TWI739563B - Fe-Co-Si-B-Nb series target - Google Patents
Fe-Co-Si-B-Nb series target Download PDFInfo
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- TWI739563B TWI739563B TW109128800A TW109128800A TWI739563B TW I739563 B TWI739563 B TW I739563B TW 109128800 A TW109128800 A TW 109128800A TW 109128800 A TW109128800 A TW 109128800A TW I739563 B TWI739563 B TW I739563B
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- 239000013077 target material Substances 0.000 claims abstract description 50
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 238000005259 measurement Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 abstract description 12
- 238000003754 machining Methods 0.000 abstract description 8
- 238000005299 abrasion Methods 0.000 abstract description 4
- 239000000843 powder Substances 0.000 description 62
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 31
- 229910045601 alloy Inorganic materials 0.000 description 21
- 239000000956 alloy Substances 0.000 description 21
- 235000019589 hardness Nutrition 0.000 description 19
- 238000005245 sintering Methods 0.000 description 14
- 239000002775 capsule Substances 0.000 description 12
- 239000011812 mixed powder Substances 0.000 description 10
- 238000001513 hot isostatic pressing Methods 0.000 description 7
- 229910001257 Nb alloy Inorganic materials 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 229910052796 boron Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000011863 silicon-based powder Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910008423 Si—B Inorganic materials 0.000 description 4
- 229910006291 Si—Nb Inorganic materials 0.000 description 4
- 230000002159 abnormal effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 229910000521 B alloy Inorganic materials 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910020630 Co Ni Inorganic materials 0.000 description 2
- 229910002440 Co–Ni Inorganic materials 0.000 description 2
- 229910003192 Nb–Ta Inorganic materials 0.000 description 2
- 229910018559 Ni—Nb Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 229910021484 silicon-nickel alloy Inorganic materials 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910020674 Co—B Inorganic materials 0.000 description 1
- 229910020711 Co—Si Inorganic materials 0.000 description 1
- 229910017061 Fe Co Inorganic materials 0.000 description 1
- 229910017082 Fe-Si Inorganic materials 0.000 description 1
- 229910017133 Fe—Si Inorganic materials 0.000 description 1
- 229910020018 Nb Zr Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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- 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
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- 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
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- 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
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- 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
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- 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
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- 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
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- 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
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- 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
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Abstract
本發明提供一種Fe-Co-Si-B-Nb系靶材，在靶材的機械加工中，能夠抑制切削工具的刀片的磨耗或破損，抑制靶材主體的裂紋或缺口的產生，還能夠抑制靶材表面的凹凸的產生。本發明的Fe-Co-Si-B-Nb系靶材中，原子比的組成式由(Fe1-a-b Coa Nib )100-X-Y-Z SiX BY NbZ 、a≦0.95、b≦0.30、15≦X+Y≦35、0.3≦X/Y≦2.0、1≦Z≦20表示，剩餘部分包含不可避免的雜質，且在5個測定點進行測定的維氏硬度的平均值為250 HV～1100 HV，且所述維氏硬度較佳為處於500 HV～1000 HV的範圍。The present invention provides a Fe-Co-Si-B-Nb-based target material. In the machining of the target material, it is possible to suppress abrasion or breakage of the blade of a cutting tool, suppress the generation of cracks or notches in the main body of the target material, and also suppress The occurrence of unevenness on the surface of the target. In the Fe-Co-Si-B-Nb target material of the present invention, the composition formula of the atomic ratio is (Fe 1-ab Co a Ni b ) 100-XYZ Si X B Y Nb Z , a≦0.95, b≦0.30 , 15≦X+Y≦35, 0.3≦X/Y≦2.0, 1≦Z≦20 means that the remainder contains unavoidable impurities, and the average value of the Vickers hardness measured at 5 measuring points is 250 HV ~1100 HV, and the Vickers hardness is preferably in the range of 500 HV to 1000 HV.
Description
本發明是有關於一種例如用於形成軟磁性膜的Fe-Co-Si-B-Nb系靶材。The present invention relates to an Fe-Co-Si-B-Nb-based target material for forming a soft magnetic film, for example.
以電子設備為首的各種產品的小型化、輕量化正在發展，功能性薄膜正在被適用。例如，在專利文獻1中，作為適合於磁頭等的芯材料的軟磁性膜，提出了以Fe為主要成分且包含選自由Nb、Nb-Ta及Ta所組成的群組中的金屬元素、選自由B（硼）及B-Si所組成的群組中的半金屬元素、以及N（氮）的軟磁性膜。所述由Fe-Si-B-Nb-N構成的軟磁性膜與以往的包含Co-Nb-Zr系合金的軟磁性膜相比，具有低矯頑力、低磁致伸縮及高飽和磁通密度等優異的軟磁性特性與良好的熱穩定性，並且在耐腐蝕性及耐磨耗性方面亦優異，因此是有用的技術。The miniaturization and weight reduction of various products such as electronic devices are progressing, and functional films are being applied. For example, in Patent Document 1, as a soft magnetic film suitable for a core material of a magnetic head, etc., it is proposed that Fe is the main component and contains metal elements selected from the group consisting of Nb, Nb-Ta, and Ta. A soft magnetic film of semi-metallic elements in the group consisting of B (boron) and B-Si, and N (nitrogen). The soft magnetic film composed of Fe-Si-B-Nb-N has low coercivity, low magnetostriction and high saturation magnetic flux compared with conventional soft magnetic films containing Co-Nb-Zr alloys It has excellent soft magnetic properties such as density, good thermal stability, and is also excellent in corrosion resistance and wear resistance, so it is a useful technology.
而且，所述由Fe-Si-B-Nb-N系構成的軟磁性膜例如可藉由濺射法形成。具體而言，提出了如下的方法：使用以Fe為主要成分且包含選自由Nb、Nb-Ta及Ta所組成的群組中的金屬元素、選自由B及B-Si所組成的群組中的半金屬元素的Fe-Si-B-Nb系合金作為靶材，在Ar等惰性濺射氣體中週期性地混合氮氣，藉此形成在膜厚方向上產生了組成調變的膜，其後進行熱處理。 [現有技術文獻] [專利文獻]Furthermore, the soft magnetic film composed of the Fe-Si-B-Nb-N system can be formed by, for example, a sputtering method. Specifically, the following method is proposed: using Fe as the main component and containing a metal element selected from the group consisting of Nb, Nb-Ta, and Ta, selected from the group consisting of B and B-Si The Fe-Si-B-Nb-based alloy of semi-metallic elements is used as a target, and nitrogen is periodically mixed in an inert sputtering gas such as Ar to form a film with compositional modulation in the film thickness direction. Carry out heat treatment. [Prior Art Literature] [Patent Literature]
[專利文獻1]日本專利特開平2-163911號公報[Patent Document 1] Japanese Patent Laid-Open No. 2-163911
[發明所欲解決之課題] 專利文獻1中揭示的Fe-Si-B-Nb系合金靶材是在加工成靶材的形狀尺寸的機械加工時，靶材主體的裂紋、缺口、脫落產生的可能性高的所謂難切削材。因此，在機械加工時，有時會導致切削工具的刀片的磨耗或破損，在獲得的靶材的表面誘發凹凸，或視情況使靶材主體破損。[The problem to be solved by the invention] The Fe-Si-B-Nb-based alloy target disclosed in Patent Document 1 is a so-called difficult-to-cut material that is highly likely to cause cracks, nicks, and detachment of the target body during machining into the shape and size of the target. . Therefore, during machining, the blade of the cutting tool may be worn or damaged, irregularities are induced on the surface of the obtained target material, or the target body may be damaged as the case may be.
本發明的目的在於提供一種Fe-Co-Si-B-Nb系靶材，在Fe-Si-B-Nb系靶材（以下亦簡稱為「靶材」）的機械加工中，能夠抑制切削工具的刀片的磨耗或破損，抑制靶材主體的裂紋或缺口的產生，還能夠抑制靶材表面的凹凸的產生。 [解決課題之手段]The object of the present invention is to provide a Fe-Co-Si-B-Nb-based target material that can suppress cutting tools in the machining of Fe-Si-B-Nb-based target materials (hereinafter also referred to as "target materials") The abrasion or breakage of the blade can suppress the generation of cracks or notches in the target body, and it can also suppress the generation of unevenness on the surface of the target. [Means to solve the problem]
關於本發明的靶材，原子比的組成式由(Fe1-a-b Coa Nib )100-X-Y-Z SiX BY NbZ 、a≦0.95、b≦0.30、15≦X+Y≦35、0.3≦X/Y≦2.0、1≦Z≦20表示，剩餘部分包含不可避免的雜質，且在5個測定點進行測定的維氏硬度（Vickers hardness）的平均值為250 HV～1100 HV。Regarding the target material of the present invention, the composition formula of the atomic ratio is (Fe 1-ab Co a Ni b ) 100-XYZ Si X B Y Nb Z , a≦0.95, b≦0.30, 15≦X+Y≦35, 0.3 ≦X/Y≦2.0 and 1≦Z≦20 indicate that the remainder contains unavoidable impurities, and the average value of Vickers hardness measured at 5 measurement points is 250 HV to 1100 HV.
本發明的靶材的所述在5個測定點進行測定的維氏硬度的平均值較佳為500 HV～1000 HV。 [發明的效果]The average value of the Vickers hardness measured at the five measurement points of the target material of the present invention is preferably 500 HV to 1000 HV. [Effects of the invention]
本發明在靶材的機械加工中，能夠抑制切削工具的刀片的磨耗或破損，抑制靶材主體的裂紋或缺口的產生，還能夠抑制靶材表面的凹凸的產生。因此，成為對製造上述軟磁特性、熱穩定性、耐腐蝕性、耐磨耗性等優異的零件有用的技術。In the machining of the target material, the present invention can suppress the abrasion or breakage of the blade of the cutting tool, suppress the generation of cracks or notches in the target body, and can also suppress the occurrence of unevenness on the surface of the target material. Therefore, it becomes a useful technology for manufacturing parts with excellent soft magnetic properties, thermal stability, corrosion resistance, and abrasion resistance.
本發明的靶材的由日本工業標準（Japanese industrial standard，JIS） Z 2244規定的維氏硬度在250 HV～1100 HV的範圍。 本發明的靶材藉由使在5個測定點進行測定的維氏硬度的平均值為250 HV～1100 HV的特定範圍，在實施用於形成靶材的形狀尺寸的切削加工或研磨加工等機械加工時，除了能夠抑制靶材主體的裂紋或缺口的產生之外，還能夠抑制表面的凹凸的產生。因此，本發明的靶材成為具有平滑的表面的靶材，能夠抑制異常放電的誘發或結核（nodule）飛散而附著在被處理材上。較佳為將上述的在5個測定點進行測定的維氏硬度全部設為250 HV～1100 HV的特定範圍。The target material of the present invention has a Vickers hardness specified by Japanese industrial standard (JIS) Z 2244 in the range of 250 HV to 1100 HV. The target material of the present invention is used in machinery such as cutting or polishing to form the shape and size of the target material by setting the average value of the Vickers hardness measured at 5 measuring points within a specific range of 250 HV to 1100 HV. During processing, in addition to suppressing the occurrence of cracks or notches in the target body, it is also possible to suppress the occurrence of irregularities on the surface. Therefore, the target material of the present invention becomes a target material having a smooth surface, and it is possible to suppress the induction of abnormal discharge or the scattering of nodules and adhesion to the material to be processed. It is preferable to set all the Vickers hardnesses measured at the five measurement points described above to a specific range of 250 HV to 1100 HV.
另外，本發明的靶材藉由將維氏硬度設為250 HV以上，例如能夠抑制在銑床、車床等的刀片上生成積屑瘤（built-up edge）。即，本發明的靶材能夠抑制隨著切削加工的進行，伴隨著積屑瘤的成長的刀片的切入量逐漸變大，在切削開始時和切削結束時能夠減小靶材的尺寸差，並且還能夠抑制隨著積屑瘤的剝離的刀片的破損。In addition, by setting the Vickers hardness to 250 HV or higher for the target of the present invention, for example, it is possible to suppress the generation of built-up edges on the blades of milling machines, lathes, and the like. That is, the target material of the present invention can prevent the cutting amount of the insert that is accompanied by the growth of the built-up edge from gradually increasing as the cutting process progresses, and can reduce the size difference between the target material at the beginning and the end of the cutting, and It is also possible to suppress the breakage of the blade due to the peeling of the built-up edge.
另外，如果在靶材的侵蝕區域，例如在Fe系合金基質相中存在低硬度的部位，則存在僅低硬度的部位殘存或脫落的情況，靶材的侵蝕區域的表面變粗糙，成膜時容易成為異常放電的起點。因此，本發明的靶材將維氏硬度設為250 HV以上。而且，自與上述同樣的理由出發，本發明的實施方式的靶材較佳為維氏硬度為500 HV以上，更佳為550 HV以上。In addition, if there are low-hardness sites in the eroded area of the target, for example, in the Fe-based alloy matrix phase, only the low-hardness sites may remain or fall off, and the surface of the eroded area of the target may become rough and the film will be formed. It is easy to become the starting point of abnormal discharge. Therefore, the target material of the present invention has a Vickers hardness of 250 HV or more. Furthermore, for the same reason as described above, the target material of the embodiment of the present invention preferably has a Vickers hardness of 500 HV or more, and more preferably 550 HV or more.
本發明的靶材藉由使維氏硬度為1100 HV以下，能夠抑制例如銑床或車床等的刀片的磨耗量。即，本發明的靶材隨著進行切削加工，伴隨著刀片的磨耗的刀片的切入量逐漸變小，除了能夠抑制在切削開始時和切削結束時靶材的尺寸差變大的情況之外，還能夠抑制刀片的破損。而且，自與上述同樣的理由出發，本發明的實施方式的靶材較佳為維氏硬度為1000 HV以下，更佳為950 HV以下。In the target material of the present invention, by setting the Vickers hardness to 1100 HV or less, it is possible to suppress the amount of wear of the blade of a milling machine or a lathe, for example. That is, with the target material of the present invention, the cutting amount of the insert accompanying the wear of the insert gradually decreases as the cutting process is performed, and it is possible to suppress the increase in the size difference between the target material at the start of cutting and the end of the cutting. It is also possible to suppress breakage of the blade. Furthermore, for the same reason as described above, the target material of the embodiment of the present invention preferably has a Vickers hardness of 1000 HV or less, and more preferably 950 HV or less.
本發明中所說的維氏硬度是指，除了抑制上述靶材主體的裂紋或缺口的產生之外，自抑制成膜時的異常放電的產生的觀點出發，在靶材的侵蝕面的任意5個測定點測定的維氏硬度的平均值處於250 HV～1100 HV的範圍內。而且，維氏硬度的測定位置設為在靶材的侵蝕面的平面方向上，相當於外周部的任意4個位置和相當於中央部的位置的合計5處。此時，負荷為9.8 N，加壓時間為10秒。 另外，本發明的實施方式的靶材自維氏硬度為250 HV～1100 HV的觀點出發，較佳為在金屬組織中不具有Fe-Si-B-Nb系的複合化合物相。The Vickers hardness mentioned in the present invention means that in addition to suppressing the generation of cracks or notches in the target body, from the viewpoint of suppressing the generation of abnormal discharges during film formation, it is possible to prevent the target's erosion surface at any 5 The average value of the Vickers hardness measured at each measurement point is in the range of 250 HV to 1100 HV. In addition, the measurement positions of the Vickers hardness were set to a total of five positions corresponding to any four positions of the outer peripheral portion and positions corresponding to the central portion in the plane direction of the erosion surface of the target material. At this time, the load was 9.8 N, and the pressure time was 10 seconds. In addition, the target material of the embodiment of the present invention preferably has no Fe-Si-B-Nb-based composite compound phase in the metal structure from the viewpoint that the Vickers hardness is 250 HV to 1100 HV.
關於本發明的靶材，原子比的組成式由(Fe1-a-b Coa Nib )100-X-Y-Z SiX BY NbZ ，a≦0.95，b≦0.30，15≦X+Y≦35，0.3≦X/Y≦2.0，1≦Z≦20表示，剩餘部分包含不可避免的雜質。Co、Ni、Si、B、Nb的含量可在不大幅損害軟磁特性、熱穩定性、耐腐蝕性、耐磨耗性的範圍內適當調整。 本發明的靶材藉由使Si與B的合計量、即組成式的X+Y為15以上，可獲得具有低矯頑力的軟磁性膜。而且，自與上述同樣的理由出發，本發明的實施方式的靶材較佳為將X+Y設為20以上。 另外，本發明的靶材藉由使X+Y為35以下，可獲得具有高飽和磁通密度的軟磁性膜。而且，自與上述同樣的理由出發，本發明的實施方式的靶材較佳為使X+Y為33以下。Regarding the target material of the present invention, the composition formula of the atomic ratio is (Fe 1-ab Co a Ni b ) 100-XYZ Si X B Y Nb Z , a≦0.95, b≦0.30, 15≦X+Y≦35, 0.3 ≦X/Y≦2.0, 1≦Z≦20 means that the remainder contains unavoidable impurities. The content 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. The target of the present invention can obtain a soft magnetic film with low coercivity by setting the total amount of Si and B, that is, X+Y of the composition formula to 15 or more. Furthermore, for the same reason as described above, it is preferable that X+Y is set to 20 or more in the target material of the embodiment of the present invention. In addition, the target of the present invention can obtain a soft magnetic film having a high saturation magnetic flux density by setting X+Y to be 35 or less. Furthermore, for the same reason as described above, it is preferable that the target material of the embodiment of the present invention has X+Y of 33 or less.
本發明的靶材藉由使Si與B的比率、即組成式的X/Y為0.3以上2.0以下，可獲得具有熱穩定性的軟磁性膜。而且，自與上述同樣的理由出發，本發明的實施方式的靶材較佳為將X/Y設為0.7以上1.6以下。The target of the present invention can obtain a thermally stable soft magnetic film by setting the ratio of Si to B, that is, X/Y of the composition formula to be 0.3 or more and 2.0 or less. Furthermore, for the same reason as described above, the target material of the embodiment of the present invention preferably has X/Y of 0.7 or more and 1.6 or less.
本發明的靶材藉由使Nb的含量、即組成式的Z為1以上，可獲得具有耐腐蝕性的軟磁性膜。而且，自與上述同樣的理由出發，本發明的實施方式的靶材較佳為將Z設為3以上。 另外，本發明的靶材藉由使Z設為20以下，可獲得具有高飽和磁通密度的軟磁性膜。而且，自與上述同樣的理由出發，本發明的實施方式的靶材較佳為將Z設為10以下。 再者，本發明的靶材藉由將Nb的一部分或全部取代為Ta，亦能夠獲得與所述同樣的效果。The target of the present invention can obtain a soft magnetic film having corrosion resistance by setting the Nb content, that is, Z of the composition formula to 1 or more. Furthermore, for the same reason as described above, it is preferable that the target material of the embodiment of the present invention has Z be 3 or more. In addition, in the target material of the present invention, by setting Z to 20 or less, a soft magnetic film having a high saturation magnetic flux density can be obtained. In addition, for the same reason as described above, it is preferable that the target material of the embodiment of the present invention set Z to 10 or less. Furthermore, the target of the present invention can also obtain the same effect as described above by substituting part or all of Nb with Ta.
本發明的靶材藉由用選自Co及Ni中的一種以上的元素取代Fe的一部分，能夠降低磁致伸縮，獲得具有高導磁率的軟磁性膜。Co對於Fe的取代量、即組成式的a為0.95以下。另外，Ni對於Fe的取代量、即組成式的b為0.30以下。而且，自與上述同樣的理由出發，本發明的實施方式的靶材較佳為a為0.50以上。 另外，本發明的實施方式的靶材藉由使a為0.90以下，b為0.10以下，能夠獲得具有高飽和磁通密度的軟磁性膜，因此較佳。而且，自與上述同樣的理由出發，本發明的實施方式的靶材更佳為a為0.60以下，b為0.05以下。The target of the present invention can reduce magnetostriction by substituting one or more elements selected from Co and Ni for a part of Fe, thereby obtaining a soft magnetic film with high magnetic permeability. The substitution amount of Co with respect to Fe, that is, a of the composition formula is 0.95 or less. In addition, the substitution amount of Ni with respect to Fe, that is, b in the composition formula is 0.30 or less. Furthermore, for the same reason as described above, the target material of the embodiment of the present invention preferably has a of 0.50 or more. In addition, in the target material of the embodiment of the present invention, since a is 0.90 or less and b is 0.10 or less, it is possible to obtain a soft magnetic film having a high saturation magnetic flux density, which is preferable. Furthermore, for the same reason as described above, it is more preferable that a is 0.60 or less in the target material of the embodiment of the present invention, and b is 0.05 or less.
本發明的靶材例如可藉由粉末燒結法獲得。具體而言，可藉由對以成為上述成分組成的方式混合純金屬粉末或合金粉末而得的混合粉末進行加壓燒結而獲得。作為合金粉末，為了儘量不在組織中形成Fe-Si-B-Nb系的複合化合物相，較佳使用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。 而且，作為加壓燒結，例如可應用熱等靜壓加壓（hot isostatic pressing，HIP）法、熱壓法、通電燒結法等。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 obtained by mixing pure metal powder or alloy powder so as to have the above-mentioned component composition. As alloy powder, in order not to form a Fe-Si-B-Nb composite compound phase in the structure as much as possible, it is preferable to use Fe-Si alloy powder, Fe-B alloy powder, Fe-Nb alloy powder, Fe-Si-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. Furthermore, as pressure sintering, for example, a hot isostatic pressing (HIP) method, a hot pressing method, an electric sintering method, etc. can be applied.
加壓燒結較佳為在燒結溫度700℃～1300℃、加壓壓力30 MPa～200 MPa、1小時～10小時的條件下進行。 藉由使燒結溫度為700℃以上，能夠進行粉末的燒結，能夠抑制空孔的產生。另外，藉由將燒結溫度設為1300℃以下，可抑制粉末的熔解。 另外，藉由使加壓壓力為30 MPa以上，能夠促進燒結的進行，抑制空孔的產生。並且，藉由使加壓壓力為200 MPa以下，能夠抑制燒結時殘留應力導入靶材，從而抑制燒結後的裂紋的產生。 另外，藉由使燒結時間為1小時以上，能夠促進燒結的進行，抑制空孔的產生。另外，藉由使燒結時間為10小時以下，可抑制製造效率的降低。 [實施例]Pressure sintering is preferably performed under the conditions of a sintering temperature of 700°C to 1300°C, a pressure of 30 MPa to 200 MPa, and 1 hour to 10 hours. By setting the sintering temperature to 700°C or higher, the powder can be sintered and the generation of voids can be suppressed. In addition, by setting the sintering temperature to 1300° C. or lower, the melting of the powder can be suppressed. In addition, by setting the pressing pressure to 30 MPa or more, the progress of sintering can be promoted and the generation of voids can be suppressed. In addition, by setting the pressing pressure to 200 MPa or less, the introduction of residual stress into the target during sintering can be suppressed, and the generation of cracks after sintering can be suppressed. In addition, by setting the sintering time to 1 hour or more, the progress of sintering can be promoted and the generation of voids can be suppressed. In addition, by setting the sintering time to 10 hours or less, it is possible to suppress a decrease in manufacturing efficiency. [Example]
首先，準備Fe粉末、Co粉末、Si粉末、B粉末及Nb粉末。而且，為了獲得作為本發明例1的靶材，以原子比的組成式為(Fe0.90 Co0.10 )67 Si13.5 B14.5 Nb5 、（a=0.10、b=0、X+Y=28、X/Y=0.9、Z=5）的方式，稱重上述所準備的各粉末後，在V型混合機中混合，獲得混合粉末。然後，將該混合粉末填充到軟鐵製的膠囊中，在450℃、4小時的條件下進行脫氣密封。然後，在750℃、122 MPa、1小時的條件下，藉由HIP對所述膠囊進行加壓燒結，製作燒結體。First, Fe powder, Co powder, Si powder, B powder, and Nb powder are prepared. Furthermore, in order to obtain the target material as Example 1 of the present invention, the composition formula with atomic ratio is (Fe 0.90 Co 0.10 ) 67 Si 13.5 B 14.5 Nb 5 , (a=0.10, b=0, X+Y=28, X /Y=0.9, Z=5), after weighing the powders prepared above, mix them in a V-type mixer to obtain mixed powders. Then, the 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, under the conditions of 750° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.
為了獲得作為本發明例2的靶材，準備Fe粉末、Co粉末、Si粉末、B粉末及Nb粉末，以原子比的組成式為(Fe0.70 Co0.30 )67 Si13.5 B14.5 Nb5 、（a=0.30、b=0、X+Y=28、X/Y=0.9、Z=5）的方式，稱重上述所準備的各粉末後，在V型混合機中混合，獲得混合粉末。然後，將該混合粉末填充到軟鐵製的膠囊中，在450℃、4小時的條件下進行脫氣密封。然後，在750℃、122 MPa、1小時的條件下，藉由HIP對所述膠囊進行加壓燒結，製作燒結體。In order to obtain the target material of Example 2 of the present invention, Fe powder, Co powder, Si powder, B powder, and Nb powder were prepared, and the composition formula in atomic ratio was (Fe 0.70 Co 0.30 ) 67 Si 13.5 B 14.5 Nb 5 , (a =0.30, b=0, X+Y=28, X/Y=0.9, Z=5), after weighing the powders prepared above, they are mixed in a V-type mixer to obtain mixed powders. Then, the 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, under the conditions of 750° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.
為了獲得作為本發明例3的靶材，準備Fe粉末、Co粉末、Si粉末、B粉末及Nb粉末，以原子比的組成式為(Fe0.95 Co0.05 )84 Si3.5 B11.5 Nb1 、（a=0.05、b=0、X+Y=15、X/Y=0.3、Z=1）的方式，稱重上述所準備的各粉末後，在V型混合機中混合，獲得混合粉末。然後，將該混合粉末填充到軟鐵製的膠囊中，在450℃、4小時的條件下進行脫氣密封。然後，在950℃、122 MPa、1小時的條件下，藉由HIP對所述膠囊進行加壓燒結，製作燒結體。In order to obtain the target material of Example 3 of the present invention, Fe powder, Co powder, Si powder, B powder, and Nb powder were prepared, and the composition formula in atomic ratio was (Fe 0.95 Co 0.05 ) 84 Si 3.5 B 11.5 Nb 1 , (a =0.05, b=0, X+Y=15, X/Y=0.3, Z=1), after weighing the powders prepared above, they are mixed in a V-type mixer to obtain mixed powders. Then, the 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, under the conditions of 950° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.
為了獲得作為本發明例4的靶材，準備Fe粉末、Co粉末、Si粉末、B粉末及Nb粉末，以原子比的組成式為(Fe0.05 Co0.95 )45 Si23.3 B11.7 Nb20 、（a=0.95、b=0、X+Y=35、X/Y=2.0、Z=20）的方式，稱重上述所準備的各粉末後，在V型混合機中混合，獲得混合粉末。然後，將該混合粉末填充到軟鐵製的膠囊中，在450℃、4小時的條件下進行脫氣密封。然後，在950℃、122 MPa、1小時的條件下，藉由HIP對所述膠囊進行加壓燒結，製作燒結體。In order to obtain the target material of Example 4 of the present invention, Fe powder, Co powder, Si powder, B powder and Nb powder were prepared, and the composition formula of atomic ratio was (Fe 0.05 Co 0.95 ) 45 Si 23.3 B 11.7 Nb 20 , (a =0.95, b=0, X+Y=35, X/Y=2.0, Z=20), after weighing the powders prepared above, they are mixed in a V-type mixer to obtain mixed powders. Then, the 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, under the conditions of 950° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.
為了獲得作為本發明例5的靶材，準備Fe粉末、Co粉末、Ni粉末、Si粉末、B粉末及Nb粉末，以原子比的組成式為(Fe0.60 Co0.10 Ni0.30 )67 Si13.5 B14.5 Nb5 、（a=0.1、b=0.3、X+Y=28、X/Y=0.9、Z=5）的方式，稱重上述所準備的各粉末後，在V型混合機中混合，獲得混合粉末。然後，將該混合粉末填充到軟鐵製的膠囊中，在450℃、4小時的條件下進行脫氣密封。然後，在950℃、122 MPa、1小時的條件下，藉由HIP對所述膠囊進行加壓燒結，製作燒結體。In order to obtain the target material of 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 was (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 the powders prepared above, mix them in a V-type mixer to obtain Mix the powder. Then, the 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, under the conditions of 950° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.
為了獲得作為比較例的靶材，準備原子比的組成式為Fe67 -Si13.5 -B14.5 -Nb5 （a=0、b=0、X+Y=28、X/Y=0.9、Z=5）的氣體霧化粉，填充到軟鐵製的膠囊中，在450℃、4小時的條件下進行脫氣密封。然後，在950℃、122 MPa、1小時的條件下，藉由HIP對上述膠囊進行加壓燒結，製作燒結體。In order to obtain a target as a comparative example, the composition formula of the atomic ratio is Fe 67 -Si 13.5 -B 14.5 -Nb 5 (a=0, b=0, X+Y=28, X/Y=0.9, Z= 5) The gas atomized powder is filled into soft iron capsules and degassed and sealed at 450°C for 4 hours. Then, under the conditions of 950° C., 122 MPa, and 1 hour, the capsule was pressure-sintered by HIP to produce a sintered body.
對上述獲得的各燒結體實施機械加工，製作靶材。此時，可確認到作為本發明例1～本發明例5的靶材在機械加工時均不產生裂紋，並且，精加工後的表面不產生凹凸，表面為平滑的狀態。 另一方面，作為比較例的靶材在機械加工時產生裂紋，無法機械加工成靶材形狀。Each sintered body obtained above was subjected to mechanical processing to produce a target. At this time, it was confirmed that none of the target materials of Inventive Example 1 to Inventive Example 5 produced cracks during machining, and the surface after finishing did not produce unevenness and the surface was in a smooth state. On the other hand, the target material as a comparative example had cracks during machining, and could not be machined into a target shape.
對於上述獲得的各燒結體，測定了在靶材的成為侵蝕面的面的平面方向上，相當於外周部的4個位置和相當於中央部的位置的合計5處的維氏硬度。再者，測定間隔是設定壓痕之間不受測定影響的距離進行測定的。而且，維氏硬度按照JIS Z 2244，使用明石製作所股份有限公司製造的MVK-E，測定了負荷為9.8 N、加壓時間為10秒時的值。其結果如表1所示。For each of the sintered bodies obtained above, the Vickers hardness was measured at a total of 5 locations corresponding to the outer peripheral portion and the central portion in the plane direction of the surface serving as the erosion surface of the target. Furthermore, the measurement interval is measured by setting the distance between the indentations that is not affected by the measurement. In addition, the Vickers hardness was measured at a load of 9.8 N and a pressing time of 10 seconds using MVK-E manufactured by Akashi Manufacturing Co., Ltd. in accordance with JIS Z 2244. The results are shown in Table 1.
[表1]
作為比較例的靶材的維氏硬度的平均值超過了1100 HV。 與此相對，確認到本發明例1～本發明例5的靶材的維氏硬度的平均值均處於250 HV～1100 HV的範圍。 藉此可確認，本發明的靶材是在機械加工時抑制裂紋或缺口的產生、並且精加工後的表面不產生凹凸、表面平滑的靶材。藉此，本發明的靶材抑制異常放電的誘發或結核飛散而附著在被處理材上，從而能夠期待作為用於形成軟磁性膜的靶材而有用。The average value of the Vickers hardness of the target as a comparative example exceeded 1100 HV. On the other hand, it was confirmed that the average value of the Vickers hardness of the target materials of Inventive Example 1 to Inventive Example 5 was in the range of 250 HV to 1100 HV. It can be confirmed from this that the target of the present invention is a target that suppresses the occurrence of cracks or notches during machining, does not produce unevenness on the surface after finishing, and has a smooth surface. Thereby, the target material of the present invention suppresses the induction of abnormal discharge or the scattering of nodules to adhere to the material to be processed, and can be expected to be useful as a target material for forming a soft magnetic film.
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| JPH02163911A (en) * | 1988-12-16 | 1990-06-25 | Matsushita Electric Ind Co Ltd | Soft magnetic alloy film and manufacture thereof |
| CN101952470A (en) * | 2008-02-20 | 2011-01-19 | 三菱制钢株式会社 | Powder for iron-based sintered alloy |
| JP2011026702A (en) * | 2009-07-01 | 2011-02-10 | Hitachi Metals Ltd | SPUTTERING TARGET MATERIAL OF Fe-Co-Ni-BASED ALLOY |
| JP2012169021A (en) * | 2011-02-16 | 2012-09-06 | Sanyo Special Steel Co Ltd | Soft magnetic alloy for magnetic recording, sputtering target material and magnetic recording medium |
| JP2013084322A (en) * | 2011-10-07 | 2013-05-09 | Hitachi Metals Ltd | Soft magnetic film for thermally assisted magnetic recording medium and manufacturing method therefor |
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| JPH02263416A (en) * | 1988-12-15 | 1990-10-26 | Matsushita Electric Ind Co Ltd | Method for manufacturing soft magnetic alloy film |
| JPH11328619A (en) * | 1998-05-11 | 1999-11-30 | Alps Electric Co Ltd | Thin film magnetic head with magnetic impedance effect element |
| JP5385018B2 (en) * | 2009-06-12 | 2014-01-08 | 山陽特殊製鋼株式会社 | Raw material powder for sputtering target material for producing soft magnetic film having high sputtering rate and sputtering target material |
| JP6405261B2 (en) | 2014-05-01 | 2018-10-17 | 山陽特殊製鋼株式会社 | Soft magnetic alloy for magnetic recording, sputtering target material, and magnetic recording medium |
| JP2016149170A (en) | 2015-02-12 | 2016-08-18 | 日立金属株式会社 | Fe-Co-Nb BASED ALLOY SPUTTERING TARGET MATERIAL AND SOFT MAGNETIC FILM |
| JP2017208147A (en) | 2016-05-16 | 2017-11-24 | 日立金属株式会社 | Sputtering target for forming soft magnetic ground layer and soft magnetic ground layer |
| JP2018188726A (en) * | 2017-04-28 | 2018-11-29 | 日立金属株式会社 | Sputtering target and production method thereof |
| JP7238527B2 (en) * | 2018-08-09 | 2023-03-14 | 株式会社プロテリアル | Soft magnetic film for heat-assisted magnetic recording medium and sputtering target for forming soft magnetic film for heat-assisted magnetic recording medium |
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| 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 |
| CN101952470A (en) * | 2008-02-20 | 2011-01-19 | 三菱制钢株式会社 | Powder for iron-based sintered alloy |
| JP2011026702A (en) * | 2009-07-01 | 2011-02-10 | Hitachi Metals Ltd | SPUTTERING TARGET MATERIAL OF Fe-Co-Ni-BASED ALLOY |
| JP2012169021A (en) * | 2011-02-16 | 2012-09-06 | Sanyo Special Steel Co Ltd | Soft magnetic alloy for magnetic recording, sputtering target material and magnetic recording medium |
| JP2013084322A (en) * | 2011-10-07 | 2013-05-09 | Hitachi Metals Ltd | Soft magnetic film for thermally assisted magnetic recording medium and manufacturing method therefor |
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| WO2021039711A1 (en) | 2021-03-04 |
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