WO2023038081A1 - Matériau cible de pulvérisation cathodique - Google Patents

Matériau cible de pulvérisation cathodique Download PDF

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WO2023038081A1
WO2023038081A1 PCT/JP2022/033712 JP2022033712W WO2023038081A1 WO 2023038081 A1 WO2023038081 A1 WO 2023038081A1 JP 2022033712 W JP2022033712 W JP 2022033712W WO 2023038081 A1 WO2023038081 A1 WO 2023038081A1
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phase
content
target material
alloy
total content
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慶明 松原
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山陽特殊製鋼株式会社
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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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/14—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on borides
    • 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
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/127—Structure or manufacture of heads, e.g. inductive
    • G11B5/33—Structure or manufacture of flux-sensitive heads, i.e. for reproduction only; Combination of such heads with means for recording or erasing only
    • G11B5/39—Structure or manufacture of flux-sensitive heads, i.e. for reproduction only; Combination of such heads with means for recording or erasing only using magneto-resistive devices or effects
    • 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

Definitions

  • the present invention relates to sputtering target materials. Specifically, the present invention relates to a CoFeB alloy-based sputtering target material that can be suitably used for manufacturing a magnetic layer.
  • Magnetic tunnel junction (MTJ) elements are used in magnetic devices such as magnetic heads and magnetic random access memories (MRAM).
  • MRAM magnetic random access memories
  • MTJ devices exhibit features such as high tunneling magnetoresistance (TMR) signal and low switching current density (Jc).
  • TMR tunneling magnetoresistance
  • Jc switching current density
  • a magnetic tunnel junction (MTJ) element usually has a structure in which a shielding layer made of MgO is sandwiched between two magnetic layers made of a CoFeB alloy.
  • This magnetic layer is a thin film obtained by sputtering using a target material made of a CoFeB alloy.
  • B boron
  • Patent Document 1 discloses a Co--Fe--B alloy target material in which a boride phase is finely dispersed in a cross-sectional microstructure.
  • Patent Document 2 a target material that suppresses particle generation includes a B high concentration phase and a B low concentration phase, and a magnetic material in which the B high concentration phase is finely dispersed. Sputtering targets have been proposed.
  • Patent Document 3 discloses a sputtering target material in which generation of particles is reduced by suppressing the formation of (CoFe) 3 B, Co 3 B and Fe 3 B.
  • Patent Document 4 discloses a magnetic material sputtering target in which generation of particles is suppressed by setting the oxygen content to 100 wtppm or less.
  • Patent Document 5 discloses a sputtering target material made of a CoFeB-based alloy with a hydrogen content reduced to 20 ppm or less for improving mechanical strength, wherein the CoFeB-based alloy contains 1 or Sputtering target materials to which two or more other elements have been added are disclosed.
  • the ratio of B is 33 at. % or more 50 at. % or less of a Co--Fe--B alloy, which suppresses the generation of particles by containing a non-B alloy phase.
  • Patent Document 7 discloses that the ratio of B is 33 at.
  • a retarded sputtering target material is disclosed.
  • the boron content when using a powder sintering method to industrially produce a target material with a boron content of 50 at%, the boron content may be more than 50 at% due to the difference between the desired composition and the finished composition.
  • the boron content is large and cases where the boron content is less than 50 atomic %.
  • the metal structure of the target material manufactured for the purpose of having a boron content of 50 at % varies greatly depending on the lot, and tends to lack stability in sputtering.
  • the pure B phase generated when the boron content exceeds 50 at % causes the generation of particles during sputtering, which poses a problem of impeding productivity.
  • the ratio of the total content of Co and Fe to the content of B [total content of Co and Fe: content of B] is a phase in which the atomic ratio is 1: 1
  • the ratio of the total content of Co and Fe to the content of B [total content of Co and Fe: content of B] is 2:1 in atomic number ratio means a phase that is
  • An object of the present invention is to provide a target material made of a CoFeB-based alloy having a boron content of close to 50 at %, which provides excellent magnetic performance and which reduces the generation of particles during sputtering.
  • the sputtering target material according to the present invention is made of an alloy containing Co and/or Fe, B, one or more additive elements M, and the balance being inevitable impurities.
  • the alloy constituting the sputtering target material according to the present invention may be simply referred to as "alloy".
  • the content of B in the alloy is 49.0 atomic % or more and 52.0 atomic % or less.
  • One or more additive elements M are selected from the group consisting of Mo, W, Nb, Ta, Zr and Hf.
  • the total content of one or more additive elements M in the alloy is 0.1 atomic % or more and 2.0 atomic % or less.
  • the “total content” means the content of the one additional element M
  • the alloy contains two or more additional elements M
  • the “total content ” means the total content of the two or more additive elements M (the same shall apply hereinafter).
  • the total content (at%) of Co and Fe in the alloy is x
  • the content (at%) of B in the alloy is y
  • the total content of one or more additive elements M in the alloy The sputtering target material according to the present invention satisfies the following formulas 1 and 2, where (at. %) is z and the composition of the alloy is represented by the composition formula: (CoFe) x B y M z . 6 ⁇ (y ⁇ x) ⁇ 0 (Formula 1) 4 ⁇ (y ⁇ x)/z ⁇ 0 (Formula 2)
  • the sputtering target material according to the present invention contains a boride phase containing B and one or more additive elements M.
  • a peak derived from a boride phase containing B and one or more additive elements M is detected.
  • the sputtering target material according to the present invention is made of an alloy in which the content of boron and one or more additive elements M is appropriate.
  • one or more additional elements M suppress the formation of the pure B phase.
  • particle generation is significantly reduced. According to the sputtering using the target material according to the present invention, it is possible to efficiently obtain a magnetic film of high quality and high performance.
  • the target material according to the present invention is suitable for manufacturing magnetic films used in magnetic devices such as magnetic heads and MRAMs.
  • FIG. 1 is a diffraction pattern obtained by X-ray diffraction of a sputtering target material according to one embodiment of the present invention.
  • CoFeB-based alloy is a concept that includes the case where either Co or Fe is 0 atomic % in the composition.
  • X to Y indicating a range means "X or more and Y or less”.
  • the sputtering target material according to the present invention comprises an alloy containing Co and/or Fe, B, and one or more additive elements M, with the balance being inevitable impurities.
  • the alloy constituting the sputtering target material according to the present invention is a CoFeB alloy containing one or more additive elements M.
  • one or more additive elements M are selected from the group consisting of Mo, W, Nb, Ta, Zr and Hf.
  • the alloy may optionally contain other elements as long as the effects of the present invention are not impaired. O, S, C, N, etc. are illustrated as an unavoidable impurity.
  • the content of B in the alloy is 49.0 at% or more and 52.0 at% or less, and the total content of one or more additional elements M in the alloy is 0.1 at% or more and 2.0 at% or less. be.
  • the alloy contains two or more additional elements M selected from the group consisting of Mo, W, Nb, Ta, Zr and Hf, the total content is 0.1 at% or more and 2.0 at% or less. .
  • the magnetic performance of the resulting magnetic film is improved.
  • One or more additive elements M selected from Mo, W, Nb, Ta, Zr and Hf can form borides in the metallographic structure of the CoFeB alloy.
  • one or two or more additive elements M form borides with excessive B, so that even though the alloy contains B at a high content of 49.0 at% or more and 52.0 at% or less, Formation of the pure B phase, which causes particle generation, is suppressed.
  • the target material according to the present invention significantly reduces particle generation during sputtering.
  • a magnetic film having high magnetic performance can be efficiently manufactured by sputtering using the target material according to the present invention. By incorporating this magnetic film, a high TMR signal of the MTJ element is achieved.
  • the target material according to the present invention is suitable for manufacturing magnetic films used in magnetic devices such as magnetic heads and MRAMs.
  • the content of B in the alloy is 49.0 at% or more, preferably more than 49.0 at%, more preferably 49.3 at% or more, and 49.5 at% or more. It is even more preferable to have From the viewpoint of suppressing excessive formation of pure B phase, the content of B in the alloy is 52.0 at% or less, preferably less than 52.0 at%, more preferably 51.5 at% or less, It is more preferably 51.0 atomic % or less.
  • the total content of one or more additional elements M in the alloy is 0.1 at% or more, and 0.2 at%. It is preferably at least 0.3 at %, more preferably at least 0.4 at %.
  • (CoFe):B 1:1 (CoFe)B phase and a pure B phase are formed.
  • the one or more additional elements M are not only a pure B phase but also (CoFe)B Reacts with B in phase to form excess boride phase.
  • Excessive boride phase formation by one or more additive elements M can cause particle generation during sputtering. From the viewpoint of avoiding excessive boride phase formation due to one or more additional elements M, the total content of one or more additional elements M in the CoFeB alloy is 2.0 at% or less.
  • (CoFe)B phase is a concept including the case where either Co or Fe is 0 at%, and in addition to the CoFeB phase, the CoB phase and / or the FeB phase are included. .
  • One or more additive elements M are not particularly limited as long as they are selected from the group consisting of Mo, W, Nb, Ta, Zr and Hf, but are preferably selected from Mo and W. Both Mo and W have similar boride-forming ability to Co and Fe. Therefore, Mo and W do not react with B in the (CoFe)B phase to form an excessive boride phase in the metal structure of a CoFeB-based alloy with a B content of approximately 50 at%. can suppress the formation of the pure B phase.
  • the CoFeB-based alloy constituting the sputtering target material according to the present invention is represented by the composition formula: (CoFe) x B y M z .
  • x is the total content (at%) of Co and Fe
  • y is the content (at%) of B
  • z is the total content of one or more additional elements M. (at.%).
  • M is one or more additive elements selected from the group consisting of Mo, W, Nb, Ta, Zr and Hf.
  • the content y of B in the alloy is 49.0 atomic % or more and 52.0 atomic % or less.
  • y may exceed 49.0 at %, more preferably 49.3 at % or more, further preferably 49.5 at % or more, and 52 It may be less than 0.0 at %, more preferably 51.5 at % or less, and even more preferably 51.0 at % or less.
  • the total content z of one or more additive elements M in the alloy is 0.1 atomic % or more and 2.0 atomic % or less. From the viewpoint of reducing particle generation during sputtering, z is preferably 0.2 at% or more, more preferably 0.3 at% or more, further preferably 0.4 at% or more, and It is preferably 1.9 at% or less, more preferably 1.8 at% or less, and even more preferably 1.7 at% or less.
  • the total content x of Co and Fe is not particularly limited as long as the content y of B and the total content z of one or more additive elements M satisfy the above range, but the effects of the present invention can be obtained.
  • x is preferably less than 50.0 at %, more preferably 49.9 at % or less, from the viewpoint that Preferably, x is 46.0 atomic % or more.
  • the blending ratio of Co and Fe in the alloy is not particularly limited as long as the effects of the present invention can be obtained, and can be appropriately adjusted within the range of 0:100 to 100:0.
  • the total content x (at %) of Co and Fe and the content y (at %) of B satisfy Formula 1 below. 6 ⁇ (y ⁇ x) ⁇ 0 (Formula 1)
  • the difference (yx) is more preferably 4 or less, more preferably 2 or less. If the difference (y ⁇ x) is less than 0, the B content is less than the total content of Co and Fe, so that no pure B phase is formed, but desired magnetic performance may not be obtained. From the viewpoint of improving magnetic performance, the preferred difference (yx) is 0 or more.
  • the total content x (at%) of Co and Fe, the content y (at%) of B, and the total content z of one or more additive elements M (at %) satisfies Equation 2 below. 4 ⁇ (y ⁇ x)/z ⁇ 0 (Formula 2)
  • the ratio (yx)/z of the difference (yx) and the total content z of one or more additional elements M is 4 or less
  • the ratio (yx)/z is more preferably 3 or less, more preferably 2 or less.
  • a target material having a ratio (yx)/z of 0 or more enables efficient production of a magnetic film having excellent magnetic performance. From this point of view, the more preferable ratio (yx)/z is 0.5 or more.
  • a boride phase containing one or more additional elements M is formed in an appropriate amount.
  • the formation of the pure B phase is suppressed, and particle generation during sputtering is reduced.
  • the sputtering target material made of this CoFeB-based alloy contains a boride phase containing B and one or more additional elements M.
  • a peak derived from a boride phase containing B and one or more additional elements M is detected. be done. The details of the X-ray diffraction measurement will be described later in Examples.
  • the boride phase may be a boride phase ([M, B] phase) consisting of a binary compound of B and the additive element M, or It may be a boride phase ([Co, M, B] phase or [Fe, M, B] phase) consisting of a ternary compound of element M and Co or Fe, or B, additional element M and Co It may be a boride phase ([Co, Fe, M, B] phase) composed of a quaternary compound with Fe.
  • the sputtering target material according to the present invention may contain one type of boride phase, or may contain two or more types of boride phases.
  • the sputtering target material according to the present invention is selected from [M, B] phase, [Co, M, B] phase, [Fe, M, B] phase and [Co, Fe, M, B] phase. 1 or 2 or more may be included.
  • the [M, B] phase means the entire phase consisting of B and the additional element M, and the composition of the [M, B] phase is not particularly limited as long as it consists of B and the additional element M.
  • the [M, B] phase for example, an MB phase in which the ratio of the content of the additive element M to the content of B [content of the additive element M: content of B] is 1:1 in atomic number ratio but not limited thereto, other phases, for example, the ratio of the content of the additive element M to the content of B [content of the additive element M: content of B] is the number of atoms M 2 B phase with a ratio of 2:1, MB with a ratio of the content of the additive element M to the content of B [content of the additive element M: content of B] with an atomic ratio of 1:2 Two phases, etc. are also included in the [M, B] phase.
  • the [Co, M, B] phase means the entire phase consisting of B, the additive element M and Co, and the composition of the [Co, M, B] phase is particularly Not limited.
  • the [Co, M, B] phase for example, the ratio of the total content of the additive elements M and Co to the content of B [total content of the additive elements M and Co: content of B] is the atomic ratio (CoM) B phase with a ratio of 1:1 in other phases, for example, the ratio of the total content of the additional elements M and Co to the content of B [addition (CoM) 2 B phase having an atomic ratio of 2:1 in the total content of elements M and Co: content of B], the ratio of the total content of additional elements M and Co to the content of B [addition
  • the [Co, M, B] phase also includes a (CoM) B2 phase in which the atomic ratio of the total content of the elements M and Co:the content of B] is 1:2.
  • the [Fe, M, B] phase means the entire phase consisting of B, the additional element M and Fe, and the composition of the [Fe, M, B] phase is particularly as long as it consists of B, the additional element M and Fe Not limited.
  • the [Fe, M, B] phase for example, the ratio of the total content of the additive elements M and Fe to the content of B [total content of the additive elements M and Fe: content of B] is the atomic ratio (FeM) B phase, which is 1:1 at , but is not limited to this, and other phases, for example, the ratio of the total content of the additional elements M and Fe to the content of B [addition (FeM) 2 B phase having an atomic ratio of 2:1 in the total content of elements M and Fe: content of B], the ratio of the total content of additional elements M and Fe to the content of B [addition
  • the [Fe, M, B] phase also includes a (FeM) B2 phase in which the atomic ratio of the total content of the elements M and Fe
  • the [Co, Fe, M, B] phase means the entire phase consisting of B, the additional element M, Co and Fe, and the composition of the [Co, Fe, M, B] phase is It is not particularly limited as long as it consists of Co and Fe.
  • the [Co, Fe, M, B] phase for example, the ratio of the total content of the additive elements M, Co and Fe to the content of B [total content of the additive elements M, Co and Fe: content of B amount] is 1:1 in atomic number ratio (CoFeM)B phase, but is not limited thereto, other phases, for example, the total content of additional elements M, Co and Fe and B (CoFeM) 2 B phase in which the ratio of the content of [total content of additional elements M, Co and Fe: content of B] is 2:1 in terms of atomic number, the sum of the additional elements M, Co and Fe (CoFeM)B2 phase, etc., in which the ratio of the content to the content of B [total content of additive elements M, Co and Fe: content of B]
  • the boride phase consists of a ternary compound of B, additive element M1 and additive element M2 ([ M1 , M2 , B] phase ) , or a boride phase ([Co, M 1 , M 2 , B] phase or [ Fe , M 1 , M 2 , B] phase), or a boride phase ( [ Co, Fe , M 1 , M 2 , B] phases).
  • the sputtering target material according to the present invention may contain one type of boride phase, or may contain two or more types of boride phases.
  • the sputtering target material according to the present invention includes [M 1 , M 2 , B] phase, [Co, M 1 , M 2 , B] phase, [Fe, M 1 , M 2 , B] phase and [ Co, Fe, M 1 , M 2 , B] phases may be included.
  • the [M 1 , M 2 , B] phase means the entire phase consisting of B, the additive element M 1 and the additive element M 2 , and the composition of the [M 1 , M 2 , B] phase is composed of B and the additive element There is no particular limitation as long as it consists of M1 and the additional element M2 .
  • the ratio of the total content of the additive element M 1 and the additive element M 2 to the content of B [the total content of the additive element M 1 and the additive element M 2 : content of B] is 1:1 in atomic number ratio (M 1 M 2 ) B phase, but is not limited thereto, other phases such as additive element M 1 and additive
  • the ratio of the total content of element M2 to the content of B [total content of additive element M1 and additive element M2 : content of B] is 2:1 in atomic number ratio ( M1M2 ) 2 B phase
  • the ratio of the total content of the additive element M1 and the additive element M2 to the content of B [total content of the additive element M1 and the additive element M2 : content of B] is the atomic ratio
  • the [M 1 , M 2 , B] phase also includes the (M 1 M 2 )B 2 phase, which is 1:2 at .
  • the [Co, M 1 , M 2 , B] phase means the entire phase consisting of B, the additive element M 1 , the additive element M 2 and Co, and the composition of the [Co, M 1 , M 2 , B] phase is not particularly limited as long as it consists of B, the additive element M1 , the additive element M2 , and Co.
  • the ratio of the total content of additive element M 1 , additive element M 2 and Co to the content of B [additive element M 1 , additive element M 2 and the total content of Co: content of B] is 1:1 in atomic number ratio (CoM 1 M 2 ) B phase, but is not limited thereto, and other phases such as
  • the ratio of the total content of additive element M 1 , additive element M 2 and Co to the content of B [total content of additive element M 1 , additive element M 2 and Co: content of B] is the atomic ratio
  • the ratio of the total content of (CoM 1 M 2 ) 2 B phase, additive element M 1 , additive element M 2 and Co to the content of B [additive element M 1 , additive element M 2 and Co A (CoM 1 M 2 )B 2 phase or the like in which the atomic ratio of the total content of B to the content of B is 1: 2 is also included in the [Co, M 1 , M 2 , B] phase
  • the [Fe, M 1 , M 2 , B] phase means the entire phase consisting of B, the additive element M 1 , the additive element M 2 and Fe, and the composition of the [Fe, M 1 , M 2 , B] phase is not particularly limited as long as it consists of B, the additive element M1 , the additive element M2 , and Fe.
  • the ratio of the total content of the additive element M 1 , the additive element M 2 and Fe to the content of B [additional element M 1 , additive element M 2 and the total content of Fe: content of B] is 1:1 in atomic number ratio (FeM 1 M 2 ) B phase, but not limited thereto, other phases such as
  • the ratio of the total content of the additional element M 1 , the additional element M 2 and Fe to the content of B [the total content of the additional element M 1 , the additional element M 2 and Fe: the content of B] is the atomic ratio
  • the ratio of the total content of (FeM 1 M 2 ) 2 B phase, additive element M 1 , additive element M 2 and Fe to the content of B [additive element M 1 , additive element M 2 and Fe (FeM 1 M 2 )B 2 phase, etc., in which the total content of B: content of B] is 1:2 in atomic number ratio is also included in the [Fe, M 1
  • [Co, Fe, M 1 , M 2 , B] phase means the entire phase consisting of B, additional element M 1 , additional element M 2 , Co and Fe, and [Co, Fe, M 1 , M 2 , B] phase is not particularly limited as long as it consists of B, the additive element M1 , the additive element M2 , Co and Fe.
  • phase for example, the ratio of the total content of additive element M 1 , additive element M 2 , Co and Fe to the content of B [total content of additive element M 1 , additive element M 2 , Co and Fe: (CoFeM 1 M 2 ) 2 B phase, the additive element M 1 , the additive element M 2 , the ratio of the total content of Co and Fe to the content of B
  • FIG. 1 An example of a diffraction pattern obtained by X-ray diffraction measurement of a sputtering target material according to one embodiment of the present invention is shown in FIG.
  • This target material is made of a CoFeB alloy containing Zr as an additive element M.
  • the peaks derived from the boride phase ZrB 2 phase, which is a compound of B and the additive element Zr, are shown as ⁇ and ⁇ .
  • the manufacturing method of the sputtering target material according to the present invention includes a sintering step of sintering the raw material powder. Specifically, this manufacturing method includes a step of forming a sintered body by so-called powder metallurgy, in which raw material powder is heated under high pressure and solidified. A target material is obtained by processing this sintered body into an appropriate shape by mechanical means or the like.
  • the raw material powder consists of a large number of particles.
  • each particle constituting the raw material powder contains Co and/or Fe, B, and one or more additional elements M, and the balance is an alloy made of unavoidable impurities.
  • the content of B in the alloy is 49.0 atomic % or more and 52.0 atomic % or less.
  • One or more additive elements M are selected from the group consisting of Mo, W, Nb, Ta, Zr and Hf.
  • the total content of one or more additive elements M in the alloy is 0.1 atomic % or more and 2.0 atomic % or less.
  • the content of boron B and one or more additive elements M is used in the raw material powder, so that the raw material powder is sintered to obtain a target material.
  • the formation of pure B phase in the metallographic structure of is suppressed.
  • the generation of particles during sputtering is remarkably reduced, and a magnetic film having excellent magnetic performance can be efficiently obtained.
  • the raw material powder can be manufactured by the atomization method.
  • the atomization method is not particularly limited, and may be a gas atomization method, a water atomization method, or a centrifugal force atomization method.
  • a known atomization device and manufacturing conditions are appropriately selected and used.
  • the raw material powder is sieved before the sintering process.
  • the purpose of this sieving is to remove particles (coarse powder) having a particle size of 500 ⁇ m or more, which hinder sintering.
  • the method and conditions for solidifying and molding the raw material powder to obtain a sintered body are not particularly limited.
  • a hot isostatic pressure method HIP method
  • a hot press method a hot press method
  • a spark plasma sintering method SPS method
  • a hot extrusion method or the like is appropriately selected.
  • the method of processing the obtained sintered body is not particularly limited, and known mechanical processing means can be used.
  • the target material obtained by the manufacturing method according to the present invention is suitably used, for example, in sputtering for forming magnetic thin films used in MTJ elements.
  • This target material reduces particle generation during sputtering despite the high boron content. According to this target material, it is possible to efficiently manufacture a high-performance and high-quality magnetic film suitable for magnetic devices such as magnetic heads and MRAMs.
  • the raw material powder obtained by the gas atomization method was sieved to remove coarse powder with a diameter of 500 ⁇ m or more.
  • the raw material powder after sieving is filled in a can made of carbon steel (outer diameter 220 mm, inner diameter 210 mm, length 200 mm) and vacuum degassed. C., a pressure of 100 to 150 MPa, and a holding time of 1 to 5 hours to produce a sintered body.
  • the obtained sintered body was processed into a disk shape having a diameter of 180 mm and a thickness of 7 mm by wire cutting, lathe processing, and surface polishing to obtain a sputtering target material.
  • Sputtering was performed by DC magnetron sputtering using the target materials of Examples and Comparative Examples. Sputtering conditions are as follows. Substrate: Aluminum substrate (diameter 95 mm, thickness 1.75 mm) Chamber atmosphere: argon gas Chamber pressure: 0.9 Pa After sputtering, particles with a diameter of 0.1 ⁇ m or more adhering to an aluminum substrate with a diameter of 95 mm were counted using an Optical Surface Analyzer, and graded according to the following criteria. The results are shown in Table 1-2 below as particle evaluation. A: The number of particles is 10 or less B: The number of particles is more than 10 and 200 or less C: The number of particles is more than 200
  • the total content z of the additive element M is 0.1 at% or more and 2.0 at% or less, and the boron content y is 49.0 at% or more and 52.0 at%.
  • the boron content y is 49.0 at% or more and 52.0 at%.
  • Example 1-13 particle generation was significantly reduced.
  • due to excessive formation of the boride phase containing the additive element M many particles were generated during sputtering.
  • Comparative Example 3 in which the total content z of the additive element M exceeds 2.0 at%, Comparative Example 4 containing no additive element M, and Comparative Examples 5 and 6 in which the boron content y exceeds 52 at%, pure Due to the formation of the B phase or excessive formation of the boride phase due to the additional element M, many particles were generated during sputtering. Further, in Comparative Examples 1 and 2, in which the boron content is small, the performance improvement effect of the resulting magnetic film cannot be expected.
  • the target materials of the examples are rated higher than the target materials of the comparative examples. From this evaluation result, the superiority of the present invention is clear.
  • the sputtering target material described above can be applied to manufacture magnetic layers in various applications.

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Electromagnetism (AREA)
  • Physics & Mathematics (AREA)
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  • Manufacturing & Machinery (AREA)
  • Physical Vapour Deposition (AREA)
  • Magnetic Heads (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

L'objectif de la présente invention est de fournir un matériau cible à base d'alliage de CoFeB qui réduit la génération de particules pendant la pulvérisation cathodique. L'invention concerne un matériau cible de pulvérisation cathodique comprenant un alliage contenant du Co et/ou du Fe, et du B et au moins un élément additif M, la portion restante étant constituée d'inévitables impuretés. La quantité de B contenue dans l'alliage est de 49,0 à 52,0 % at. Ledit élément additif M est choisi dans le groupe constitué par Mo, W, Nb, Ta, Zr et Hf. La quantité totale dudit élément additif M contenue dans l'alliage est de 0,1 à 2,0 % at.
PCT/JP2022/033712 2021-09-09 2022-09-08 Matériau cible de pulvérisation cathodique WO2023038081A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2020025077A (ja) * 2018-08-02 2020-02-13 株式会社東芝 複数の扁平磁性金属粒子、圧粉材料及び回転電機
WO2020175424A1 (fr) * 2019-02-26 2020-09-03 山陽特殊製鋼株式会社 Alliage approprié pour un matériau cible de pulvérisation
JP2020143372A (ja) * 2015-09-18 2020-09-10 山陽特殊製鋼株式会社 Ｃｏ−Ｆｅ−Ｂ系合金ターゲット材
JP2021109980A (ja) * 2020-01-06 2021-08-02 山陽特殊製鋼株式会社 スパッタリングターゲット材の製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2020143372A (ja) * 2015-09-18 2020-09-10 山陽特殊製鋼株式会社 Ｃｏ−Ｆｅ−Ｂ系合金ターゲット材
JP2020025077A (ja) * 2018-08-02 2020-02-13 株式会社東芝 複数の扁平磁性金属粒子、圧粉材料及び回転電機
WO2020175424A1 (fr) * 2019-02-26 2020-09-03 山陽特殊製鋼株式会社 Alliage approprié pour un matériau cible de pulvérisation
JP2021109980A (ja) * 2020-01-06 2021-08-02 山陽特殊製鋼株式会社 スパッタリングターゲット材の製造方法

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