WO2021039711A1 - Fe-co-si-b-nb-based target - Google Patents

Fe-co-si-b-nb-based target Download PDF

Info

Publication number
WO2021039711A1
WO2021039711A1 PCT/JP2020/031823 JP2020031823W WO2021039711A1 WO 2021039711 A1 WO2021039711 A1 WO 2021039711A1 JP 2020031823 W JP2020031823 W JP 2020031823W WO 2021039711 A1 WO2021039711 A1 WO 2021039711A1
Authority
WO
WIPO (PCT)
Prior art keywords
target
powder
present
vickers hardness
alloy powder
Prior art date
Application number
PCT/JP2020/031823
Other languages
French (fr)
Japanese (ja)
Inventor
福岡　淳
Original Assignee
日立金属株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 日立金属株式会社 filed Critical 日立金属株式会社
Priority to JP2021542883A priority Critical patent/JPWO2021039711A1/ja
Publication of WO2021039711A1 publication Critical patent/WO2021039711A1/en

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering

Definitions

  • the present invention relates to, for example, a Fe-Co-Si-B-Nb-based target used for forming a soft magnetic film.
  • Patent Document 1 As a soft magnetic film suitable for a core material such as a magnetic head, Fe is a main component, a metal element selected from the group consisting of Nb, Nb-Ta and Ta, and B (boron). A soft magnetic film containing a metalloid element selected from the group consisting of B-Si and N (nitrogen) has been proposed.
  • This soft magnetic film composed of Fe-Si-B-Nb-N is superior to the conventional soft magnetic film made of Co-Nb-Zr alloy in terms of low coercive force, low magnetostriction and high saturation magnetic flux density. It is a useful technique in that it has soft magnetic properties and good thermal stability, and is also excellent in corrosion resistance and abrasion resistance.
  • the soft magnetic film composed of the above-mentioned Fe—Si—B—Nb—N system can be formed by, for example, a sputtering method.
  • Fe-Si- having Fe as a main component and containing a metal element selected from the group consisting of Nb, Nb-Ta and Ta and a metalloid element selected from the group consisting of B and B-Si- A method in which a B—Nb alloy is used as a target and nitrogen gas is periodically mixed with an inert sputter gas such as Ar to form a film whose composition is modulated in the film thickness direction, and then heat-treated.
  • an inert sputter gas such as Ar
  • the Fe—Si—B—Nb alloy target disclosed in Patent Document 1 is a so-called difficult-to-cut material in which the target body is likely to crack, chip, or fall off during machining to the shape and dimensions of the target. Is. For this reason, during machining, the tip of the cutting tool may be worn or damaged, causing unevenness on the surface of the obtained target, or in some cases, damaging the target body.
  • An object of the present invention is to suppress wear and breakage of a cutting tool tip in machining a Fe-Si-B-Nb-based target (hereinafter, also simply referred to as "target"), and to prevent cracks and chips in the target body. It is an object of the present invention to provide a Fe—Co—Si—B—Nb-based target capable of suppressing the generation and suppressing the generation of irregularities on the target surface.
  • the target of the present invention has a composition formula in atomic ratio (Fe 1-ab Co a Ni b ) 100-XYZ Si X BY Nb Z , a ⁇ 0.95, b ⁇ 0.30, It is represented by 15 ⁇ X + Y ⁇ 35, 0.3 ⁇ X / Y ⁇ 2.0, 1 ⁇ Z ⁇ 20, and the balance is composed of unavoidable impurities, and the Vickers hardness measured at 5 measurement points. The average value is 250 to 1100 HV.
  • the target of the present invention preferably has an average value of Vickers hardness of 500 to 1000 HV measured at the above five measurement points.
  • the present invention in machining a target, it is possible to suppress wear and breakage of a cutting tool tip, suppress the occurrence of cracks and chips in the target body, and suppress the occurrence of irregularities on the target surface. Therefore, it is a useful technique for manufacturing a member having excellent soft magnetic properties, thermal stability, corrosion resistance, wear resistance and the like described above.
  • the target of the present invention has a Vickers hardness in the range of 250 to 1100 HV as defined by JIS Z 2244.
  • the target of the present invention is a machining process such as cutting or polishing to make the target shape and dimension by setting the average value of Vickers hardness measured at five measurement points in a specific range of 250 to 1100 HV.
  • the target of the present invention becomes a target having a smooth surface, and it is possible to suppress the induction of abnormal discharge and the scattering of nodules and adhesion to the material to be treated.
  • all of the Vickers hardness measured at the above five measurement points is set to a specific range of 250 to 1100 HV.
  • the target of the present invention by setting the Vickers hardness to 250 HV or more, it is possible to suppress the generation of a built edge on a tip such as a milling machine or a lathe. That is, in addition to the fact that the target of the present invention is prevented from gradually increasing the depth of cut of the insert as the constituent cutting edge grows as the cutting process progresses, and the dimensional difference of the target can be reduced between the start of cutting and the completion of cutting. It is also possible to suppress damage to the tip due to peeling of the built-up edge.
  • the target of the present invention has a Vickers hardness of 250 HV or more.
  • the target according to the embodiment of the present invention preferably has a Vickers hardness of 500 HV or more, and more preferably 550 HV or more.
  • the target of the present invention has a Vickers hardness of 1100 HV or less, so that the amount of wear of chips such as a milling machine and a lathe can be suppressed, for example. That is, in addition to being able to suppress that the cutting amount of the tip due to the wear of the tip gradually decreases as the cutting process progresses, and the dimensional difference of the target becomes large at the start of cutting and at the completion of cutting. It is also possible to suppress damage to the chip.
  • the target according to the embodiment of the present invention preferably has a Vickers hardness of 1000 HV or less, and more preferably 950 HV or less.
  • the Vickers hardness referred to in the present invention has any five points on the erosion surface of the target from the viewpoint of suppressing the occurrence of cracks and chips of the target body as described above and also suppressing the occurrence of abnormal discharge during film formation. It means that the average value of Vickers hardness measured at the measurement point is in the range of 250 to 1100 HV. Then, the Vickers hardness is measured at a total of five positions in the plane direction of the erosion surface of the target, which are arbitrary four positions corresponding to the outer peripheral portion and positions corresponding to the central portion. At this time, the load is 9.8 N and the pressurization time is 10 seconds. Further, the target according to the embodiment of the present invention preferably does not have a Fe—Si—B—Nb-based composite compound phase in the metal structure from the viewpoint of setting the Vickers hardness to 250 to 1100 HV.
  • the target of the present invention has a composition formula in atomic ratio (Fe 1-ab Co a Ni b ) 100-XYZ Si X BY Nb Z , a ⁇ 0.95, b ⁇ 0.30, It is represented by 15 ⁇ X + Y ⁇ 35, 0.3 ⁇ X / Y ⁇ 2.0, and 1 ⁇ Z ⁇ 20, and the balance is composed of unavoidable impurities.
  • the contents of Co, Ni, Si, B, and Nb can be appropriately adjusted within a range that does not significantly impair soft magnetic properties, thermal stability, corrosion resistance, and wear resistance.
  • a soft magnetic film having a low coercive force can be obtained by setting the total amount of Si and B, that is, X + Y in the composition formula to 15 or more.
  • the target according to the embodiment of the present invention preferably has X + Y of 20 or more for the same reason as described above. Further, the target of the present invention can obtain a soft magnetic film having a high saturation magnetic flux density by setting X + Y to 35 or less.
  • the target according to the embodiment of the present invention preferably has X + Y of 33 or less for the same reason as described above.
  • the target of the present invention is to obtain a soft magnetic film having thermal stability by setting the ratio of Si and B, that is, X / Y of the composition formula to 0.3 or more and 2.0 or less.
  • the target according to the embodiment of the present invention preferably has an X / Y of 0.7 or more and 1.6 or less for the same reason as described above.
  • a soft magnetic film having corrosion resistance can be obtained by setting the Nb content, that is, Z in the composition formula to 1 or more.
  • the target according to the embodiment of the present invention preferably has a Z of 3 or more for the same reason as described above.
  • a soft magnetic film having a high saturation magnetic flux density can be obtained by setting Z to 20 or less.
  • the target according to the embodiment of the present invention preferably has a Z of 10 or less for the same reason as described above.
  • the target of the present invention can also obtain the same effect as described above by substituting a part or all of Nb with Ta.
  • the target of the present invention can obtain a soft magnetic film having a high magnetic permeability by reducing magnetostriction by substituting a part of Fe with one or more elements selected from Co and Ni.
  • the amount of Co substituted with respect to Fe, that is, a in the composition formula is 0.95 or less.
  • the substitution amount of Ni with respect to Fe, that is, b in the composition formula is 0.30 or less.
  • the target according to the embodiment of the present invention preferably has a of 0.50 or more for the same reason as described above.
  • the target according to the embodiment of the present invention is preferable in that a soft magnetic film having a high saturation magnetic flux density can be obtained by setting a to 0.90 or less and b to 0.10 or less.
  • the target of the present invention can be obtained by, for example, a powder sintering method. Specifically, it can be obtained by pressure sintering a mixed powder in which a pure metal powder or an alloy powder is mixed so as to have the above-mentioned component composition.
  • a powder sintering method Specifically, it can be obtained by pressure sintering a mixed powder in which a pure metal powder or an alloy powder is mixed so as to have the above-mentioned component composition.
  • the alloy powder Fe—Si alloy powder, Fe—B alloy powder, Fe—Nb alloy powder, Fe—Si in order to prevent the structure from forming a Fe—Si—B—Nb-based composite compound phase as much as possible.
  • the pressure sintering is preferably performed under the conditions of a sintering temperature of 700 to 1300 ° C. and a pressure pressure of 30 to 200 MPa for 1 to 10 hours.
  • a sintering temperature of 700 to 1300 ° C.
  • a pressure pressure of 30 to 200 MPa for 1 to 10 hours.
  • the pressurizing pressure to 200 MPa or less
  • the introduction of residual stress to the target during sintering can be suppressed, and the occurrence of cracks after sintering can be suppressed.
  • the sintering time to 1 hour or more
  • the progress of sintering can be promoted and the generation of vacancies can be suppressed.
  • the sintering time to 10 hours or less, a decrease in production efficiency can be suppressed.
  • Fe powder, Co powder, Si powder, B powder and Nb powder were prepared, and the composition formula (Fe 0.70 Co 0.30 ) 67 Si 13.5 in atomic ratio was prepared.
  • Mixing was performed with a V-type mixer to obtain a mixed powder.
  • this mixed powder was filled in a capsule made of soft iron and degassed and sealed under the conditions of 450 ° C. for 4 hours.
  • the capsule was pressure-sintered by HIP under the conditions of 750 ° C., 122 MPa, and 1 hour to prepare a sintered body.
  • Fe powder, Co powder, Si powder, B powder and Nb powder were prepared, and the composition formula in atomic ratio (Fe 0.05 Co 0.95 ) 45 Si 23.3 was prepared.
  • Mixing was performed with a V-type mixer to obtain a mixed powder.
  • this mixed powder was filled in a capsule made of soft iron and degassed and sealed under the conditions of 450 ° C. for 4 hours.
  • the capsule was pressure-sintered by HIP under the conditions of 950 ° C., 122 MPa, and 1 hour to prepare a sintered body.
  • this mixed powder was filled in a capsule made of soft iron and degassed and sealed under the conditions of 450 ° C. for 4 hours.
  • the capsule was pressure-sintered by HIP under the conditions of 950 ° C., 122 MPa, and 1 hour to prepare a sintered body.
  • each of the sintered bodies obtained above was machined to prepare a target.
  • the targets according to the first to fifth aspects of the present invention do not crack during machining, and the surface after finishing is not uneven and the surface is smooth. It was confirmed that it was in a state.
  • the target as a comparative example could not be machined into the target shape due to cracks during machining.
  • the Vickers hardness was measured at four positions corresponding to the outer peripheral portion and a total of five positions corresponding to the central portion in the plane direction of the surface to be the erosion surface of the target. .. The measurement interval was set so that the indentations were not affected by the measurement. Then, the Vickers hardness was measured according to JIS Z 2244 using MVK-E manufactured by Akashi Seisakusho Co., Ltd. when the load was 9.8 N and the pressurization time was 10 seconds. The results are shown in Table 1.
  • the target of the present invention is a target in which cracks and chips are suppressed during machining, the surface after finishing is not uneven, and the surface is smooth. ..
  • the target of the present invention can be expected to be useful as a target for forming a soft magnetic film in which the induction of abnormal discharge and the scattering of nodules and adhesion to the material to be treated are suppressed.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Electromagnetism (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)
  • Powder Metallurgy (AREA)

Abstract

Provided is an Fe-Co-Si-B-Nb-based target which is such that abrasion and damage of the tip of a cutting tool, the occurrence of cracking and chipping of the target body, and formation of bumps and recesses on the target surface can be suppressed during machining of the target.　The Fe-Co-Si-B-Nb-based target has a composition formula, in terms of atomic ratio, expressed by (Fe1-a-bCoaNib)100-X-Y-ZSiXBYNbZ, wherein a ≤ 0.95, b ≤ 0.30, 15 ≤ X + Y ≤ 35, 0.3 ≤ X/Y ≤ 2.0, 1 ≤ Z ≤ 20 and the balance inevitable impurities, and has an average Vickers hardness value of 250 to 1,100 HV as measured at five measurement points. The Vickers hardness is preferably in the range of 500 to 1,000 HV.

Description

Ｆｅ－Ｃｏ－Ｓｉ－Ｂ－Ｎｂ系ターゲットFe-Co-Si-B-Nb system target
　本発明は、例えば、軟磁性膜を形成するために用いるＦｅ－Ｃｏ－Ｓｉ－Ｂ－Ｎｂ系ターゲットに関するものである。 The present invention relates to, for example, a Fe-Co-Si-B-Nb-based target used for forming a soft magnetic film.
　電子機器をはじめとする各種製品の小型化、軽量化が進んでおり、機能性薄膜が適用されている。例えば、特許文献１においては、磁気ヘッド等のコア材料に適した軟磁性膜として、Ｆｅを主成分とし、Ｎｂ、Ｎｂ－ＴａおよびＴａからなる群から選択された金属元素と、Ｂ（ボロン）およびＢ－Ｓｉからなる群より選択された半金属元素と、Ｎ（窒素）を含む軟磁性膜が提案されている。このＦｅ－Ｓｉ－Ｂ－Ｎｂ－Ｎで構成される軟磁性膜は、従来のＣｏ－Ｎｂ－Ｚｒ系合金からなる軟磁性膜よりも、低保磁力、低磁歪および高飽和磁束密度等の優れた軟磁気特性と良好な熱安定性を有しており、さらに耐食性および耐摩耗性にも優れている点で有用な技術である。 Various products such as electronic devices are becoming smaller and lighter, and functional thin films are being applied. For example, in Patent Document 1, as a soft magnetic film suitable for a core material such as a magnetic head, Fe is a main component, a metal element selected from the group consisting of Nb, Nb-Ta and Ta, and B (boron). A soft magnetic film containing a metalloid element selected from the group consisting of B-Si and N (nitrogen) has been proposed. This soft magnetic film composed of Fe-Si-B-Nb-N is superior to the conventional soft magnetic film made of Co-Nb-Zr alloy in terms of low coercive force, low magnetostriction and high saturation magnetic flux density. It is a useful technique in that it has soft magnetic properties and good thermal stability, and is also excellent in corrosion resistance and abrasion resistance.
　そして、上述したＦｅ－Ｓｉ－Ｂ－Ｎｂ－Ｎ系で構成される軟磁性膜は、例えば、スパッタ法により形成することができる。具体的には、Ｆｅを主成分とし、Ｎｂ、Ｎｂ－ＴａおよびＴａよりなる群から選択された金属元素と、ＢおよびＢ－Ｓｉよりなる群より選択された半金属元素を含むＦｅ－Ｓｉ－Ｂ－Ｎｂ系合金をターゲットとして用いて、Ａｒ等の不活性スパッタガス中に窒素ガスを周期的に混合することで、膜厚方向に組成変調させた膜を成膜し、その後、熱処理する方法が提案されている。 Then, the soft magnetic film composed of the above-mentioned Fe—Si—B—Nb—N system can be formed by, for example, a sputtering method. Specifically, Fe-Si- having Fe as a main component and containing a metal element selected from the group consisting of Nb, Nb-Ta and Ta and a metalloid element selected from the group consisting of B and B-Si- A method in which a B—Nb alloy is used as a target and nitrogen gas is periodically mixed with an inert sputter gas such as Ar to form a film whose composition is modulated in the film thickness direction, and then heat-treated. Has been proposed.
特開平２－１６３９１１号公報Japanese Unexamined Patent Publication No. 2-163911
　特許文献１に開示されるＦｅ－Ｓｉ－Ｂ－Ｎｂ系合金ターゲットは、ターゲットの形状寸法に加工する機械加工時に、ターゲット本体の割れや欠け、脱落が発生する可能性が高い、いわゆる難削材である。このため、機械加工時に、切削工具のチップの摩耗や破損を招き、得られるターゲットの表面に凹凸を誘発させたり、場合によっては、ターゲット本体を破損させてしまう場合がある。 The Fe—Si—B—Nb alloy target disclosed in Patent Document 1 is a so-called difficult-to-cut material in which the target body is likely to crack, chip, or fall off during machining to the shape and dimensions of the target. Is. For this reason, during machining, the tip of the cutting tool may be worn or damaged, causing unevenness on the surface of the obtained target, or in some cases, damaging the target body.
　本発明の目的は、Ｆｅ－Ｓｉ－Ｂ－Ｎｂ系ターゲット（以下、単に「ターゲット」ともいう。）の機械加工において、切削工具のチップの摩耗や破損を抑制し、ターゲット本体の割れや欠けの発生を抑制でき、ターゲット表面における凹凸の発生も抑制できる、Ｆｅ－Ｃｏ－Ｓｉ－Ｂ－Ｎｂ系ターゲットを提供することである。 An object of the present invention is to suppress wear and breakage of a cutting tool tip in machining a Fe-Si-B-Nb-based target (hereinafter, also simply referred to as "target"), and to prevent cracks and chips in the target body. It is an object of the present invention to provide a Fe—Co—Si—B—Nb-based target capable of suppressing the generation and suppressing the generation of irregularities on the target surface.
　本発明のターゲットは、原子比における組成式が（Ｆｅ１－ａ－ｂＣｏａＮｉｂ）１００－Ｘ－Ｙ－ＺＳｉＸＢＹＮｂＺ、ａ≦０．９５、ｂ≦０．３０、１５≦Ｘ＋Ｙ≦３５、０．３≦Ｘ／Ｙ≦２．０、１≦Ｚ≦２０で表わされ、残部が不可避的不純物からなり、５点の測定点で測定を行なったビッカース硬さの平均値が２５０～１１００ＨＶである。 The target of the present invention has a composition formula in atomic ratio (Fe 1-ab Co a Ni b ) 100-XYZ Si X BY Nb Z , a ≤ 0.95, b ≤ 0.30, It is represented by 15 ≦ X + Y ≦ 35, 0.3 ≦ X / Y ≦ 2.0, 1 ≦ Z ≦ 20, and the balance is composed of unavoidable impurities, and the Vickers hardness measured at 5 measurement points. The average value is 250 to 1100 HV.
　本発明のターゲットは、上記の５点の測定点で測定を行なったビッカース硬さの平均値が５００～１０００ＨＶであることが好ましい。 The target of the present invention preferably has an average value of Vickers hardness of 500 to 1000 HV measured at the above five measurement points.
　本発明は、ターゲットの機械加工において、切削工具のチップの摩耗や破損を抑制し、ターゲット本体の割れや欠けの発生を抑制でき、ターゲット表面における凹凸の発生も抑制できる。このため、上述した軟磁気特性、熱安定性、耐食性、耐摩耗性等に優れる部材の製造に有用な技術となる。 According to the present invention, in machining a target, it is possible to suppress wear and breakage of a cutting tool tip, suppress the occurrence of cracks and chips in the target body, and suppress the occurrence of irregularities on the target surface. Therefore, it is a useful technique for manufacturing a member having excellent soft magnetic properties, thermal stability, corrosion resistance, wear resistance and the like described above.
　本発明のターゲットは、ＪＩＳ　Ｚ　２２４４で規定されるビッカース硬さが２５０～１１００ＨＶの範囲である。
　本発明のターゲットは、５点の測定点で測定を行なったビッカース硬さの平均値を２５０～１１００ＨＶという特定範囲にすることで、ターゲットの形状寸法にするための切削加工や研磨加工といった機械加工を施す際に、ターゲット本体の割れや欠けの発生を抑制できることに加え、表面における凹凸の発生も抑制できる。このため、本発明のターゲットは、平滑な表面を有するターゲットとなり、異常放電の誘発や、ノジュールが飛散して被処理材に付着することを抑制できる。好ましくは、上記の５点の測定点で測定を行なったビッカース硬さの全てを２５０～１１００ＨＶという特定範囲にすることである。 The target of the present invention has a Vickers hardness in the range of 250 to 1100 HV as defined by JIS Z 2244.
The target of the present invention is a machining process such as cutting or polishing to make the target shape and dimension by setting the average value of Vickers hardness measured at five measurement points in a specific range of 250 to 1100 HV. In addition to being able to suppress the occurrence of cracks and chips in the target body, it is also possible to suppress the occurrence of irregularities on the surface. Therefore, the target of the present invention becomes a target having a smooth surface, and it is possible to suppress the induction of abnormal discharge and the scattering of nodules and adhesion to the material to be treated. Preferably, all of the Vickers hardness measured at the above five measurement points is set to a specific range of 250 to 1100 HV.
　また、本発明のターゲットは、ビッカース硬さを２５０ＨＶ以上にすることで、例えば、フライス盤や旋盤等のチップに構成刃先が生成されることを抑制できる。すなわち、本発明のターゲットは、切削加工を進めるにつれて、構成刃先の成長に伴うチップの切り込み量が次第に大きくなることが抑制され、切削開始時と切削完了時でターゲットの寸法差を小さくできることに加え、構成刃先の剥離に伴うチップの破損を抑制することもできる。 Further, in the target of the present invention, by setting the Vickers hardness to 250 HV or more, it is possible to suppress the generation of a built edge on a tip such as a milling machine or a lathe. That is, in addition to the fact that the target of the present invention is prevented from gradually increasing the depth of cut of the insert as the constituent cutting edge grows as the cutting process progresses, and the dimensional difference of the target can be reduced between the start of cutting and the completion of cutting. It is also possible to suppress damage to the tip due to peeling of the built-up edge.
　また、ターゲットのエロージョン領域に、例えば、Ｆｅ系合金マトリックス相の中に、低硬度の部位が存在してしまうと、低硬度の部位のみが残存したり、脱落したりする場合があり、ターゲットのエロージョン領域の表面が粗くなり、成膜時に異常放電の起点となりやすくなる。このため、本発明のターゲットは、ビッカース硬さを２５０ＨＶ以上にする。そして、上記と同様の理由から、本発明の実施形態に係るターゲットは、ビッカース硬さを５００ＨＶ以上にすることが好ましく、５５０ＨＶ以上にすることがより好ましい。 Further, if a low-hardness portion exists in the erosion region of the target, for example, in the Fe-based alloy matrix phase, only the low-hardness portion may remain or fall off, and the target The surface of the erosion region becomes rough, and it becomes easy to become a starting point of abnormal discharge during film formation. Therefore, the target of the present invention has a Vickers hardness of 250 HV or more. For the same reason as described above, the target according to the embodiment of the present invention preferably has a Vickers hardness of 500 HV or more, and more preferably 550 HV or more.
　本発明のターゲットは、ビッカース硬さを１１００ＨＶ以下にすることで、例えば、フライス盤や旋盤等のチップの摩耗量を抑えることができる。すなわち、本発明のターゲットは、切削加工を進めるにつれて、チップの磨耗に伴うチップの切り込み量が次第に小さくなり、切削開始時と切削完了時でターゲットの寸法差が大きくなることを抑制できることに加え、チップの破損を抑制することもできる。そして、上記と同様の理由から、本発明の実施形態に係るターゲットは、ビッカース硬さを１０００ＨＶ以下にすることが好ましく、９５０ＨＶ以下にすることがより好ましい。 The target of the present invention has a Vickers hardness of 1100 HV or less, so that the amount of wear of chips such as a milling machine and a lathe can be suppressed, for example. That is, in addition to being able to suppress that the cutting amount of the tip due to the wear of the tip gradually decreases as the cutting process progresses, and the dimensional difference of the target becomes large at the start of cutting and at the completion of cutting. It is also possible to suppress damage to the chip. For the same reason as described above, the target according to the embodiment of the present invention preferably has a Vickers hardness of 1000 HV or less, and more preferably 950 HV or less.
　本発明でいうビッカース硬さは、上述したターゲット本体の割れや欠けの発生を抑制することに加え、成膜時の異常放電の発生を抑制する観点から、ターゲットのエロージョン面における任意の５点の測定点で測定したビッカース硬さの平均値が２５０～１１００ＨＶの範囲にあることをいう。そして、ビッカース硬さの測定位置は、ターゲットのエロージョン面の平面方向において、外周部に相当する任意の４つの位置と、中央部に相当する位置の合計５か所とする。このとき、荷重は９．８Ｎとし、加圧時間は１０秒とする。
　また、本発明の実施形態に係るターゲットは、ビッカース硬さを２５０～１１００ＨＶにする観点から、金属組織中にＦｅ－Ｓｉ－Ｂ－Ｎｂ系の複合化合物相を有しないことが好ましい。 The Vickers hardness referred to in the present invention has any five points on the erosion surface of the target from the viewpoint of suppressing the occurrence of cracks and chips of the target body as described above and also suppressing the occurrence of abnormal discharge during film formation. It means that the average value of Vickers hardness measured at the measurement point is in the range of 250 to 1100 HV. Then, the Vickers hardness is measured at a total of five positions in the plane direction of the erosion surface of the target, which are arbitrary four positions corresponding to the outer peripheral portion and positions corresponding to the central portion. At this time, the load is 9.8 N and the pressurization time is 10 seconds.
Further, the target according to the embodiment of the present invention preferably does not have a Fe—Si—B—Nb-based composite compound phase in the metal structure from the viewpoint of setting the Vickers hardness to 250 to 1100 HV.
　本発明のターゲットは、原子比における組成式が（Ｆｅ１－ａ－ｂＣｏａＮｉｂ）１００－Ｘ－Ｙ－ＺＳｉＸＢＹＮｂＺ、ａ≦０．９５、ｂ≦０．３０、１５≦Ｘ＋Ｙ≦３５、０．３≦Ｘ／Ｙ≦２．０、１≦Ｚ≦２０で表わされ、残部が不可避的不純物からなる。Ｃｏ、Ｎｉ、Ｓｉ、Ｂ、Ｎｂの含有量は、軟磁気特性、熱安定性、耐食性、耐摩耗性を大きく損なわない範囲で適宜調整することができる。
　本発明のターゲットは、ＳｉとＢの合計量、すなわち組成式のＸ＋Ｙを１５以上にすることにより、低い保磁力を備える軟磁性膜を得ることができる。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、Ｘ＋Ｙを２０以上にすることが好ましい。
　また、本発明のターゲットは、Ｘ＋Ｙを３５以下にすることにより、高い飽和磁束密度を備える軟磁性膜を得ることができる。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、Ｘ＋Ｙを３３以下にすることが好ましい。 The target of the present invention has a composition formula in atomic ratio (Fe 1-ab Co a Ni b ) 100-XYZ Si X BY Nb Z , a ≤ 0.95, b ≤ 0.30, It is represented by 15 ≦ X + Y ≦ 35, 0.3 ≦ X / Y ≦ 2.0, and 1 ≦ Z ≦ 20, and the balance is composed of unavoidable impurities. The contents of Co, Ni, Si, B, and Nb can be appropriately adjusted within a range that does not significantly impair soft magnetic properties, thermal stability, corrosion resistance, and wear resistance.
In the target of the present invention, a soft magnetic film having a low coercive force can be obtained by setting the total amount of Si and B, that is, X + Y in the composition formula to 15 or more. The target according to the embodiment of the present invention preferably has X + Y of 20 or more for the same reason as described above.
Further, the target of the present invention can obtain a soft magnetic film having a high saturation magnetic flux density by setting X + Y to 35 or less. The target according to the embodiment of the present invention preferably has X + Y of 33 or less for the same reason as described above.
　本発明のターゲットは、ＳｉとＢの比率、すなわち組成式のＸ／Ｙを０．３以上２．０以下にすることにより、熱安定性を備える軟磁性膜を得ることができる。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、Ｘ／Ｙを０．７以上１．６以下にすることが好ましい。 The target of the present invention is to obtain a soft magnetic film having thermal stability by setting the ratio of Si and B, that is, X / Y of the composition formula to 0.3 or more and 2.0 or less. The target according to the embodiment of the present invention preferably has an X / Y of 0.7 or more and 1.6 or less for the same reason as described above.
　本発明のターゲットは、Ｎｂの含有量、すなわち組成式のＺを１以上にすることにより、耐食性を備える軟磁性膜を得ることができる。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、Ｚを３以上にすることが好ましい。
　また、本発明のターゲットは、Ｚを２０以下にすることにより、高い飽和磁束密度を備える軟磁性膜を得ることができる。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、Ｚを１０以下にすることが好ましい。
　尚、本発明のターゲットは、Ｎｂの一部または全てをＴａに置換することでも、上記と同様の効果を得ることができる。 In the target of the present invention, a soft magnetic film having corrosion resistance can be obtained by setting the Nb content, that is, Z in the composition formula to 1 or more. The target according to the embodiment of the present invention preferably has a Z of 3 or more for the same reason as described above.
Further, in the target of the present invention, a soft magnetic film having a high saturation magnetic flux density can be obtained by setting Z to 20 or less. The target according to the embodiment of the present invention preferably has a Z of 10 or less for the same reason as described above.
The target of the present invention can also obtain the same effect as described above by substituting a part or all of Nb with Ta.
　本発明のターゲットは、Ｆｅの一部を、ＣｏおよびＮｉから選択される一種以上の元素で置換することにより、磁歪を低減して高い透磁率を備える軟磁性膜を得ることができる。Ｆｅに対するＣｏの置換量、すなわち組成式のａは０．９５以下とする。また、Ｆｅに対するＮｉの置換量、すなわち組成式のｂは０．３０以下とする。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、aを０．５０以上にすることが好ましい。
　また、本発明の実施形態に係るターゲットは、ａを０．９０以下、ｂを０．１０以下にすることにより、高い飽和磁束密度を備える軟磁性膜を得ることができる点で好ましい。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、ａを０．６０以下、ｂを０．０５以下にすることがより好ましい。 The target of the present invention can obtain a soft magnetic film having a high magnetic permeability by reducing magnetostriction by substituting a part of Fe with one or more elements selected from Co and Ni. The amount of Co substituted with respect to Fe, that is, a in the composition formula is 0.95 or less. Further, the substitution amount of Ni with respect to Fe, that is, b in the composition formula is 0.30 or less. The target according to the embodiment of the present invention preferably has a of 0.50 or more for the same reason as described above.
Further, the target according to the embodiment of the present invention is preferable in that a soft magnetic film having a high saturation magnetic flux density can be obtained by setting a to 0.90 or less and b to 0.10 or less. For the target according to the embodiment of the present invention, it is more preferable that a is 0.60 or less and b is 0.05 or less for the same reason as described above.
　本発明のターゲットは、例えば、粉末焼結法で得ることができる。具体的には、上記した成分組成となるように、純金属粉末や合金粉末を混合した混合粉末を加圧焼結することにより得ることができる。合金粉末としては、組織にＦｅ－Ｓｉ－Ｂ－Ｎｂ系の複合化合物相を極力形成させないようにするために、Ｆｅ－Ｓｉ合金粉末、Ｆｅ－Ｂ合金粉末、Ｆｅ－Ｎｂ合金粉末、Ｆｅ－Ｓｉ－Ｂ合金粉末、Ｆｅ－Ｓｉ－Ｎｂ合金粉末、Ｆｅ－Ｂ－Ｎｂ合金粉末、Ｆｅ－Ｃｏ－Ｓｉ合金粉末、Ｆｅ－Ｃｏ－Ｂ合金粉末、Ｆｅ－Ｃｏ－Ｎｂ合金粉末、Ｆｅ－Ｃｏ－Ｓｉ－Ｂ合金粉末、Ｆｅ－Ｃｏ－Ｓｉ－Ｎｂ合金粉末、Ｆｅ－Ｃｏ－Ｂ－Ｎｂ合金粉末、Ｆｅ－Ｎｉ－Ｓｉ合金粉末、Ｆｅ－Ｎｉ－Ｂ合金粉末、Ｆｅ－Ｎｉ－Ｎｂ合金粉末、Ｆｅ－Ｎｉ－Ｓｉ－Ｂ合金粉末、Ｆｅ－Ｎｉ－Ｓｉ－Ｎｂ合金粉末、Ｆｅ－Ｎｉ－Ｂ－Ｎｂ合金粉末、Ｆｅ－Ｃｏ－Ｎｉ－Ｓｉ合金粉末、Ｆｅ－Ｃｏ－Ｎｉ－Ｂ合金粉末、Ｆｅ－Ｃｏ－Ｎｉ－Ｎｂ合金粉末、Ｆｅ－Ｃｏ－Ｎｉ－Ｓｉ－Ｂ合金粉末、Ｆｅ－Ｃｏ－Ｎｉ－Ｓｉ－Ｎｂ合金粉末、Ｆｅ－Ｃｏ－Ｎｉ－Ｂ－Ｎｂ合金粉末、Ｆｅ－Ｃｏ合金粉末、Ｆｅ－Ｎｉ合金粉末、Ｃｏ－Ｎｉ合金粉末、Ｆｅ－Ｃｏ－Ｎｉ合金粉末を用いることが好ましい。
　そして、加圧焼結としては、例えば、熱間静水圧プレス（ＨＩＰ）法、ホットプレス法、通電焼結法等を適用することができる。 The target of the present invention can be obtained by, for example, a powder sintering method. Specifically, it can be obtained by pressure sintering a mixed powder in which a pure metal powder or an alloy powder is mixed so as to have the above-mentioned component composition. As the alloy powder, Fe—Si alloy powder, Fe—B alloy powder, Fe—Nb alloy powder, Fe—Si in order to prevent the structure from forming a Fe—Si—B—Nb-based composite compound phase as much as possible. -B alloy powder, Fe-Si-Nb alloy powder, Fe-B-Nb alloy powder, Fe-Co-Si alloy powder, Fe-Co-B alloy powder, Fe-Co-Nb alloy powder, Fe-Co-Si -B alloy powder, Fe-Co-Si-Nb alloy powder, Fe-Co-B-Nb alloy powder, Fe-Ni-Si alloy powder, Fe-Ni-B alloy powder, Fe-Ni-Nb alloy powder, Fe -Ni—Si—B alloy powder, Fe—Ni—Si—Nb alloy powder, Fe—Ni—B—Nb alloy powder, Fe—Co—Ni—Si alloy powder, Fe—Co—Ni—B alloy powder, Fe -Co-Ni-Nb alloy powder, Fe-Co-Ni-Si-B alloy powder, Fe-Co-Ni-Si-Nb alloy powder, Fe-Co-Ni-B-Nb alloy powder, Fe-Co alloy powder , Fe—Ni alloy powder, Co—Ni alloy powder, Fe—Co—Ni alloy powder is preferably used.
As the pressure sintering, for example, a hot hydrostatic pressure press (HIP) method, a hot press method, an energization sintering method, or the like can be applied.
　加圧焼結は、焼結温度７００～１３００℃、加圧圧力３０～２００ＭＰａ、１～１０時間の条件で行なうことが好ましい。
　焼結温度は、７００℃以上にすることで、粉末の焼結を進行させることができ、空孔の発生を抑制することができる。また、焼結温度は、１３００℃以下にすることで、粉末の溶解を抑制できる。
　また、加圧圧力は、３０ＭＰａ以上にすることで、焼結の進行を促進し、空孔の発生を抑制することができる。また、加圧圧力は、２００ＭＰａ以下にすることで、焼結時にターゲットへの残留応力の導入が抑制され、焼結後の割れの発生を抑制することができる。
　また、焼結時間は、１時間以上にすることで、焼結の進行を促進し、空孔の発生を抑制することができる。また、焼結時間は、１０時間以下にすることで、製造効率の低下を抑制できる。 The pressure sintering is preferably performed under the conditions of a sintering temperature of 700 to 1300 ° C. and a pressure pressure of 30 to 200 MPa for 1 to 10 hours.
By setting the sintering temperature to 700 ° C. or higher, the sintering of the powder can proceed and the generation of pores can be suppressed. Further, by setting the sintering temperature to 1300 ° C. or lower, dissolution of the powder can be suppressed.
Further, by setting the pressurizing pressure to 30 MPa or more, the progress of sintering can be promoted and the generation of vacancies can be suppressed. Further, by setting the pressurizing pressure to 200 MPa or less, the introduction of residual stress to the target during sintering can be suppressed, and the occurrence of cracks after sintering can be suppressed.
Further, by setting the sintering time to 1 hour or more, the progress of sintering can be promoted and the generation of vacancies can be suppressed. Further, by setting the sintering time to 10 hours or less, a decrease in production efficiency can be suppressed.
　先ず、Ｆｅ粉末、Ｃｏ粉末、Ｓｉ粉末、Ｂ粉末およびＮｂ粉末を準備した。そして、本発明例１となるターゲットを得るために、原子比における組成式が（Ｆｅ０．９０Ｃｏ０．１０）６７Ｓｉ１３．５Ｂ１４．５Ｎｂ５、（ａ＝０．１０、ｂ＝０、Ｘ＋Ｙ＝２８、Ｘ／Ｙ＝０．９、Ｚ＝５）となるように、上記で準備した各粉末を秤量した後にＶ型混合機で混合して混合粉末を得た。そして、この混合粉末を軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、７５０℃、１２２ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。 First, Fe powder, Co powder, Si powder, B powder and Nb powder were prepared. Then, in order to obtain the target according to Example 1 of the present invention, the composition formula in atomic ratio is (Fe 0.90 Co 0.10 ) 67 Si 13.5 B 14.5 Nb 5 , (a = 0.10, b). Each powder prepared above was weighed so as to have = 0, X + Y = 28, X / Y = 0.9, Z = 5) and then mixed with a V-type mixer to obtain a mixed powder. Then, this mixed powder was filled in a capsule made of soft iron and degassed and sealed under the conditions of 450 ° C. for 4 hours. Then, the capsule was pressure-sintered by HIP under the conditions of 750 ° C., 122 MPa, and 1 hour to prepare a sintered body.
　本発明例２となるターゲットを得るために、Ｆｅ粉末、Ｃｏ粉末、Ｓｉ粉末、Ｂ粉末およびＮｂ粉末を準備し、原子比における組成式（Ｆｅ０．７０Ｃｏ０．３０）６７Ｓｉ１３．５Ｂ１４．５Ｎｂ５、（ａ＝０．３０、ｂ＝０、Ｘ＋Ｙ＝２８、Ｘ／Ｙ＝０．９、Ｚ＝５）となるように、上記で準備した各粉末を秤量した後に、Ｖ型混合機で混合して混合粉末を得た。そして、この混合粉末を軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、７５０℃、１２２ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。 In order to obtain the target according to Example 2 of the present invention, Fe powder, Co powder, Si powder, B powder and Nb powder were prepared, and the composition formula (Fe 0.70 Co 0.30 ) 67 Si 13.5 in atomic ratio was prepared. After weighing each powder prepared above so as to be B 14.5 Nb 5 , (a = 0.30, b = 0, X + Y = 28, X / Y = 0.9, Z = 5), Mixing was performed with a V-type mixer to obtain a mixed powder. Then, this mixed powder was filled in a capsule made of soft iron and degassed and sealed under the conditions of 450 ° C. for 4 hours. Then, the capsule was pressure-sintered by HIP under the conditions of 750 ° C., 122 MPa, and 1 hour to prepare a sintered body.
　本発明例３となるターゲットを得るために、Ｆｅ粉末、Ｃｏ粉末、Ｓｉ粉末、Ｂ粉末およびＮｂ粉末を準備し、原子比における組成式（Ｆｅ０．９５Ｃｏ０．０５）８４Ｓｉ３．５Ｂ１１．５Ｎｂ１、（ａ＝０．０５、ｂ＝０、Ｘ＋Ｙ＝１５、Ｘ／Ｙ＝０．３、Ｚ＝１）となるように、上記で準備した各粉末を秤量した後に、Ｖ型混合機で混合して混合粉末を得た。そして、この混合粉末を軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、９５０℃、１２２ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。 In order to obtain a target according to Example 3 of the present invention, Fe powder, Co powder, Si powder, B powder and Nb powder were prepared, and the composition formula (Fe 0.95 Co 0.05 ) 84 Si 3.5 in atomic ratio was prepared. After weighing each powder prepared above so as to be B 11.5 Nb 1 , (a = 0.05, b = 0, X + Y = 15, X / Y = 0.3, Z = 1), Mixing was performed with a V-type mixer to obtain a mixed powder. Then, this mixed powder was filled in a capsule made of soft iron and degassed and sealed under the conditions of 450 ° C. for 4 hours. Then, the capsule was pressure-sintered by HIP under the conditions of 950 ° C., 122 MPa, and 1 hour to prepare a sintered body.
　本発明例４となるターゲットを得るために、Ｆｅ粉末、Ｃｏ粉末、Ｓｉ粉末、Ｂ粉末およびＮｂ粉末を準備し、原子比における組成式（Ｆｅ０．０５Ｃｏ０．９５）４５Ｓｉ２３．３Ｂ１１．７Ｎｂ２０、（ａ＝０．９５、ｂ＝０、Ｘ＋Ｙ＝３５、Ｘ／Ｙ＝２．０、Ｚ＝２０）となるように、上記で準備した各粉末を秤量した後に、Ｖ型混合機で混合して混合粉末を得た。そして、この混合粉末を軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、９５０℃、１２２ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。 In order to obtain the target according to Example 4 of the present invention, Fe powder, Co powder, Si powder, B powder and Nb powder were prepared, and the composition formula in atomic ratio (Fe 0.05 Co 0.95 ) 45 Si 23.3 was prepared. After weighing each powder prepared above so that B 11.7 Nb 20 , (a = 0.95, b = 0, X + Y = 35, X / Y = 2.0, Z = 20) Mixing was performed with a V-type mixer to obtain a mixed powder. Then, this mixed powder was filled in a capsule made of soft iron and degassed and sealed under the conditions of 450 ° C. for 4 hours. Then, the capsule was pressure-sintered by HIP under the conditions of 950 ° C., 122 MPa, and 1 hour to prepare a sintered body.
　本発明例５となるターゲットを得るために、Ｆｅ粉末、Ｃｏ粉末、Ｎｉ粉末、Ｓｉ粉末、Ｂ粉末およびＮｂ粉末を準備し、原子比における組成式（Ｆｅ０．６０Ｃｏ０．１０Ｎｉ０．３０）６７Ｓｉ１３．５Ｂ１４．５Ｎｂ５、（ａ＝０．１、ｂ＝０．３、Ｘ＋Ｙ＝２８、Ｘ／Ｙ＝０．９、Ｚ＝５）となるように、上記で準備した各粉末を秤量した後に、Ｖ型混合機で混合して混合粉末を得た。そして、この混合粉末を軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、９５０℃、１２２ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。 In order to obtain the target according to Example 5 of the present invention, Fe powder, Co powder, Ni powder, Si powder, B powder and Nb powder were prepared, and the composition formula in atomic ratio (Fe 0.60 Co 0.10 Ni 0. 30 ) 67 Si 13.5 B 14.5 Nb 5 , (a = 0.1, b = 0.3, X + Y = 28, X / Y = 0.9, Z = 5). After weighing each of the prepared powders, they were mixed with a V-type mixer to obtain a mixed powder. Then, this mixed powder was filled in a capsule made of soft iron and degassed and sealed under the conditions of 450 ° C. for 4 hours. Then, the capsule was pressure-sintered by HIP under the conditions of 950 ° C., 122 MPa, and 1 hour to prepare a sintered body.
　比較例となるターゲットを得るために、原子比における組成式がＦｅ６７－Ｓｉ１３．５－Ｂ１４．５－Ｎｂ５（ａ＝０、ｂ＝０、Ｘ＋Ｙ＝２８、Ｘ／Ｙ＝０．９、Ｚ＝５）であるガスアトマイズ粉を準備し、軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、９５０℃、１２２ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。 In order to obtain a target as a comparative example, the composition formula in atomic ratio is Fe 67- Si 13.5- B 14.5- Nb 5 (a = 0, b = 0, X + Y = 28, X / Y = 0. A gas atomized powder of 9, Z = 5) was prepared, filled in a soft iron capsule, and degassed and sealed at 450 ° C. for 4 hours. Then, the capsule was pressure-sintered by HIP under the conditions of 950 ° C., 122 MPa, and 1 hour to prepare a sintered body.
　上記で得た各焼結体に機械加工を施してターゲットを作製した。このとき、本発明例１～本発明例５となるターゲットは、いずれも、機械加工の際に、割れが発生せず、また、仕上げ加工後の表面に凹凸が発生せず、表面が平滑な状態であることが確認できた。
　一方、比較例となるターゲットは、機械加工の際に、割れが発生し、ターゲット形状に機械加工することができなかった。 Each of the sintered bodies obtained above was machined to prepare a target. At this time, the targets according to the first to fifth aspects of the present invention do not crack during machining, and the surface after finishing is not uneven and the surface is smooth. It was confirmed that it was in a state.
On the other hand, the target as a comparative example could not be machined into the target shape due to cracks during machining.
　上記で得た各焼結体について、ターゲットのエロージョン面となる面の平面方向において、外周部に相当する４つの位置と、中央部に相当する位置の合計５か所のビッカース硬さを測定した。尚、測定間隔は、圧痕どうしで測定の影響を受けない距離を設けて測定した。そして、ビッカース硬さは、ＪＩＳ　Ｚ　２２４４に準じ、株式会社明石製作所製のＭＶＫ－Ｅを用いて、荷重を９．８Ｎとし、加圧時間を１０秒としたときの値を測定した。その結果を表１に示す。 For each of the sintered bodies obtained above, the Vickers hardness was measured at four positions corresponding to the outer peripheral portion and a total of five positions corresponding to the central portion in the plane direction of the surface to be the erosion surface of the target. .. The measurement interval was set so that the indentations were not affected by the measurement. Then, the Vickers hardness was measured according to JIS Z 2244 using MVK-E manufactured by Akashi Seisakusho Co., Ltd. when the load was 9.8 N and the pressurization time was 10 seconds. The results are shown in Table 1.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
　比較例となるターゲットは、ビッカース硬度の平均値が１１００ＨＶを超えていた。
　これに対して、本発明例１～本発明例５のターゲットは、いずれも、ビッカース硬度の平均値が２５０～１１００ＨＶの範囲にあることが確認できた。
　これにより、本発明のターゲットは、機械加工の際に、割れや欠けの発生が抑制され、また、仕上げ加工後の表面に凹凸が発生せず、表面が平滑なターゲットであることが確認できた。これにより、本発明のターゲットは、異常放電の誘発や、ノジュールが飛散して被処理材に付着することが抑制された、軟磁性膜を形成するためのターゲットとして有用となることが期待できる。

  In the target as a comparative example, the average value of Vickers hardness exceeded 1100 HV.
On the other hand, it was confirmed that the average value of the Vickers hardness of all the targets of the first to fifth inventions was in the range of 250 to 1100 HV.
As a result, it was confirmed that the target of the present invention is a target in which cracks and chips are suppressed during machining, the surface after finishing is not uneven, and the surface is smooth. .. As a result, the target of the present invention can be expected to be useful as a target for forming a soft magnetic film in which the induction of abnormal discharge and the scattering of nodules and adhesion to the material to be treated are suppressed.

Claims (2)

  1. 　原子比における組成式が（Ｆｅ１－ａ－ｂＣｏａＮｉｂ）１００－Ｘ－Ｙ－ＺＳｉＸＢＹＮｂＺ、ａ≦０．９５、ｂ≦０．３０、１５≦Ｘ＋Ｙ≦３５、０．３≦Ｘ／Ｙ≦２．０、１≦Ｚ≦２０で表わされ、残部が不可避的不純物からなり、５点の測定点で測定を行なったビッカース硬さの平均値が２５０～１１００ＨＶであるＦｅ－Ｃｏ－Ｓｉ－Ｂ－Ｎｂ系ターゲット。 The composition formula in atomic ratio is (Fe 1-ab Co a Ni b ) 100-XYZ Si X BY Nb Z , a≤0.95, b≤0.30, 15≤X + Y≤35, Represented by 0.3 ≤ X / Y ≤ 2.0, 1 ≤ Z ≤ 20, the balance is composed of unavoidable impurities, and the average value of Vickers hardness measured at 5 measurement points is 250 to 1100 HV. Fe-Co-Si-B-Nb system target.
  2. 　前記５点の測定点で測定を行なったビッカース硬さの平均値が５００～１０００ＨＶである請求項１に記載のＦｅ－Ｃｏ－Ｓｉ－Ｂ－Ｎｂ系ターゲット。 The Fe-Co-Si-B-Nb system target according to claim 1, wherein the average value of Vickers hardness measured at the above five measurement points is 500 to 1000 HV.
PCT/JP2020/031823 2019-08-26 2020-08-24 Fe-co-si-b-nb-based target WO2021039711A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2021542883A JPWO2021039711A1 (en) 2019-08-26 2020-08-24

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2019153616 2019-08-26
JP2019-153616 2019-08-26

Publications (1)

Publication Number Publication Date
WO2021039711A1 true WO2021039711A1 (en) 2021-03-04

Family

ID=74684176

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2020/031823 WO2021039711A1 (en) 2019-08-26 2020-08-24 Fe-co-si-b-nb-based target

Country Status (3)

Country Link
JP (1) JPWO2021039711A1 (en)
TW (1) TWI739563B (en)
WO (1) WO2021039711A1 (en)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02163911A (en) * 1988-12-16 1990-06-25 Matsushita Electric Ind Co Ltd Soft magnetic alloy film and manufacture thereof
JPH02263409A (en) * 1988-12-15 1990-10-26 Matsushita Electric Ind Co Ltd Mild magnetic alloy film and manufacture thereof
JPH11328619A (en) * 1998-05-11 1999-11-30 Alps Electric Co Ltd Thin film magnetic head with magnetic impedance effect element
JP2010285659A (en) * 2009-06-12 2010-12-24 Sanyo Special Steel Co Ltd Sputtering target material for producing soft magnetic film having high sputtering yield
JP2011026702A (en) * 2009-07-01 2011-02-10 Hitachi Metals Ltd SPUTTERING TARGET MATERIAL OF Fe-Co-Ni-BASED ALLOY
JP2013084322A (en) * 2011-10-07 2013-05-09 Hitachi Metals Ltd Soft magnetic film for thermally assisted magnetic recording medium and manufacturing method therefor
JP2018188726A (en) * 2017-04-28 2018-11-29 日立金属株式会社 Sputtering target and production method thereof
JP2020027677A (en) * 2018-08-09 2020-02-20 日立金属株式会社 Soft magnetic film of heat-assisted magnetic recording medium and sputtering target for forming soft magnetic film of heat-assisted magnetic recording medium

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5270926B2 (en) * 2008-02-20 2013-08-21 三菱製鋼株式会社 Iron-based sintered alloy powder
JP5698023B2 (en) * 2011-02-16 2015-04-08 山陽特殊製鋼株式会社 Soft magnetic alloy for magnetic recording, sputtering target material, and magnetic recording medium

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02263409A (en) * 1988-12-15 1990-10-26 Matsushita Electric Ind Co Ltd Mild magnetic alloy film and manufacture thereof
JPH02163911A (en) * 1988-12-16 1990-06-25 Matsushita Electric Ind Co Ltd Soft magnetic alloy film and manufacture thereof
JPH11328619A (en) * 1998-05-11 1999-11-30 Alps Electric Co Ltd Thin film magnetic head with magnetic impedance effect element
JP2010285659A (en) * 2009-06-12 2010-12-24 Sanyo Special Steel Co Ltd Sputtering target material for producing soft magnetic film having high sputtering yield
JP2011026702A (en) * 2009-07-01 2011-02-10 Hitachi Metals Ltd SPUTTERING TARGET MATERIAL OF Fe-Co-Ni-BASED ALLOY
JP2013084322A (en) * 2011-10-07 2013-05-09 Hitachi Metals Ltd Soft magnetic film for thermally assisted magnetic recording medium and manufacturing method therefor
JP2018188726A (en) * 2017-04-28 2018-11-29 日立金属株式会社 Sputtering target and production method thereof
JP2020027677A (en) * 2018-08-09 2020-02-20 日立金属株式会社 Soft magnetic film of heat-assisted magnetic recording medium and sputtering target for forming soft magnetic film of heat-assisted magnetic recording medium

Also Published As

Publication number Publication date
TWI739563B (en) 2021-09-11
JPWO2021039711A1 (en) 2021-03-04
TW202108781A (en) 2021-03-01

Similar Documents

Publication Publication Date Title
EP2462083B1 (en) Tough coated hard particles consolidated in a tough matrix material
TWI525206B (en) Ytterbium sputtering target and manufacturing method of the target
WO2009116610A1 (en) Sintered cubic boron nitride tool
KR20150132582A (en) Surface-coated boron nitride sintered tool
CN110042294B (en) Hard alloy blade for milling quenched steel and preparation method thereof
TW201839150A (en) Sputtering target and method for manufacturing same
WO2021039711A1 (en) Fe-co-si-b-nb-based target
WO2021039710A1 (en) Fe-si-b-nb-based target
JP6814758B2 (en) Sputtering target
WO2021039712A1 (en) Fe-si-b-nb-based target
JP2016188394A (en) Mo alloy target
KR20150133813A (en) Surface-coated boron nitride sintered tool
JP7293787B2 (en) TaWSi target and manufacturing method thereof
EP3951003B1 (en) V alloy target
EP3951002B1 (en) V alloy target
JP5787274B2 (en) Method for producing Fe-Co-Ta-based sputtering target material and Fe-Co-Ta-based sputtering target material
JP5266587B2 (en) CBN sintered body for cutting tools containing coarse cBN particles
JPS63286549A (en) Nitrogen-containing titanium carbide-base sintered alloy having excellent resistance to plastic deformation
JPH05230589A (en) Wc-based cemented carbide
JPH036218B2 (en)
WO2022208766A1 (en) Superhard alloy and mold
JP6156734B2 (en) Fe-Co alloy sputtering target material and method for producing the same
JP5239061B2 (en) Coated cBN sintered body tool that suppresses damage at the lateral boundary of the cutting edge
KR20230133222A (en) Chromium sintered body, method of manufacturing the same, sputtering target, and method of manufacturing substrate with chromium film
JPS6372843A (en) Manufacture of sintered compact containing high density phase boron nitride for cutting tool

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 20857215

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2021542883

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 20857215

Country of ref document: EP

Kind code of ref document: A1