pressure was increased to 150 MPa while being held at 1100 ° C. After completion of the holding, it was naturally cooled in the furnace.
The end of the sintered body thus obtained was cut out and the cross section was observed by SEM. As a result, it was confirmed that there was no layered structure in the direction perpendicular to the sputtering surface. Next, the cross section of the sintered body was measured using an X-ray diffraction method (XRD). As a result, the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 82, and the X-ray diffraction peak intensity of the BN (002) plane in the horizontal plane with respect to the sputtering plane is 53, The intensity ratio was 1.5.
Next, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm with a lathe and then attached to a magnetron sputtering apparatus (C-3010 sputtering system manufactured by Canon Anelva), under the same conditions as in Example 1. Sputtering was performed. The number of particles adhering to the substrate was measured with a particle counter. At this time, the number of particles was 2530, which was remarkably increased as compared with the example.

The Fe—Pt sintered body using BN as the nonmagnetic material of the present invention has an excellent effect of providing a sputtering target with a reduced amount of particles generated during sputtering. Therefore, it is useful as a sputtering target used for forming a magnetic thin film having a granular structure.

Claims (7)

1. A Fe—Pt-based sintered sputtering target containing BN, which has a hexagonal BN in a cross section perpendicular to a sputtering surface with respect to an X-ray diffraction peak intensity of a hexagonal BN (002) surface in a horizontal plane with respect to the sputtering surface. A sintered body sputtering target, wherein the intensity ratio of the X-ray diffraction peak intensity of the (002) plane is 2 or more.
2. The sintered body sputtering target according to claim 1, wherein the average thickness of the hexagonal BN phase in a cross section perpendicular to the sputtering surface is 30 µm or less.
3. The sintered compact sputtering target according to claim 1 or 2, wherein the Pt content is 5 mol% or more and 60 mol% or less.
4. The sintered body sputtering target according to any one of claims 1 to 3, wherein the BN content is 1 mol% or more and 60 mol% or less.
5. The additive element according to any one of claims 1 to 4, wherein the additive element contains at least one element selected from the group consisting of C, Ru, Ag, Au, and Cu in an amount of 0.5 mol% to 40.0 mol%. The sintered compact sputtering target according to Item.
6. The sintered body according to any one of claims 1 to 5, wherein the additive contains one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides. Sputtering target.
7. The sputtering target according to any one of claims 1 to 6, characterized in that flaky or plate-like raw material powders are mixed, molded, and then the compact is uniaxially pressed and sintered. A method for producing a sputtering target.

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