JP5913620B2 - Fe-Pt sintered sputtering target and method for producing the same - Google Patents

Fe-Pt sintered sputtering target and method for producing the same Download PDF

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JP5913620B2
JP5913620B2 JP2014543263A JP2014543263A JP5913620B2 JP 5913620 B2 JP5913620 B2 JP 5913620B2 JP 2014543263 A JP2014543263 A JP 2014543263A JP 2014543263 A JP2014543263 A JP 2014543263A JP 5913620 B2 JP5913620 B2 JP 5913620B2
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真一 荻野
真一 荻野
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/851—Coating a support with a magnetic layer by sputtering

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Description

本発明は、熱アシスト磁気記録メディアにおける磁性薄膜の製造に用いられるＦｅ−Ｐｔ系焼結体スパッタリングターゲット及びその製造方法に関する。   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.

ハードディスクドライブに代表される磁気記録の分野では、磁気記録媒体中の磁性薄膜の材料として、強磁性金属であるＣｏ、ＦｅあるいはＮｉをベースとした材料が用いられている。例えば、面内磁気記録方式を採用するハードディスクの磁性薄膜では、Ｃｏを主成分とするＣｏ−Ｃｒ系やＣｏ−Ｃｒ−Ｐｔ系の強磁性合金が用いられてきた。また、近年実用化された垂直磁気記録方式を採用するハードディスクの磁性薄膜には、Ｃｏを主成分とするＣｏ−Ｃｒ−Ｐｔ系の強磁性合金と非磁性の無機物粒子からなる複合材料が多く用いられている。そして上記の磁性薄膜は生産性の高さから、上記材料を成分とするスパッタリングターゲットをＤＣマグネトロンスパッタ装置でスパッタして作製されることが多い。   In the field of magnetic recording typified by a hard disk drive, a material based on Co, Fe, or Ni, which is a ferromagnetic metal, is used as a material for a magnetic thin film in a magnetic recording medium. For example, in a magnetic thin film of a hard disk adopting the in-plane magnetic recording method, a Co—Cr-based or Co—Cr—Pt-based ferromagnetic alloy mainly containing Co has been used. In addition, a composite material composed of a Co—Cr—Pt ferromagnetic alloy containing Co as a main component and nonmagnetic inorganic particles is often used for a magnetic thin film of a hard disk that employs a perpendicular magnetic recording method that has been put into practical use in recent years. 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.

ハードディスクの記録密度は年々急速に増大しており、現状の６００Ｇｂｉｔ／ｉｎ２の面密度から、将来は１Ｔｂｉｔ／ｉｎ２に達すると考えられている。１Ｔｂｉｔ／ｉｎ２に記録密度が達すると記録ｂｉｔのサイズが１０ｎｍを下回るようになり、その場合、熱揺らぎによる超常磁性化が問題となってくると予想され、現在使用されている磁気記録媒体の材料、例えばＣｏ−Ｃｒ基合金にＰｔを添加して結晶磁気異方性を高めた材料では十分ではないことが予想される。１０ｎｍ以下のサイズで安定的に強磁性として振る舞う磁性粒子は、より高い結晶磁気異方性を持っている必要があるからである。 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.

上記の理由から、Ｌ１０構造を持つＦｅＰｔ相が超高密度記録媒体用材料として注目されている。ＦｅＰｔ相は高い結晶磁気異方性とともに、耐食性、耐酸化性に優れているため、磁気記録媒体としての応用に適した材料と期待されているものである。そして、ＦｅＰｔ相を超高密度記録媒体用材料として使用する場合は、規則化したＦｅＰｔ磁性粒子を磁気的に孤立させた状態で出来るだけ高密度に方位をそろえて分散させるという技術の開発が求められている。 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.

このようなことから、Ｌ１０構造を有するＦｅＰｔ磁性粒子を酸化物や炭素といった非磁性材料で孤立させたグラニュラー構造磁性薄膜が、熱アシスト磁気記録方式を採用した次世代ハードディスクの磁気記録媒体用として、提案されている。このグラニュラー構造磁性薄膜は、磁性粒子同士が非磁性物質の介在により磁気的に絶縁される構造となっている。一般的に、Ｆｅ−Ｐｔ相を有するグラニュラー構造磁性薄膜はＦｅ−Ｐｔ系の焼結体スパッタリングターゲットを用いて成膜される。 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 structure magnetic thin film having an Fe—Pt phase is formed using an Fe—Pt-based sintered sputtering target.

Ｆｅ−Ｐｔ系の磁性材焼結体スパッタリングターゲットについて、本発明者らは以前Ｆｅ−Ｐｔ合金などの磁性相と、それを分離している非磁性相から構成されており、非磁性相の材料の一つとして金属酸化物を利用した強磁性材スパッタリングターゲットに関する技術を開示した（特許文献１）。
その他にも、特許文献２には、ＦｅＰｔ合金相中にＣ層が分散した組織を有した焼結体からなる磁気記録媒体膜形成用スパッタリングターゲットが開示されており、特許文献３には、ＳｉＯ２相とＦｅＰｔ合金相と相互拡散相とからなる磁気記録媒体膜形成用スパッタリングターゲットが開示されている。また、特許文献４には、Ｐｔ、ＳｉＯ２、Ｓｎ、残余がＦｅからなるＦｅ−Ｐｔ系強磁性材スパッタリングターゲットが開示されており、特許文献５には、Ｘ線回折におけるバックグラウンド強度に対する石英の（０１１）面のピーク強度比が１．４０以上である磁気記録膜用スパッタリングターゲットが開示されている。 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.

前記非磁性材料としての六方晶系ＢＮ（ボロンと窒素の化合物）は、潤滑剤として優れた性能を発揮するものの、粉末冶金の原料に用いる場合には、焼結性が悪いために、高密度の焼結体を製造することが難しい。そして、このような焼結体の密度が低い場合には、焼結体をターゲットに加工する際に割れやチッピングなどの不良を起こし、歩留まりを低下させるといった問題がある。また、密度が低いとターゲット中に多数の空孔が発生し、この空孔が異常放電の原因となって、スパッタリング中にパーティクル（基板上に付着するゴミ）を発生し、製品歩留まりを低下させるという問題があった。   Although the hexagonal BN (boron and nitrogen compound) as the non-magnetic material exhibits excellent performance as a lubricant, 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.

国際公開第ＷＯ２０１２／０２９４９８号International Publication No. WO2012 / 029498 特開２０１２−１０２３８７号公報JP 2012-102387 A 特開２０１１−２０８１６７号公報JP 2011-208167 A 国際公開第ＷＯ２０１２／０８６５７８号International Publication No. WO2012 / 085578 特許第５００９４４７号Patent No. 5009447

本発明は、熱アシスト磁気記録メディアの磁性薄膜の作製を可能にする、非磁性材料として六方晶系ＢＮを用いたＦｅ−Ｐｔ系焼結体を提供することであって、スパッタリング時に発生するパーティクル量を低減したスパッタリングターゲットを提供することを課題とする。   The present invention is to provide an Fe—Pt sintered body using hexagonal BN as a nonmagnetic material, which makes it possible to produce a magnetic thin film of a thermally assisted magnetic recording medium. It is an object to provide a sputtering target with a reduced amount.

上記課題を解決するために、本発明者らは鋭意研究を行った結果、非磁性材料である六方晶系ＢＮは二次元の結晶構造を有しているため、焼結体中において、この六方晶系ＢＮの結晶の向きがランダムになっていると、電気伝導に影響を及ぼし、異常放電を発生させるなど、スパッタリングを不安定にする原因となることを見出した。   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.

このような知見に基づき、本発明は、
１）ＢＮを含有するＦｅ−Ｐｔ系焼結体スパッタリングターゲットであって、スパッタ面に対して垂直断面における六方晶ＢＮ（００２）面のＸ線回折ピーク強度に対する、スパッタ面に対して水平面における六方晶ＢＮ（００２）面のＸ線回折ピーク強度の強度比が２以上であることを特徴とする焼結体スパッタリングターゲット、
２）スパッタ面に対して垂直断面における六方晶ＢＮ相の平均厚みが３０μｍ以下であることを特徴とする上記１）記載の焼結体スパッタリングターゲット、
３）Ｐｔ含有量が５ｍｏｌ％以上６０ｍｏｌ％以下であることを特徴とする上記１）又は２）記載の焼結体スパッタリングターゲット
４）ＢＮ含有量が１ｍｏｌ％以上６０ｍｏｌ％以下であることを特徴とする上記１）〜３）のいずれか一に記載の焼結体スパッタリングターゲット、
５）添加元素として、Ｃ、Ｒｕ、Ａｇ、Ａｕ、Ｃｕからなる群から選択した一種以上の元素を０．５ｍｏｌ％以上４０．０ｍｏｌ％以下含有することを特徴とする上記１）〜４）のいずれか一に記載の焼結体スパッタリングターゲット、
６）添加材として、酸化物、窒化物、炭化物、炭窒化物からなる群から選択した一種以上の無機物材料を含有することを特徴とする上記１）〜５）のいずれか一に記載の焼結体スパッタリングターゲット、
７）上記１）〜６）のいずれか一に記載のスパッタリングターゲットの製造方法において、薄片状あるいは板状の原料粉末を混合し、これを成形した後、この成形体を一軸加圧焼結することを特徴とするスパッタリングターゲットの製造方法、を提供する。 Based on such knowledge, the present invention
1) Fe—Pt sintered sputtering target containing BN, which is hexagonal in the horizontal plane with respect to the sputter plane, with respect to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the cross section perpendicular to the sputter plane. 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 body sputtering target according to any one of 1) to 3) above,
5) The additive element according to 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) In the method for producing a sputtering target according to any one of 1) to 6) above, flaky or plate-like raw material powders are mixed and molded, and then the compact is uniaxially pressed and sintered. There is provided a method for producing a sputtering target characterized by the above.

本発明の非磁性材料としてＢＮを用いたＦｅ−Ｐｔ系焼結体は、六方晶ＢＮの配向性を改善することにより、スパッタリング中の異常放電を抑制することができ、発生するパーティクル量を低減できるという優れた効果を有する。   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.

実施例１のターゲット（スパッタ面に対して水平面とスパッタ面に対して垂直断面）の顕微鏡写真である。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). 実施例２のターゲット（スパッタ面に対して水平面とスパッタ面に対して垂直断面）の顕微鏡写真である。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. 実施例３のターゲット（スパッタ面に対して水平面とスパッタ面に対して垂直断面）の顕微鏡写真である。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). 比較例１のターゲット（スパッタ面に対して水平面とスパッタ面に対して垂直断面）の顕微鏡写真である。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). 実施例１のターゲット（スパッタ面に対して水平面）のＸ線回折プロファイルである（最上段）。It is an X-ray diffraction profile of the target of Example 1 (horizontal plane with respect to the sputtering surface) (uppermost stage). 実施例１のターゲット（スパッタ面に対して垂直段面）のＸ線回折プロファイルである（最上段）。It is an X-ray diffraction profile of the target of Example 1 (a step surface perpendicular to the sputtering surface) (the uppermost step). 実施例２のターゲット（スパッタ面に対して水平面）のＸ線回折プロファイルである（最上段）。It is an X-ray-diffraction profile of the target of Example 2 (horizontal surface with respect to a sputtering surface) (top stage). 実施例２のターゲット（スパッタ面に対して垂直断面）のＸ線回折プロファイルである（最上段）。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). 実施例３のターゲット（スパッタ面に対して水平面）のＸ線回折プロファイルである（最上段）。It is an X-ray-diffraction profile of the target of Example 3 (horizontal surface with respect to a sputtering surface) (top stage). 実施例３のターゲット（スパッタ面に対して垂直断面）のＸ線回折プロファイルである（最上段）。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). 比較例１のターゲット（スパッタ面に対して水平面）のＸ線回折プロファイルである（最上段）。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). 比較例１のターゲット（スパッタ面に対して垂直断面）のＸ線回折プロファイルである（最上段）。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).

非磁性材料である六方晶系ＢＮは、二次元の結晶構造を有しているため、ターゲットにおいて、この六方晶系ＢＮの結晶の向きがランダムになっていると、電気伝導に影響を及ぼし、スパッタリングが不安定になることがある。したがって、この六方晶系ＢＮの結晶の向きを一方向に揃えることにより、安定的なスパッタリングを可能にすることができる。   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.

すなわち、本発明のＦｅ−Ｐｔ系焼結体スパッタリングターゲットは、非磁性材料として六方晶ＢＮを含有し、スパッタ面に対して垂直断面における六方晶ＢＮ（００２）面のＸ線回折ピーク強度に対する、スパッタ面に対して水平面における六方晶ＢＮ（００２）面のＸ線回折ピーク強度の強度比を２以上とする。 That is, the Fe—Pt-based sintered sputtering target of the present invention contains hexagonal BN as a nonmagnetic material, with respect to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in a cross section perpendicular to the sputtering plane. The intensity ratio of the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the horizontal plane with respect to the sputtering plane is set to 2 or more.

また、本発明のＦｅ−Ｐｔ系焼結体スパッタリングターゲットにおいて、六方晶ＢＮ相が薄片状又は板状であることが好ましく、より好ましくは、スパッタ面に対して垂直断面における六方晶ＢＮ相の平均厚みが３０μｍ以下である。これにより、六方晶ＢＮに起因する電気伝導の影響を低減することができ、安定的なスパッタリングを実施することが可能となる。   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.

本発明は、Ｐｔ含有量を５ｍｏｌ％以上６０ｍｏｌ％以下とするのが好ましい。Ｐｔ含有量を５ｍｏｌ％以上６０ｍｏｌ％以下とすることで、良好な磁気特性が得られる。また、六方晶ＢＮの含有量を１ｍｏｌ％以上６０ｍｏｌ％以下とするのが好ましい。非磁性材料としてのＢＮ含有量を１ｍｏｌ％以上６０ｍｏｌ％以下とすることで、磁気的な絶縁を向上させることができる。
なお、本発明のＦｅ−Ｐｔ系焼結体スパッタリングターゲットにおいて、Ｐｔや六方晶ＢＮ、後述する添加元素や添加材を除き、残部はＦｅである。 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, additive elements and additives described later.

また、本発明は、添加元素として、Ｃ、Ｒｕ、Ａｇ、Ａｕ、Ｃｕからなる群から選択した一種以上の元素を総量で０．５ｍｏｌ％以上４０．０ｍｏｌ％以下添加することが好ましい。また、添加材として、酸化物、窒化物、炭化物、炭窒化物からなる群から選択した一種以上の無機物材料を添加することが好ましい。これらの添加元素や添加材は、スパッタ後の膜の磁気特性を向上させるために有効な成分である。   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.

本発明のＦｅ−Ｐｔ系磁性材焼結体は、例えば、次の方法で作製することができる。
まず、各原料粉末（Ｆｅ粉末、Ｐｔ粉末、ＢＮ粉末）を用意する。また、原料粉末として、合金粉末（Ｆｅ−Ｐｔ粉）を用いてもよい。Ｐｔを含む合金粉末はその組成にもよるが、原料粉末中の酸素量を少なくするために有効である。さらに、必要に応じて、上記に掲げた添加成分である各原料粉末を用意する。 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, you may use alloy powder (Fe-Pt powder) as 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.

次に、金属粉末（Ｆｅ粉末、Ｐｔ粉末）あるいは合金粉末（Ｆｅ−Ｐｔ合金粉末）をボールミルや媒体攪拌ミルなどを用いて粉砕する。通常、このような金属の原料粉末は、球状、塊状、その他不定形のものが使用されるが、六方晶ＢＮは板状あるいは薄片状をしているため、これらを混合して焼結すると、焼結体における六方晶ＢＮの向きを揃えることは困難となる。そのため、金属の原料粉末を粉砕によって板状あるいは薄片状とすることにより、金属原料と六方晶ＢＮとを相互に積み重なるような構造とすることができ、六方晶ＢＮの配向を揃えることが可能となる。   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 aligned. Become.

このように粉砕処理して得られた金属粉末あるいは合金粉末と六方晶ＢＮ粉末とを乳鉢、媒体攪拌ミル、篩などを用いて混合する。添加成分や添加材については、金属の原料粉末と一緒に投入したり、六方晶ＢＮ粉末と一緒に投入したり、あるいは、金属の原料粉末と六方晶ＢＮ粉末とを混合した段階で投入することができる。
その後、この混合粉末をホットプレスで成型・焼結する。ホットプレス以外にも、プラズマ放電焼結法、熱間静水圧焼結法を使用することもできる。焼結時の保持温度は、スパッタリングターゲットの組成にもよるが、多くの場合、８００°Ｃ〜１４００°Ｃの温度範囲とする。 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. Although the holding temperature at the time of sintering depends on the composition of the sputtering target, it is often in the temperature range of 800 ° C. to 1400 ° C.

次に、ホットプレスから取り出した焼結体に熱間等方加圧加工を施す。熱間等方加圧加工は焼結体の密度向上に有効である。熱間等方加圧加工時の保持温度は焼結体の組成にもよるが、多くの場合、８００°Ｃ〜１２００°Ｃの温度範囲である。また加圧力は１００ＭＰａ以上に設定する。そして、このようにして得られた焼結体を旋盤で所望の形状に加工することにより、スパッタリングターゲットを作製できる。
以上により、六方晶ＢＮを含有し、スパッタ面に対して垂直断面における六方晶ＢＮ（００２）面のＸ線回折ピーク強度に対する、スパッタ面に対して水平面における六方晶ＢＮ（００２）面のＸ線回折ピーク強度の強度比が２以上であることを特徴とするＦｅ−Ｐｔ系焼結体スパッタリングターゲットを作製することができる。
結晶配向性の評価については、Ｘ線回折装置を用いて、スパッタリングターゲット用焼結体のスパッタ面に対して水平面とスパッタ面に対して垂直断面のＸ線回折強度を次の測定条件で測定した。装置：株式会社リガク社製（ＵｌｔｉｍａIV ｐｒｏｔｅｃｔｕｓ）、管球：Ｃｕ、管電圧：４０ｋＶ、管電流：３０ｍＡ、走査範囲（２θ）：１０°〜９０°、測定ステップ（２θ）：０．０１°、スキャンスピード（２θ）：毎分１°、スキャンモード２θ／θ。なお、六方晶ＢＮ（００２）面の回折ピークは（２θ）：２６．７５°付近に現れる。 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-rays of the hexagonal BN (002) plane in the horizontal plane with respect to the sputter plane with respect to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the cross section perpendicular to the sputter plane are 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 °.

以下、実施例および比較例に基づいて説明する。なお、本実施例はあくまで一例であり、この例によって何ら制限されるものではない。すなわち、本発明は特許請求の範囲によってのみ制限されるものであり、本発明に含まれる実施例以外の種々の変形を包含するものである。   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.

（実施例１）
原料粉として、Ｆｅ−Ｐｔ合金粉末、六方晶ＢＮ粉末（薄片状）を用意し、これらの粉末を７０（５０Ｆｅ−５０Ｐｔ）−３０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末とＢＮ粉末とをＶ型混合機で混ぜ合わせた後、さらに１５０μｍ目の篩を用いて混合し、この混合粉末をカーボン製の型に充填しホットプレスした。
ホットプレスの条件は、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果を図１に示す。図１より、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのが分かる。また、図１から六方晶ＢＮ相の平均厚みが３μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は６５７であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は５４であって、その強度比は１２．２であった。
次にこの焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、スパッタリングを行った。スパッタリングの条件は、投入電力１ｋＷ、Ａｒガス圧１．７Ｐａとし、２ｋＷｈｒのプレスパッタリングを実施した後、４インチ径のＳｉ基板上に２０秒間成膜した。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は２５０個と良好な結果が得られた。 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 with respect to the sputtering surface is 657, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 with 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.

（実施例２）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、ＳｉＯ２粉末を用意した。これらの粉末を７０（５０Ｆｅ−５０Ｐｔ）−５ＳｉＯ２−２５ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末とＳｉＯ２粉末とを粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末とＢＮ粉末とをＶ型混合機で混ぜ合わせた後、さらに１００μｍ目の篩を用いて混合し、この混合粉末をカーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内ＳＥＭによって観察した。その結果を図２に示す。図２より、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのが分かる。また、図２から六方晶ＢＮ相の平均厚みが９μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は５６６であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４５であって、その強度比は１２．６であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は３０個と良好な結果が得られた。 (Example 2)
Fe-Pt alloy powder, BN powder (flakes), and SiO 2 powder were prepared as raw material powders. It was weighed these powders so that 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 surface is 566, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（実施例３）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、Ａｇ粉末、Ｃ（薄片化黒鉛）粉末を用意した。これらの粉末を５８（３５Ｆｅ−１０Ｐｔ）−２０Ａｇ−２０ＢＮ−２Ｃ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末とＣ粉末とＡｇ粉末とをＶ型混合機で混ぜ合わせた後、乳鉢にて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果を図３に示す。図３より、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのが分かる。また、図３から六方晶ＢＮ相の平均厚みが２．２μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は３２７であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４５であって、その強度比は７．３であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数２５個と良好な結果が得られた。 (Example 3)
Fe-Pt alloy powder, BN powder (flaky shape), Ag powder, and C (flaky graphite) powder were prepared as raw material powder. 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 sputter plane is 327, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputter 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 by 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.

（実施例４）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、Ａｇ粉末を用意した。これらの粉末を５５（４５Ｆｅ−４５Ｐｔ−１０Ａｇ）−４５ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末とＡｇ粉末をＶ型混合機で混ぜ合わせた後、さらに１５０μｍ目の篩を用いて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのを確認した。また、六方晶ＢＮ相の平均厚みが６μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は７１３であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は５２であって、その強度比は１３．７であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数８３個と良好な結果が得られた。 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 with respect to the sputtering surface is 713, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（実施例５）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、Ａｇ粉末、ＳｉＯ２粉末を用意した。これらの粉末を８０（５０Ｆｅ−４０Ｐｔ−１０Ａｇ）−５ＳｉＯ２−１５ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末とＡｇ粉末とＳｉＯ２をＶ型混合機で混ぜ合わせた後、乳鉢にて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのを確認した。また、六方晶ＢＮ相の平均厚みが２．４μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は１５８であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４６であって、その強度比は３．４であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数２５個と良好な結果が得られた。 (Example 5)
Fe—Pt alloy powder, BN powder (flaky shape), Ag powder, and SiO 2 powder were prepared as raw material powders. It was weighed these powders so that 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 with respect to the sputter plane is 158, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputter 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 by 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.

（実施例６）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、Ｃｕ粉末を用意した。これらの粉末を８０（５０Ｆｅ−４５Ｐｔ−５Ｃｕ）−２０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末とＣｕ粉末をＶ型混合機で混ぜ合わせた後、さらに１５０μｍ目の篩を用いて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのを確認した。また、六方晶ＢＮ相の平均厚みが３μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は４９８であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４３であって、その強度比は１１．６であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数１２６個と良好な結果が得られた。 (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 surface is 498, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（実施例７）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、Ａｕ粉末を用意した。これらの粉末を８０（５０Ｆｅ−４５Ｐｔ−５Ａｕ）−２０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末とＡｕ粉末をＶ型混合機で混ぜ合わせた後、さらに１５０μｍ目の篩を用いて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのを確認した。また、六方晶ＢＮ相の平均厚みが２．５μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は５２３であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４６であって、その強度比は１１．４であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数１７４個と良好な結果が得られた。 (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 cross section perpendicular 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 by 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.

（実施例８）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、Ｒｕ粉末、ＳｉＯ２粉末、ＴｉＯ２粉末を用意した。これらの粉末を７４（４８Ｆｅ−４８Ｐｔ−４Ｒｕ）−３ＳｉＯ２−３ＴｉＯ２−２０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末とＲｕ粉末とＳｉＯ２粉末とＴｉＯ２粉末をＶ型混合機で混ぜ合わせた後、乳鉢にて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのを確認した。また、六方晶ＢＮ相の平均厚みが２．４μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は３６９であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４２であって、その強度比は８．８であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数３６個と良好な結果が得られた。 (Example 8)
Fe-Pt alloy powder, BN powder (flakes), Ru powder, SiO 2 powder, and TiO 2 powder were prepared as raw material powders. It was weighed these powders so that 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 cross section perpendicular 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 by 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.

（実施例９）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、Ｃｒ２Ｏ３粉末を用意した。これらの粉末を７５（５５Ｆｅ−４５Ｐｔ）−５Ｃｒ２Ｏ３−２０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末とＣｒ２Ｏ３粉末をＶ型混合機で混ぜ合わせた後、乳鉢にて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのを確認した。また、六方晶ＢＮ相の平均厚みが３．２μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は２５２であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４８であって、その強度比は５．３であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数７６個と良好な結果が得られた。 Example 9
Fe-Pt alloy powder, BN powder (flakes), and Cr 2 O 3 powder were prepared as raw material powders. It was weighed these powders so that 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 surface is 252 and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（実施例１０）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、Ａｇ粉末、ＴｉＮ粉末を用意した。これらの粉末を７５（４５Ｆｅ−５５Ｐｔ−１０Ａｇ）−３ＴｉＮ−２２ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末とＴｉＮ粉末をＶ型混合機で混ぜ合わせた後、乳鉢にて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのを確認した。また、六方晶ＢＮ相の平均厚みが５μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は２８９であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４３であって、その強度比は６．７であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数１２９個と良好な結果が得られた。 (Example 10)
Fe-Pt alloy powder, BN powder (flakes), Ag powder, and TiN powder were prepared as raw material powders. These powders were weighed so as 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 vertical section 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 by 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.

（実施例１１）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）、Ａｇ粉末、ＳｉＣ粉末を用意した。これらの粉末を７５（４５Ｆｅ−５５Ｐｔ−１０Ａｇ）−３ＴｉＮ−２２ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末とＳｉＣ粉末をＶ型混合機で混ぜ合わせた後、乳鉢にて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのを確認した。また、六方晶ＢＮ相の平均厚みが４．２μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は３０４であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４９であって、その強度比は６．２であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数１３７個と良好な結果が得られた。 (Example 11)
Fe-Pt alloy powder, BN powder (flakes), Ag powder, and SiC powder were prepared as raw material powders. These powders were weighed so as 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 surface is 304, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（実施例１２）
原料粉として、Ｆｅ−Ｐｔ合金粉末、ＢＮ粉末（薄片状）を用意した。これらの粉末を４０（５５Ｆｅ−４５Ｐｔ）−６０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、Ｆｅ−Ｐｔ合金粉末を粉砕媒体のジルコニアボールと共に容量５Ｌの媒体攪拌ミルに投入し、２時間、回転数３００ｒｐｍで処理した。処理後のＦｅ−Ｐｔ合金粉末の平均粒子径は１０μｍであった。そして媒体攪拌ミルから取り出した粉末と、ＢＮ粉末をＶ型混合機で混ぜ合わせた後、さらに１５０μｍ目の篩を用いて混合し、カーボン製の型に充填しホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度９５０°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、９５０°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向では層状構造になっておりＢＮが配向しているのを確認した。また、六方晶ＢＮ相の平均厚みが９．５μｍであった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は８１０であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は５３であって、その強度比は１５．３であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数３５８個と良好な結果が得られた。 (Example 12)
Fe-Pt alloy powder and BN powder (flaky shape) 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 surface is 810, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（比較例１）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）、Ｃ粉末を用意した。これらの粉末を６０（３０Ｆｅ−７０Ｐｔ）−５ＢＮ−３５Ｃ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果を図４に示す。図４から、スパッタ面に対して垂直断面方向には層状構造にはなっていないことが分かった。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は５２であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４４であって、その強度比は１．２であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は１１００個と、実施例に比べて著しく増加していた。 (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 surface is 52, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（比較例２）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）、Ａｇ粉末を用意した。これらの粉末を５５（４５Ｆｅ−４５Ｐｔ−１０Ａｇ）−４５ＢＮ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向には層状構造にはなっていないことを確認した。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は６７であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は５２であって、その強度比は１．３であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は８６０個と、実施例に比べて著しく増加していた。 (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 sputter plane is 67, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputter 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 by 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.

（比較例３）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）、Ａｇ粉末、ＳｉＯ２粉末を用意した。これらの粉末を８０（５０Ｆｅ−４０Ｐｔ−１０Ａｇ）−５ＳｉＯ２−１５ＢＮ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向には層状構造にはなっていないことを確認した。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は５８であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４６であって、その強度比は１．３であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は７１２個と、実施例に比べて著しく増加していた。 (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. It was weighed these powders so that 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 with respect to the sputtering surface is 58, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（比較例４）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）、Ｃｕ粉末を用意した。これらの粉末を８０（５０Ｆｅ−４５Ｐｔ−５Ｃｕ）−２０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向には層状構造にはなっていないことを確認した。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は７１であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４３であって、その強度比は１．７であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は６１６個と、実施例に比べて著しく増加していた。 (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 sputter surface is 71, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputter surface 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 by 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.

（比較例５）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）、Ａｕ粉末を用意した。これらの粉末を８０（５０Ｆｅ−４５Ｐｔ−５Ａｕ）−２０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向には層状構造にはなっていないことを確認した。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は６４であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４６であって、その強度比は１．４であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は７３２個と、実施例に比べて著しく増加していた。 (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 vertical section 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 by 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.

（比較例６）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）、Ｒｕ粉末、ＴｉＯ２粉末、ＳｉＯ２粉末を用意した。これらの粉末を７４（４８Ｆｅ−４８Ｐｔ−４Ｒｕ）−３ＴｉＯ２−３ＳｉＯ２−２０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向には層状構造にはなっていないことを確認した。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は４６であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４２であって、その強度比は１．１であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は１０４７個と、実施例に比べて著しく増加していた。 (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. It was weighed these powders so that 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 surface is 46, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（比較例７）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）、Ｃｒ２Ｏ３粉末を用意した。これらの粉末を７５（５５Ｆｅ−４５Ｐｔ）−５Ｃｒ２Ｏ３−２０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向には層状構造にはなっていないことを確認した。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は５２であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４８であって、その強度比は１．１であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は８２３個と、実施例に比べて著しく増加していた。 (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. It was weighed these powders so that 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 surface is 52, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（比較例８）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）、Ａｇ粉末、ＴｉＮ粉末を用意した。これらの粉末を７５（４５Ｆｅ−５５Ｐｔ−１０Ａｇ）−３ＴｉＮ−２２ＢＮ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向には層状構造にはなっていないことを確認した。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は５３であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４３であって、その強度比は１．２であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は１０７９個と、実施例に比べて著しく増加していた。 (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 so as 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 surface is 53, and the X-ray diffraction peak intensity of the BN (002) plane in the cross section perpendicular to the sputtering surface 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 by 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.

（比較例９）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）、Ａｇ粉末、ＳｉＣ粉末を用意した。これらの粉末を７５（４５Ｆｅ−５５Ｐｔ−１０Ａｇ）−３ＳｉＣ−２２ＢＮ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向には層状構造にはなっていないことを確認した。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は７７であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は４９であって、その強度比は１．６であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は１０５５個と、実施例に比べて著しく増加していた。 (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 vertical section 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 by 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.

（比較例１０）
原料粉として、平均粒子径５μｍのＦｅ粉末、平均粒子径６μｍのＰｔ粉末、ＢＮ粉末（薄片状）を用意した。これらの粉末を４０（５５Ｆｅ−４５Ｐｔ）−６０ＢＮ（ｍｏｌ％）となるように秤量した。
次に、秤量した粉末をＶ型混合機で混ぜ合わせた後、乳鉢で混合し、カーボン製の型に充填し、ホットプレスした。
ホットプレスの条件は、実施例１と同様に、真空雰囲気、昇温速度３００°Ｃ／時間、保持温度１２００°Ｃ、保持時間２時間とし、昇温開始時から保持終了まで３０ＭＰａで加圧した。保持終了後はチャンバー内でそのまま自然冷却させた。
次にホットプレスの型から取り出した焼結体に熱間等方加圧加工を施した。熱間等方加圧加工の条件は、実施例１と同様に、昇温速度３００°Ｃ／時間、保持温度１１００°Ｃ、保持時間２時間とし、昇温開始時からＡｒガスのガス圧を徐々に高めて、１１００°Ｃで保持中は１５０ＭＰａで加圧した。保持終了後は炉内でそのまま自然冷却させた。
こうして得られた焼結体の端部を切り出し、その断面をＳＥＭによって観察した。その結果、スパッタ面に対して垂直断面方向には層状構造にはなっていないことを確認した。次に、Ｘ線回折法（ＸＲＤ）を用いて焼結体の断面を測定した。その結果、スパッタ面に対して水平面のＢＮ（００２）面のＸ線回折ピーク強度は８２であり、スパッタ面に対して垂直断面のＢＮ（００２）面のＸ線回折ピーク強度は５３であって、その強度比は１．５であった。
次に焼結体を直径１８０．０ｍｍ、厚さ５．０ｍｍの形状へ旋盤で切削加工した後、マグネトロンスパッタ装置（キヤノンアネルバ製Ｃ−３０１０スパッタリングシステム）に取り付け、実施例１と同様の条件で、スパッタリングを行った。そして基板上へ付着したパーティクルの個数をパーティクルカウンターで測定した。このときのパーティクル個数は２５３０個と、実施例に比べて著しく増加していた。 (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 vertical section 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 by 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.

本発明の非磁性材料としてＢＮを用いたＦｅ−Ｐｔ系焼結体は、スパッタリング時に発生するパーティクル量を低減したスパッタリングターゲットを提供できる優れた効果を有する。したがって、グラニュラー構造の磁性薄膜の成膜に用いられるスパッタリングターゲットとして有用である。   The Fe—Pt-based 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)

ＢＮを含有するＦｅ−Ｐｔ系焼結体スパッタリングターゲットであって、スパッタ面に対して垂直断面における六方晶ＢＮ（００２）面のＸ線回折ピーク強度に対する、スパッタ面に対して水平面における六方晶ＢＮ（００２）面のＸ線回折ピーク強度の強度比が２以上であることを特徴とする焼結体スパッタリングターゲット。   A Fe—Pt-based sintered sputtering target containing BN, which has hexagonal BN in the horizontal plane with respect to the sputter plane with respect to the X-ray diffraction peak intensity of the hexagonal BN (002) plane in the cross section perpendicular to the sputter plane. A sintered body sputtering target, wherein the intensity ratio of the X-ray diffraction peak intensity of the (002) plane is 2 or more. スパッタ面に対して垂直断面における六方晶ＢＮ相の平均厚みが３０μｍ以下であることを特徴とする請求項１記載の焼結体スパッタリングターゲット。   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. Ｐｔ含有量が５ｍｏｌ％以上６０ｍｏｌ％以下であることを特徴とする請求項１又は２記載の焼結体スパッタリングターゲット。   Pt content is 5 mol% or more and 60 mol% or less, The sintered compact sputtering target of Claim 1 or 2 characterized by the above-mentioned. ＢＮ含有量が１ｍｏｌ％以上６０ｍｏｌ％以下であることを特徴とする請求項１〜３のいずれか一項に記載の焼結体スパッタリングターゲット。   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. 添加元素として、Ｃ、Ｒｕ、Ａｇ、Ａｕ、Ｃｕからなる群から選択した一種以上の元素を０．５ｍｏｌ％以上４０．０ｍｏｌ％以下含有することを特徴とする請求項１〜４のいずれか一項に記載の焼結体スパッタリングターゲット。   One or more elements selected from the group consisting of C, Ru, Ag, Au, and Cu are contained as additive elements in an amount of 0.5 mol% to 40.0 mol%, respectively. The sintered compact sputtering target according to Item. 添加材として、酸化物、窒化物、炭化物、炭窒化物からなる群から選択した一種以上の無機物材料を含有することを特徴とする請求項１〜５のいずれか一項に記載の焼結体スパッタリングターゲット。   The sintered body according to any one of claims 1 to 5, wherein the additive includes one or more inorganic materials selected from the group consisting of oxides, nitrides, carbides, and carbonitrides. Sputtering target. 請求項１〜６のいずれか一項に記載のスパッタリングターゲットの製造方法において、薄片状あるいは板状の原料粉末を混合し、これを成形した後、この成形体を一軸加圧焼結することを特徴とするスパッタリングターゲットの製造方法。 In the manufacturing method of the sputtering target as described in any one of Claims 1-6, after mixing a flaky or plate-shaped raw material powder and shape | molding this, it is carrying out uniaxial pressure sintering of this molded object. A method for producing a sputtering target.
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