WO2022244243A1 - 切削工具 - Google Patents

切削工具 Download PDF

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Publication number
WO2022244243A1
WO2022244243A1 PCT/JP2021/019381 JP2021019381W WO2022244243A1 WO 2022244243 A1 WO2022244243 A1 WO 2022244243A1 JP 2021019381 W JP2021019381 W JP 2021019381W WO 2022244243 A1 WO2022244243 A1 WO 2022244243A1
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WO
WIPO (PCT)
Prior art keywords
layer
alumina
alumina layer
titanium compound
cutting tool
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2021/019381
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English (en)
French (fr)
Japanese (ja)
Inventor
晋 奥野
貴翔 山西
将仁 引地
史佳 小林
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Sumitomo Electric Hardmetal Corp
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Sumitomo Electric Hardmetal Corp
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 Sumitomo Electric Hardmetal Corp filed Critical Sumitomo Electric Hardmetal Corp
Priority to JP2021572085A priority Critical patent/JP7135262B1/ja
Priority to US17/924,360 priority patent/US12269098B2/en
Priority to EP21940857.2A priority patent/EP4144466B1/en
Priority to PCT/JP2021/019381 priority patent/WO2022244243A1/ja
Priority to CN202180035212.1A priority patent/CN115697599B/zh
Publication of WO2022244243A1 publication Critical patent/WO2022244243A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
    • B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
    • B23B27/148—Composition of the cutting inserts
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/308—Oxynitrides
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/36—Carbonitrides
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/403—Oxides of aluminium, magnesium or beryllium
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/044—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material coatings specially adapted for cutting tools or wear applications
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
    • C23C28/42—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by the composition of the alternating layers
    • 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
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
    • B23B2228/10—Coatings
    • B23B2228/105—Coatings with specified thickness

Definitions

  • the present disclosure relates to cutting tools.
  • Patent Document 1 discloses a coated cutting tool comprising a base material and a coating layer formed on the surface of the base material, wherein the coating layer is on the side of the base material.
  • the lower layer is Ti and at least one selected from the group consisting of C, N, O, and B
  • the intermediate layer contains ⁇ -type Al 2 O 3
  • the upper layer contains TiCN
  • the average of the lower layer The thickness is 4.0 ⁇ m or more and 10.0 ⁇ m or less
  • the average thickness of the intermediate layer is 3.0 ⁇ m or more and 10.0 ⁇ m or less
  • the average thickness of the upper layer is 1.5 ⁇ m or more and 6.5 ⁇ m or less.
  • Patent Document 2 discloses that a surface of a substrate made of cemented carbide, high-speed steel or special steel is coated with boron and one or two metals of groups 4a, 5a and 6a of the periodic table. Boron-containing single-layer coating of any one of carbides, nitrides, carbonitrides, carbonates, nitroxides, and carbonitrides, or multilayer coatings of two or more types, having tensile residual stress. Disclosed is a boron-containing film-coated tool characterized in that the film is coated on the tool surface side rather than the aluminum oxide film.
  • the cutting tool according to the present disclosure is A cutting tool comprising a substrate and a coating provided on the substrate,
  • the coating is a first alumina layer provided on the substrate;
  • a second alumina layer provided immediately above the titanium compound layer A portion of the first alumina layer adjacent to the titanium compound layer forms an interface region,
  • a portion of the first alumina layer that is not the interface region forms a non-interface region,
  • the content of nitrogen in the interface region is 0.2 atomic % or more and 12 atomic % or less
  • the content of nitrogen in the non-interface region is 0 atomic % or more and 0.15 atomic % or less
  • the titanium compound layer includes a multilayer structure layer adjacent to the first alumina layer,
  • the multilayer structure layer consists of a first unit layer and a second unit layer, In the multilayer structure layer, the first unit layers and the second unit layers are alternately laminated,
  • the first unit layer is made of titanium
  • FIG. 1 is a perspective view illustrating one aspect of a substrate of a cutting tool.
  • FIG. 2 is a schematic cross-sectional view of a cutting tool in one aspect of the present embodiment.
  • FIG. 3 is a schematic cross-sectional view of a cutting tool in another aspect of this embodiment.
  • FIG. 4 is a schematic cross-sectional view of a coating layer in one aspect of the present embodiment.
  • FIG. 5 is a schematic cross-sectional view showing an example of a chemical vapor deposition apparatus used for producing a coating.
  • FIG. 6 is a photograph showing the surface quality of the machined surface and the corresponding rank.
  • Patent Documents 1 and 2 the coating having the structure described above improves wear resistance and adhesion between the aluminum oxide layer and other layers in contact with the aluminum oxide layer. Therefore, it is expected that the life of the cutting tool will be extended.
  • the present disclosure has been made in view of the above circumstances, and aims to provide a cutting tool with improved wear resistance and fracture resistance.
  • the cutting tool according to the present disclosure is A cutting tool comprising a substrate and a coating provided on the substrate,
  • the coating is a first alumina layer provided on the substrate;
  • a titanium compound layer provided immediately above the first alumina layer;
  • a second alumina layer provided immediately above the titanium compound layer,
  • a portion of the first alumina layer adjacent to the titanium compound layer forms an interface region,
  • a portion of the first alumina layer that is not the interface region forms a non-interface region,
  • the content of nitrogen in the interface region is 0.2 atomic % or more and 12 atomic % or less
  • the content of nitrogen in the non-interface region is 0 atomic % or more and 0.15 atomic % or less
  • the titanium compound layer includes a multilayer structure layer adjacent to the first alumina layer,
  • the multilayer structure layer consists of a first unit layer and a second unit layer, In the multilayer structure layer, the first unit layers and the second unit layers are alternately laminated,
  • the first unit layer
  • the above-described cutting tool has improved wear resistance and chipping resistance due to the configuration as described above.
  • “wear resistance” means resistance to abrasion of the coating when used for cutting.
  • the term “fracture resistance” means resistance to chipping of the coating when used for cutting.
  • the above cutting tools are used for cutting such as turning. In turning, the hottest part is not the edge of the cutting tool (cutting edge ridge), but the part slightly away from the edge (when the chips come into contact with the edge). is known to be the part that In this case, the edge portion is required to have high hardness, while the portion slightly away from the edge is required to have heat resistance and chipping resistance.
  • coatings have not been designed with consideration given to the properties required for the edge of the cutting tool and for the portion remote from the edge. In the present disclosure, by providing a titanium compound layer and a second alumina layer further on the first alumina layer, the properties required for the edge of the cutting tool and the part away from the edge are successfully achieved.
  • the thickness of the first alumina layer is preferably greater than the thickness of the second alumina layer.
  • the thickness of the titanium compound layer is preferably 1 ⁇ m or more and 11 ⁇ m or less. By defining in this way, wear resistance is further improved.
  • the thickness of the second alumina layer is preferably 0.2 ⁇ m or more and 6.5 ⁇ m or less.
  • the thickness of the first alumina layer is preferably 2.5 ⁇ m or more and 20.5 ⁇ m or less. By defining in this way, it becomes a cutting tool excellent in wear resistance.
  • the interface region of the first alumina layer includes an interface S with the titanium compound layer and a virtual plane A parallel to the interface S passing through a point 0.5 ⁇ m away from the interface S in the thickness direction. It is preferable that the region is sandwiched between. By defining in this way, a cutting tool having excellent chipping resistance can be obtained.
  • the nitrogen content in the interface region of the first alumina layer is preferably 0.5 atomic % or more and 10 atomic % or less.
  • the thickness of the second alumina layer is 0.2 ⁇ m or more and 6.5 ⁇ m or less, and the residual stress of the titanium compound layer is -3 GPa or more and 0 GPa or less.
  • the bottom layer of the multilayer structure layer is preferably the second unit layer.
  • the titanium compound layer preferably further includes a layer of titanium nitride or titanium carbide. By defining in this way, it becomes a cutting tool excellent in wear resistance.
  • this embodiment An embodiment of the present disclosure (hereinafter referred to as "this embodiment") will be described below. However, this embodiment is not limited to this.
  • a notation of the form "X to Z” means the upper and lower limits of a range (that is, X to Z or less), and when no unit is described for X and only a unit is described for Z, then X and the unit of Z are the same.
  • the chemical formula when a compound is represented by a chemical formula in which the composition ratio of constituent elements is not limited, such as "TiC", the chemical formula can be any conventionally known composition ratio (element ratio) shall include At this time, the above chemical formula includes not only stoichiometric compositions but also non-stoichiometric compositions.
  • the chemical formula of “TiC” includes not only the stoichiometric composition “Ti 1 C 1 ” but also non-stoichiometric compositions such as “Ti 1 C 0.8 ”. This also applies to the description of compounds other than "TiC".
  • the cutting tool according to the present disclosure is A cutting tool comprising a substrate and a coating provided on the substrate, The coating is a first alumina layer provided on the substrate; A titanium compound layer provided immediately above the first alumina layer; a second alumina layer provided immediately above the titanium compound layer, A portion of the first alumina layer adjacent to the titanium compound layer forms an interface region, A portion of the first alumina layer that is not the interface region forms a non-interface region, The content of nitrogen in the interface region is 0.2 atomic % or more and 12 atomic % or less, The content of nitrogen in the non-interface region is 0 atomic % or more and 0.15 atomic % or less,
  • the titanium compound layer includes a multilayer structure layer adjacent to the first alumina layer, The multilayer structure layer consists of a first unit layer and a second unit layer, In the multilayer structure layer, the first unit layers and the second unit layers are alternately laminated, The first unit layer is made of titanium carbonitride, The second unit layer
  • a cutting tool 50 of the present embodiment includes a base material 10 and a coating 40 provided on the base material 10 (hereinafter sometimes simply referred to as "cutting tool") (Fig. 2).
  • the coating 40 includes a first alumina layer 20 provided on the base material 10, a titanium compound layer 21 provided directly above the first alumina layer 20, and a titanium compound layer 21 provided directly above the titanium compound layer 21. and a second alumina layer 22 provided.
  • the cutting tool 50 may further include an underlying layer 23 provided between the substrate 10 and the first alumina layer 20 (FIG. 3), in addition to the layers described above.
  • the cutting tool 50 may further include a surface layer provided on the second alumina layer 22 . Other layers such as the underlying layer 23 and the surface layer will be described later.
  • a cutting tool (hereinafter sometimes simply referred to as "cutting tool") 50 of the present embodiment includes a base material 10 and a coating 40 covering the base material 10 (see FIGS. 2 and 3).
  • the coating may cover the rake face of the substrate, or may cover a portion other than the rake face (for example, the flank face).
  • the cutting tools include drills, end mills, indexable cutting inserts for drills, indexable cutting inserts for end mills, indexable cutting inserts for milling, indexable cutting inserts for turning, metal saws, and gear cutting tools. , reamers, taps, and the like.
  • the base material is a cemented carbide (for example, a tungsten carbide (WC)-based cemented carbide, a cemented carbide containing Co in addition to WC, a carbonitride such as Cr, Ti, Ta, Nb in addition to WC).
  • WC tungsten carbide
  • a cemented carbide containing Co in addition to WC a cemented carbide containing Co in addition to WC
  • carbonitride such as Cr, Ti, Ta, Nb in addition to WC.
  • cemented carbide, etc. cermet (mainly composed of TiC, TiN, TiCN, etc.), high-speed steel, ceramics (titanium carbide, silicon carbide, silicon nitride, aluminum nitride, aluminum oxide, etc.), cubic It preferably contains at least one selected from the group consisting of type boron nitride sintered bodies (cBN sintered bodies) and diamond sintered bodies, and at least one selected from the group consisting of cemented carbide, cermet and cBN sintered bodies It is more preferred to contain seeds.
  • cBN sintered bodies type boron nitride sintered bodies
  • diamond sintered bodies at least one selected from the group consisting of cemented carbide, cermet and cBN sintered bodies It is more preferred to contain seeds.
  • these various base materials it is particularly preferable to select a WC-based cemented carbide or a cBN sintered body.
  • the reason for this is that these base materials have an excellent balance of hardness and strength, particularly at high temperatures, and have excellent properties as base materials for cutting tools for the above applications.
  • the effect of the present embodiment is exhibited even if such a cemented carbide contains free carbon or an abnormal phase called ⁇ phase in the structure.
  • the base material used in this embodiment may have a modified surface.
  • a ⁇ -free layer may be formed on the surface, or in the case of a cBN sintered body, a surface-hardened layer may be formed. Even if the surface is modified in this way, The effect of this embodiment is shown.
  • FIG. 1 is a perspective view illustrating one aspect of the substrate of the cutting tool.
  • a base material having such a shape is used, for example, as a base material for an indexable cutting insert for turning.
  • the base material 10 has a rake face 1, a flank face 2, and a cutting edge ridge line portion 3 where the rake face 1 and the flank face 2 intersect. That is, the rake face 1 and the flank face 2 are surfaces connected with the cutting edge ridge 3 interposed therebetween.
  • the cutting edge ridge 3 constitutes the tip of the cutting edge of the substrate 10 .
  • Such a shape of the base material 10 can also be grasped as the shape of the cutting tool.
  • the substrate 10 may or may not have a chip breaker.
  • the shape of the cutting edge ridge line 3 is a sharp edge (a ridge where the rake face and the flank face intersect), a honing (a shape in which the sharp edge is rounded), a negative land (a shape in which the sharp edge is chamfered), and a combination of honing and negative land. any shape is included.
  • the cutting tool has a rake face, a flank face, and a cutting edge ridge connecting the rake face and the flank face.
  • the coating 40 includes the first alumina layer 20 provided on the base material 10, the titanium compound layer 21 provided directly above the first alumina layer 20, and the titanium compound layer and a second alumina layer 22, which is provided immediately above 21 (see FIG. 2).
  • the "coating” is a coating that covers at least a part of the base material (for example, the rake face that comes into contact with the work material during cutting), thereby improving the chipping resistance, wear resistance, adhesion resistance, etc. of the cutting tool. It has the effect of improving the characteristics. It is preferable that the film covers not only a part of the base material but also the entire surface of the base material. However, it does not depart from the scope of the present embodiment even if a part of the substrate is not covered with the coating or the composition of the coating is partially different.
  • the thickness of the coating is preferably 10 ⁇ m or more and 40 ⁇ m or less, more preferably 15 ⁇ m or more and 35 ⁇ m or less.
  • the thickness of the coating means the total thickness of each layer constituting the coating.
  • the "coating layer” include a first alumina layer, a titanium compound layer, a second alumina layer, an underlying layer, a surface layer, and the like, which will be described later.
  • the thickness of the coating is, for example, using a field emission scanning electron microscope (SEM), measuring arbitrary 10 points in a cross-sectional sample parallel to the normal direction of the surface of the substrate, and measuring 10 points It can be obtained by averaging the thickness.
  • SEM field emission scanning electron microscope
  • the measurement cross section of the cross section sample is polished by ion milling.
  • Examples of field emission scanning electron microscopes include SU3500 (trade name) manufactured by Hitachi High-Tech Corporation.
  • IM4000 trade name manufactured by Hitachi High-Tech Co., Ltd. can be used.
  • the first alumina layer 20 in this embodiment is provided on the substrate 10 described above.
  • “provided on the base material” is not limited to the aspect of being provided directly on the base material (see FIG. 2), but is provided on the base material via another layer Aspects (see FIG. 3) are also included. That is, the first alumina layer may be provided directly above the base material as long as the effect of the present disclosure is exhibited, or may be provided on the base material via another layer such as a base layer to be described later. may be provided.
  • the first alumina layer may be composed only of aluminum oxide (Al 2 O 3 ), or may be composed of aluminum oxide and inevitable impurities. Examples of the inevitable impurities include chlorine and sulfur.
  • the aluminum oxide is preferably ⁇ -type aluminum oxide ( ⁇ -Al 2 O 3 ).
  • a portion of the first alumina layer adjacent to the titanium compound layer forms an interface region. Further, the portion of the first alumina layer that is not the interface region constitutes a non-interface region.
  • the interface region of the first alumina layer is sandwiched between an interface S with the titanium compound layer and a virtual plane A parallel to the interface S passing through a point 0.5 ⁇ m away from the interface S in the thickness direction. It is preferable that the region is a flat region (Fig. 4).
  • the non-interface region of the first alumina layer is preferably a region sandwiched between the virtual plane A and the interface Q of the first alumina layer on the substrate side (FIG. 4). A clear boundary may or may not exist between the interface region and the non-interface region in the first alumina layer.
  • the nitrogen content in the interface region of the first alumina layer is 0.2 at% or more and 12 at% or less, preferably 0.5 at% or more and 10 at% or less, and 1 at% or more and 9 at% or less. is more preferred.
  • the content ratio of nitrogen is the atomic ratio based on the total of aluminum, oxygen and nitrogen in the first alumina layer.
  • the first alumina layer having the structure described above nitrogen atoms are unevenly distributed in the interface region with the titanium compound layer. Therefore, nitrogen atoms are diffused from the interface region into the titanium compound layer, and adhesion between the first alumina layer and the titanium compound layer is improved.
  • the titanium compound layer provided on the alumina layer was required only to serve as a layer indicating the state of use, so the adhesion with the alumina layer and other mechanical properties were not regarded as important. Further, it has been conventionally known that the presence of nitrogen inside the alumina layer causes thermal instability and deteriorates the performance of the alumina layer. Therefore, conventionally, nitrogen was not positively added to the inside of the alumina layer.
  • the uneven distribution of nitrogen atoms in the interface region of the first alumina layer improves the adhesion with the titanium compound layer (especially the multilayer structure layer adjacent to the first alumina layer), and furthermore, the titanium compound layer has a predetermined of mechanical properties can be attached.
  • the nitrogen content can be determined by performing line analysis on a cross-sectional sample parallel to the normal direction of the surface of the base material described above by Auger electron spectroscopy (AES method). Specifically, first, the cut surface of the cross-sectional sample is polished by cross-section polisher processing (CP processing) or the like. Cross-sectional SEM of the substrate (underlying layer if provided), the first alumina layer and the titanium compound layer by analysis using a field emission scanning microscope (FE-SEM) on the polished cut surface. get the image. The measurement magnification at this time is 50000 times. At this time, the substrate, underlayer, and titanium compound layer are observed as dark regions, and the first alumina layer is observed as a bright region.
  • AES method Auger electron spectroscopy
  • the distance from the measurement start point is plotted on the X axis (horizontal axis), and the atomic ratio (at%) of each element to be measured is plotted on the Y axis (vertical axis).
  • the point at which the atomic ratio of aluminum is 10 at % and which is closer to the titanium compound layer is defined as the "interface S between the first alumina layer and the titanium compound layer" (see FIG. 4).
  • a plane including a point 0.5 ⁇ m away from the interface S on the side of the first alumina layer is defined as a “virtual plane A” (see FIG. 4).
  • the average value of the atomic ratio of nitrogen in the region (interface region) sandwiched between the interface S and the imaginary plane A is obtained.
  • the measurement as described above is performed at least three times, and the average value of the values obtained in each measurement is taken as the nitrogen content in the interface region of the first alumina layer.
  • the nitrogen content in the non-interface region of the first alumina layer is 0 atomic % or more and 0.15 atomic % or less, preferably 0 atomic % or more and 0.1 atomic % or less.
  • the content of nitrogen in the non-interface region can be obtained by performing line analysis on a cross-sectional sample by the AES method, as described above. At this time, in the graph obtained based on the results of the line analysis, the point at which the atomic ratio of aluminum is 10 at% and the point closer to the substrate is "the interface Q on the substrate side of the first alumina layer". (see FIG. 4).
  • the average atomic ratio of nitrogen in the region (non-interface region) sandwiched between the virtual plane A and the interface Q is obtained.
  • the measurement as described above is performed at least three times, and the average value of the values obtained in each measurement is taken as the nitrogen content in the non-interface region of the first alumina layer.
  • the thickness of the first alumina layer is preferably 2.5 ⁇ m or more and 20.5 ⁇ m or less, more preferably 3 ⁇ m or more and 20 ⁇ m or less, and more preferably 6 ⁇ m or more and 17 ⁇ m or less.
  • the thickness of the first alumina layer can be confirmed by observing vertical cross sections of the substrate and the coating using SEM in the same manner as described above.
  • the thickness of the first alumina layer is preferably greater than the thickness of the second alumina layer described later.
  • the titanium compound layer 21 is provided directly above the first alumina layer 20 (FIG. 2).
  • the titanium compound layer includes a multilayer structure layer adjacent to the first alumina layer.
  • the multilayer structure layer is provided directly above the first alumina layer.
  • the titanium compound layer may be composed only of a multilayer structure layer adjacent to the first alumina layer, or composed of a multilayer structure layer adjacent to the first alumina layer and another titanium compound layer.
  • the thickness of the titanium compound layer is preferably 1 ⁇ m or more and 11 ⁇ m or less, more preferably 1.5 ⁇ m or more and 9.5 ⁇ m or less, and even more preferably 2.5 ⁇ m or more and 8.5 ⁇ m or less.
  • the thickness of the titanium compound layer is thinner than before. However, since the titanium compound layer has a predetermined residual stress as described later, the layer has sufficient hardness. The thickness of the titanium compound layer can be confirmed by observing vertical cross sections of the substrate and the coating using SEM in the same manner as described above.
  • the multilayer structure layer 24 consists of a first unit layer 24a and a second unit layer 24b (Fig. 2).
  • the first unit layers and the second unit layers are alternately laminated.
  • the bottom layer of the multilayer structure layer is preferably the second unit layer.
  • the uppermost layer of the multilayer structure layer may be the first unit layer or the second unit layer.
  • the “lowermost layer” means the layer closest to the substrate among the layers constituting the multilayer structure layer.
  • the “uppermost layer” means the layer farthest from the substrate among the layers constituting the multilayer structure layer.
  • the thickness of the multilayer structure layer is preferably 1 ⁇ m or more and 11 ⁇ m or less, more preferably 1.5 ⁇ m or more and 9.5 ⁇ m or less, and even more preferably 3.0 ⁇ m or more and 8.0 ⁇ m or less.
  • the thickness of the multilayer structure layer can be confirmed by observing vertical cross sections of the base material and the coating using SEM in the same manner as described above.
  • the first unit layer is made of titanium carbonitride (TiCN).
  • the first unit layer may be composed only of titanium carbonitride, or may be composed of titanium carbonitride and inevitable impurities. Examples of the inevitable impurities include oxygen and chlorine.
  • the thickness of the first unit layer is preferably 50 nm or more and 2000 nm or less, more preferably 100 nm or more and 1000 nm or less, and even more preferably 300 nm or more and 700 nm or less.
  • the thickness of the first unit layer can be confirmed by observing vertical cross sections of the substrate and the coating using SEM in the same manner as described above. The magnification at this time is, for example, 20000 times.
  • the thickness of each of the ten first unit layers is obtained by the method described above in the arbitrarily selected ten first unit layers. , the average value of the values obtained from the respective first unit layers is taken as the thickness of the first unit layer in the multilayer structure layer.
  • the second unit layer is made of titanium carbonitride (TiCNO).
  • the second unit layer may be composed of titanium carbonitride oxide only, or may be composed of titanium carbonitride oxide and inevitable impurities. Examples of the inevitable impurities include oxygen and chlorine.
  • the thickness of the second unit layer is preferably 50 nm or more and 2000 nm or less, more preferably 100 nm or more and 1000 nm or less, and even more preferably 300 nm or more and 700 nm or less.
  • the thickness of the second unit layer can be confirmed by observing vertical cross sections of the substrate and the coating using SEM in the same manner as described above. The magnification at this time is, for example, 20000 times.
  • the thickness of each of the ten second unit layers is obtained by the method described above in the arbitrarily selected ten second unit layers. , the average value of the values obtained from the respective second unit layers is taken as the thickness of the second unit layer in the multilayer structure layer.
  • the titanium compound layer preferably further includes a layer of titanium nitride (TiN) or titanium carbide (TiC).
  • the thickness of the titanium nitride or titanium carbide layer is preferably 0.5 ⁇ m or more and 5.5 ⁇ m or less, more preferably 0.5 ⁇ m or more and 2.5 ⁇ m or less.
  • the thickness of the titanium nitride or titanium carbide layer can be confirmed by observing vertical cross sections of the substrate and the coating using SEM in the same manner as described above.
  • the residual stress of the titanium compound layer is preferably -3 GPa or more and 0 GPa or less, more preferably -2.5 GPa or more and -0.5 GPa or less.
  • residual stress is a kind of internal stress (intrinsic strain) existing in the layer.
  • the residual stress is roughly classified into compressive residual stress and tensile residual stress.
  • Compressive residual stress refers to residual stress represented by a numerical value of "-" (minus) (in this specification, the unit is represented by "GPa”).
  • GPa the unit is represented by "compressive residual stress of 10 GPa”
  • the concept that the compressive residual stress is large indicates that the absolute value of the numerical value is large
  • the concept that the compressive residual stress is small indicates that the absolute value of the numerical value is small.
  • Tensile residual stress refers to residual stress represented by a "+” (plus) numerical value (in this specification, the unit is represented by "GPa”).
  • GPa the unit is represented by "GPa”
  • tensile residual stress of 10 GPa can be grasped as a residual stress of 10 GPa. Therefore, the concept that the tensile residual stress is large indicates that the numerical value is large, and the concept that the tensile residual stress is small indicates that the numerical value is small.
  • the residual stress of the titanium compound layer is obtained by residual stress measurement by the 2 ⁇ -sin 2 ⁇ method using X-rays.
  • the crystal plane spacing of the (331) plane which is the diffraction plane of titanium carbonitride
  • the diffraction angle at the time of measurement designates the diffraction angle according to the crystal plane of the object to be measured.
  • the measurement field of view mentioned above means "the measurement field of view on the surface of the titanium compound layer”.
  • the residual stress in the entire measurement field is calculated. Such measurements are performed in a plurality of measurement fields, and the average value of the residual stress obtained in each measurement field is defined as "residual stress of the titanium compound layer".
  • the second alumina layer 22 in this embodiment is provided directly above the titanium compound layer 21 .
  • the second alumina layer may be provided with another layer such as a surface layer thereon.
  • the second alumina layer may be the outermost surface of the coating.
  • the second alumina layer may be composed only of aluminum oxide (Al 2 O 3 ), or may be composed of aluminum oxide and inevitable impurities. Examples of the inevitable impurities include chlorine and sulfur.
  • the aluminum oxide is preferably ⁇ -type aluminum oxide ( ⁇ -Al 2 O 3 ).
  • the second alumina layer may or may not have the same composition as the first alumina layer.
  • the thickness of the second alumina layer is preferably 0.2 ⁇ m or more and 6.5 ⁇ m or less, more preferably 0.5 ⁇ m or more and 5 ⁇ m or less, and even more preferably 1 ⁇ m or more and 4.5 ⁇ m or less.
  • the thickness of the second alumina layer is thinner than before.
  • the second alumina layer is thin, it is possible to apply a predetermined residual stress to the titanium compound layer by performing blasting after forming the second alumina layer, as described later.
  • the thickness of the second alumina layer can be confirmed by observing vertical cross-sections of the substrate and coating using SEM in the same manner as described above.
  • the thickness of the second alumina layer is 0.2 ⁇ m or more and 6.5 ⁇ m or less, and the residual stress of the titanium compound layer is ⁇ 3 GPa or more and 0 GPa or less.
  • a portion of the second alumina layer adjacent to the titanium compound layer forms an interface region, and the interface region may contain nitrogen.
  • the portion of the second alumina layer that is not the interface region constitutes a non-interface region.
  • the interface region of the second alumina layer is sandwiched between an interface R with the titanium compound layer and a virtual plane B parallel to the interface R passing through a point 0.5 ⁇ m away from the interface R in the thickness direction. It is preferable that the area is
  • the nitrogen content in the interface region of the second alumina layer is preferably 0.5 at % or more and 10 at % or less. By doing so, it is possible to provide a cutting tool having excellent adhesion between the second alumina layer and the titanium compound layer.
  • the content of nitrogen in the non-interface region of the second alumina layer is preferably 0 at % or more and 0.15 at % or less.
  • the nitrogen content in the interfacial region or the non-interfacial region of the second alumina layer can be obtained by performing line analysis on a cross-sectional sample by the AES method according to the method described above.
  • the coating 40 further includes an underlying layer 23 provided between the substrate 10 and the first alumina layer 20 (see FIG. 3).
  • the underlayer 23 preferably contains titanium nitride (TiN), titanium carbonitride (TiCN), or titanium carbonitride (TiCNO).
  • TiN titanium nitride
  • TiCN titanium carbonitride
  • TiCNO titanium carbonitride
  • the thickness of the underlayer is preferably 3 ⁇ m or more and 20 ⁇ m or less, more preferably 5 ⁇ m or more and 15 ⁇ m or less. Such a thickness can be confirmed by observing vertical cross sections of the substrate and the coating using SEM in the same manner as described above.
  • the coating further includes a surface layer provided on the second alumina layer.
  • the surface layer preferably contains a compound composed of titanium and at least one element selected from the group consisting of C, N and B.
  • Compounds contained in the surface include, for example, TiC, TiN, TiCN and TiB2 .
  • the thickness of the surface layer is preferably 0.2 ⁇ m or more and 3 ⁇ m or less, more preferably 0.5 ⁇ m or more and 1.5 ⁇ m or less. Such a thickness can be confirmed by observing vertical cross sections of the substrate and the coating using SEM in the same manner as described above.
  • the coating may further include other layers as long as the effects of the cutting tool according to the present embodiment are not impaired.
  • the composition of the other layer may be different from or the same as that of the first alumina layer, the titanium compound layer, the second alumina layer, the base layer or the surface layer. Examples of compounds contained in other layers include TiN, TiCN, TiBN and Al 2 O 3 .
  • the order of lamination of the other layers is not particularly limited.
  • the thickness of the other layer is not particularly limited as long as the effect of the present embodiment is not impaired.
  • the method for manufacturing a cutting tool includes: A first step of preparing the base material (hereinafter sometimes simply referred to as "first step”); a second step of forming the first alumina layer on the substrate by chemical vapor deposition (hereinafter sometimes simply referred to as “second step”); a third step of forming the titanium compound layer directly on the first alumina layer by chemical vapor deposition (hereinafter sometimes simply referred to as the “third step”); a fourth step of forming the second alumina layer directly on the titanium compound layer by chemical vapor deposition (hereinafter sometimes simply referred to as the "fourth step”); including At the end of the second step, the first alumina layer is formed using a raw material gas containing a gas containing aluminum as a constituent element, a gas containing nitrogen as a constituent element, and a gas containing oxygen as a constituent element, In the third step, a multilayer structure layer is formed directly on the first alumina layer.
  • first step A first step of preparing the base material
  • a substrate is prepared in the first step.
  • a cemented carbide substrate is prepared as the substrate.
  • the cemented carbide substrate may be a commercially available product or may be produced by a general powder metallurgy method.
  • a mixed powder is obtained by mixing WC powder and Co powder with a ball mill or the like. After drying the mixed powder, it is molded into a predetermined shape to obtain a molded body. Further, by sintering the molded body, a WC—Co-based cemented carbide (sintered body) is obtained.
  • the sintered body is subjected to a predetermined cutting edge processing such as honing treatment to produce a base material made of a WC—Co based cemented carbide.
  • a predetermined cutting edge processing such as honing treatment to produce a base material made of a WC—Co based cemented carbide.
  • any substrate other than those described above can be prepared as long as it is a conventionally known substrate of this type.
  • ⁇ Second step step of forming the first alumina layer on the substrate>
  • a first alumina layer is formed on the substrate by chemical vapor deposition (CVD).
  • the first alumina layer is formed using a source gas containing a gas containing aluminum as a constituent element, a gas containing nitrogen as a constituent element, and a gas containing oxygen as a constituent element.
  • FIG. 5 is a schematic cross-sectional view showing an example of a chemical vapor deposition apparatus (CVD apparatus) used for manufacturing a film.
  • the second step will be described below with reference to FIG.
  • the CVD apparatus 30 includes a plurality of substrate setting jigs 31 for holding the substrate 10 and a reaction vessel 32 made of heat-resistant alloy steel covering the substrate setting jigs 31 .
  • a temperature control device 33 for controlling the temperature inside the reaction vessel 32 is provided around the reaction vessel 32 .
  • a gas introduction pipe 35 having a gas introduction port 34 is provided in the reaction vessel 32 .
  • the gas introduction pipe 35 extends in the vertical direction and is rotatable about the vertical direction in the inner space of the reaction vessel 32 in which the substrate setting jig 31 is arranged. Further, the gas introduction pipe 35 is provided with a plurality of ejection holes 36 for ejecting the gas into the reaction vessel 32 .
  • the first alumina layer and the like constituting the coating can be formed in the following manner.
  • the substrate 10 is placed on the substrate setting jig 31, and while the temperature and pressure in the reaction vessel 32 are controlled within a predetermined range, the material gas for the first alumina layer is introduced from the gas introduction pipe 35 into the reaction vessel. 32. Thereby, the first alumina layer 20 is formed on the substrate 10 .
  • the raw material gas for the underlayer is introduced into the reaction vessel 32 from the gas introduction pipe 35, so that the base material 10 It is preferable to form an underlayer (for example, a layer containing TiN) on the surface of the .
  • an underlayer for example, a layer containing TiN
  • the raw material gas for the underlayer is not particularly limited, but in the case of forming a TiN layer, for example, a mixed gas of TiCl 4 and N 2 can be used.
  • the raw material gas includes, for example, a mixed gas of TiCl 4 , N 2 , CH 3 CN, CH 4 and C 2 H 4 .
  • the raw material gas includes, for example, a mixed gas of TiCl 4 , N 2 , CO, and CH 4 .
  • the temperature inside the reaction vessel 32 when forming the underlayer is preferably controlled to 1000 to 1100.degree.
  • the pressure inside the reaction vessel 32 during the formation of the underlayer is preferably controlled to 0.1 to 1013 hPa.
  • H 2 is preferably used as the carrier gas.
  • the gas introduction pipe 35 is rotated by a drive unit (not shown) when the gas is introduced. Thereby, each gas can be uniformly dispersed in the reaction vessel 32 .
  • the underlayer may be formed by the MT (Medium Temperature)-CVD method.
  • the temperature inside the reaction vessel 32 is set to a relatively low temperature of 850 to 950° C., unlike the CVD method (hereinafter also referred to as “HT-CVD method”) which is performed at a temperature of 1000 to 1100° C. It is a method of forming a layer while maintaining the temperature. Since the MT-CVD method is performed at a relatively low temperature compared to the HT-CVD method, damage to the substrate 10 due to heating can be reduced.
  • the underlying layer is a TiN layer, it is preferably formed by the MT-CVD method.
  • a mixed gas of AlCl 3 , CO, CO 2 and HCl is used as the source gas in the nucleation step.
  • a mixed gas of AlCl 3 , CO, CO 2 , HCl and H 2 S is used as the raw material gas in the crystal growth stage.
  • a mixed gas of AlCl 3 (a gas containing aluminum as a constituent element), CO, CO 2 , HCl and N 2 (a gas containing nitrogen as a constituent element) is used as the raw material gas used at the end of the second step, for example.
  • the content of AlCl 3 in the source gas is preferably 1 to 5% by volume, more preferably 1.5 to 4% by volume, and even more preferably 2 to 3.5% by volume.
  • a preferred flow rate for AlCl 3 is 0.5-3.5 L/min.
  • the content of CO in the source gas is preferably 0.5 to 4% by volume, more preferably 0.8 to 3.5% by volume, and 1 to 2.5% by volume. More preferred.
  • a preferred flow rate for CO is 0.5 to 2 L/min.
  • the content of CO 2 in the raw material gas is preferably 0.2 to 2.5% by volume, more preferably 0.3 to 2% by volume, and 0.5 to 1.5% by volume. It is even more preferable to have A preferred flow rate for CO 2 is 0.4-1.5 L/min.
  • the content of HCl in the source gas is preferably 1 to 6% by volume, more preferably 1.5 to 5.5% by volume, and even more preferably 2 to 4.5% by volume. .
  • a preferred flow rate for HCl is 0.5 to 4.5 L/min.
  • the content of H 2 S in the source gas is preferably 0.5 to 3.5% by volume, more preferably 1.0 to 3.0% by volume, and 1.5 to 2.5% by volume. % by volume is more preferred.
  • a preferred flow rate for H 2 S is 0.3-2.5 L/min.
  • the content of N 2 in the source gas is preferably 0.1 to 1% by volume, more preferably 0.2 to 0.8% by volume, and more preferably 0.3 to 0.6% by volume. It is even more preferable to have A preferred flow rate of N 2 is 0.1-0.5 L/min.
  • the temperature inside the reaction vessel 32 is preferably controlled at 950-1000.degree.
  • the pressure inside the reaction vessel 32 is preferably controlled at 50-100 hPa.
  • H 2 can be used as the carrier gas. It should be noted that the fact that the gas introduction pipe 35 is preferably rotated during gas introduction is the same as described above.
  • the mode of each layer changes by controlling each condition of the CVD method.
  • the composition of each layer is determined by the composition of the raw material gas introduced into the reaction vessel 32 .
  • the thickness of each layer is controlled by the execution time (deposition time).
  • ⁇ Third step Step of forming a titanium compound layer directly on the first alumina layer>
  • the titanium compound layer is formed directly on the first alumina layer by chemical vapor deposition.
  • a multilayer structure layer is formed directly on the first alumina layer. The multilayer structure layer is formed by alternately laminating the first unit layer and the second unit layer.
  • the material gas for the first unit layer for example, a mixed gas of TiCl 4 , CH 4 and N 2 is used.
  • the content of TiCl 4 in the source gas is preferably 2 to 7% by volume, more preferably 3 to 6% by volume, and even more preferably 4 to 5% by volume.
  • a preferred flow rate for TiCl 4 is 1.5-5.0 L/min.
  • the content of CH 4 in the source gas is preferably 2 to 7% by volume, more preferably 2.5 to 6.5% by volume, even more preferably 3 to 6% by volume.
  • a preferred flow rate for CH 4 is 1.5-5.0 L/min.
  • the content of N 2 in the source gas is preferably 5 to 40% by volume, more preferably 7 to 35% by volume, even more preferably 10 to 25% by volume.
  • a preferred flow rate for N 2 is 4-28 L/min.
  • the temperature inside the reaction vessel 32 is preferably controlled at 950-1005°C.
  • the pressure inside the reaction vessel 32 is preferably controlled at 50-200 hPa.
  • H 2 can be used as the carrier gas. It should be noted that the fact that the gas introduction pipe 35 is preferably rotated during gas introduction is the same as described above.
  • a mixed gas of TiCl 4 , CH 4 , N 2 and CO, for example, is used as the raw material gas for the second unit layer.
  • the content of TiCl 4 in the raw material gas is preferably 1.5 to 4.5% by volume, more preferably 2.0 to 4.0% by volume, and 2.5 to 3.5% by volume. % is more preferred.
  • a preferred flow rate for TiCl 4 is 0.8-2.3 L/min.
  • the content of CH 4 in the raw material gas is preferably 0.5 to 3.5% by volume, more preferably 1.0 to 3.0% by volume, and 1.5 to 2.5% by volume. % is more preferred.
  • a preferred flow rate for CH 4 is 0.3-1.8 L/min.
  • the content of N 2 in the source gas is preferably 15 to 45% by volume, more preferably 20 to 40% by volume, even more preferably 25 to 35% by volume.
  • a preferred flow rate for N 2 is 7.5-22.5 L/min.
  • the content of CO in the source gas is preferably 1.5 to 4.5% by volume, more preferably 2.0 to 4.0% by volume, and 2.5 to 3.5% by volume. is more preferable.
  • a preferred flow rate for CO is 0.8 to 2.3 L/min.
  • the temperature inside the reaction vessel 32 is preferably controlled at 950-1005°C.
  • the pressure inside the reaction vessel 32 is preferably controlled at 100-300 hPa.
  • H 2 can be used as the carrier gas. It should be noted that the fact that the gas introduction pipe 35 is preferably rotated during gas introduction is the same as described above.
  • a layer of titanium nitride, titanium carbide, titanium carbonitride oxide, or the like may be formed as a layer constituting the titanium compound layer.
  • ⁇ Fourth step Step of forming a second alumina layer directly on the titanium compound layer>
  • a second alumina layer is formed directly on the titanium compound layer by chemical vapor deposition.
  • a mixed gas of AlCl 3 , CO, CO 2 , H 2 S, HCl and TiCl 4 is used as the source gas, for example.
  • the content of AlCl 3 in the source gas is preferably 1 to 5% by volume, more preferably 1.5 to 4% by volume, and even more preferably 2 to 3.5% by volume.
  • a preferred flow rate for AlCl 3 is 0.5-3.5 L/min.
  • the content of CO in the source gas is preferably 0.5 to 4% by volume, more preferably 0.8 to 3.5% by volume, and 1 to 2.5% by volume. More preferred.
  • a preferred flow rate for CO is 0.3 to 3 L/min.
  • the content of CO 2 in the raw material gas is preferably 0.2 to 2.5% by volume, more preferably 0.3 to 2% by volume, and 0.5 to 1.5% by volume. It is even more preferable to have A preferred flow rate for CO 2 is 0.1-1.5 L/min.
  • the content of H 2 S in the source gas is preferably 0.2 to 2.5% by volume, more preferably 0.3 to 2.0% by volume, and more preferably 0.5 to 1.5% by volume. % by volume is more preferred.
  • a preferred flow rate for H 2 S is 0.1-1.5 L/min.
  • the content of HCl in the source gas is preferably 1 to 7% by volume, more preferably 1.5 to 6.5% by volume, and even more preferably 2 to 6% by volume.
  • a preferred flow rate for HCl is 0.5 to 4.5 L/min, and a more preferred flow rate is 1 to 4 L/min.
  • the content of TiCl 4 in the source gas is preferably 0.01 to 0.09% by volume, more preferably 0.02 to 0.08% by volume, and 0.03 to 0.07% by volume. % is more preferred.
  • a preferred flow rate for TiCl 4 is 0.05-0.6 L/min.
  • the temperature inside the reaction vessel 32 is preferably controlled at 950-1000.degree.
  • the pressure inside the reaction vessel 32 is preferably controlled at 50-200 hPa.
  • H 2 can be used as the carrier gas. It should be noted that the fact that the gas introduction pipe 35 is preferably rotated during gas introduction is the same as described above.
  • the second An alumina layer may be formed. By doing so, it is possible to provide a cutting tool having excellent adhesion between the second alumina layer and the titanium compound layer.
  • the source gas for example, a mixed gas of AlCl 3 , CO, CO 2 , H 2 S, HCl, TiCl 4 and N 2 is used.
  • the content ratios of AlCl 3 , CO, CO 2 , H 2 S, HCl and TiCl 4 in the source gas are preferably within the ranges described above.
  • the content of N 2 in the source gas is preferably 0.1 to 1% by volume, more preferably 0.2 to 0.8% by volume, and more preferably 0.3 to 0.6% by volume. It is even more preferable to have A preferred flow rate of N 2 is 0.1-0.5 L/min, a more preferred flow rate is 0.2-0.4 L/min.
  • additional steps may be performed as appropriate within a range that does not impair the effects of the present embodiment.
  • additional step include a step of forming a surface layer on the second alumina layer and a step of subjecting the coating to blasting.
  • the thickness of the second alumina layer directly on the titanium compound layer is less than the thickness of the first alumina layer. Therefore, when the blasting process is performed after the fourth step, a predetermined compressive residual stress can be applied to the titanium compound layer.
  • Conditions for the blasting include, for example, the conditions described in Examples described later.
  • the method of forming the surface layer is not particularly limited, and examples thereof include a method of forming by a CVD method or the like.
  • a base layer was formed on the prepared base material under the raw material gas composition and film formation conditions shown in Table 1 using a CVD apparatus.
  • the film formation time was appropriately adjusted so that the thicknesses shown in Table 5 were obtained.
  • Table 5 shows the thickness of the underlayer and the composition of the underlayer.
  • the composition of the underlayer is listed in order of proximity to the substrate.
  • the notation “TiN (1.0)/TiCN (10.5)/TiCNO (1.5)” is a layer of TiN (thickness 1.0 ⁇ m), a layer of TiCN in order from the layer closest to the substrate. This means that a layer (10.5 ⁇ m thick) and a layer of TiCNO (1.5 ⁇ m thick) are formed.
  • ⁇ Second step step of forming the first alumina layer on the substrate>
  • a CVD apparatus was used to form a first alumina layer on the prepared base material or the base material on which the underlying layer was formed, and the process was shifted to the third step, which is a post-process.
  • Table 2 shows the conditions for forming the first alumina layer. As shown in Table 2, the composition of the raw material gas was changed according to each stage of "nucleation" (early stage), "crystal growth” (middle stage), and "N-containing layer formation” (final stage). An alumina layer was deposited.
  • the first alumina layer was formed in two stages of “nucleation” (initial stage) and “crystal growth” (middle stage) without using the source gas in "N-containing layer formation” (final stage). filmed.
  • the film formation time was appropriately adjusted so that the thicknesses shown in Table 5 were obtained.
  • Table 5 shows the thickness of the first alumina layer and the composition of the first alumina layer.
  • ⁇ Third step Step of forming a titanium compound layer directly on the first alumina layer>
  • a titanium compound layer was formed directly above the first alumina layer on the substrate on which the first alumina layer was formed.
  • a multilayer structure layer was formed directly above the first alumina layer.
  • the multi-layer structure layer was formed by alternately laminating the first unit layer (titanium carbonitride layer) and the second unit layer (titanium carbonitride layer).
  • Table 3 shows the conditions for forming the titanium compound layer. The film formation time was appropriately adjusted so that the thicknesses shown in Table 5 were obtained.
  • Table 5 shows the thickness of the titanium compound layer and the composition of the titanium compound layer.
  • compositions of the titanium compound layers are listed in order from the first alumina layer.
  • the notation "ML (8.0) / TiN (3.0)” is a multilayer structure layer (thickness 8.0 ⁇ m) and a TiN layer (thickness 3 .0 ⁇ m) is formed.
  • ⁇ Fourth step Step of forming a second alumina layer directly on the titanium compound layer>
  • a second alumina layer was formed directly on the titanium compound layer by using a CVD device on the substrate on which the titanium compound layer was formed.
  • Table 4 shows the conditions for forming the second alumina layer. The film formation time was appropriately adjusted so that the thicknesses shown in Table 5 were obtained.
  • Table 5 shows the thickness of the second alumina layer and the composition of the second alumina layer.
  • the thickness of each layer constituting the coating is determined using a field emission scanning electron microscope (SEM) (manufactured by Hitachi High-Tech Co., Ltd., product name: SU3500), and any cross-sectional sample parallel to the normal direction of the surface of the base material. was obtained by measuring 10 points and averaging the thickness of the measured 10 points. At this time, the measurement cross section of the above cross section sample was polished by ion milling treatment (trade name: IM4000, manufactured by Hitachi High-Tech Co., Ltd.) and then measured. Tables 5 and 6 show the results. Also, it was determined from the SEM image whether the bottom layer in the multilayer structure layer was the first unit layer or the second unit layer.
  • SEM field emission scanning electron microscope
  • ⁇ Nitrogen content in interface region and non-interface region of first alumina layer (AES measurement)> The atomic ratio of each element (oxygen, nitrogen, aluminum) in the interfacial region and non-interfacial region of the first alumina layer was determined by Auger electron spectroscopy ( It was obtained by line analysis by the AES method). Specifically, first, the cut surface of the cross-sectional sample was polished by cross-section polisher processing. Cross-sectional SEM images of the underlying layer, the first alumina layer and the titanium compound layer were obtained by analyzing the polished cut surface using a field emission scanning microscope (FE-SEM). The measurement magnification at this time was 50000 times.
  • FE-SEM field emission scanning microscope
  • a graph was created from the data obtained by the above line analysis.
  • the X-axis (horizontal axis) indicates the distance from the measurement start point
  • the Y-axis (vertical axis) indicates the atomic ratio (at %) of each element to be measured.
  • the point at which the atomic ratio of aluminum is 10 at % and which is closer to the titanium compound layer is defined as the "interface S between the first alumina layer and the titanium compound layer" (for example, FIG. 4).
  • a plane including a point 0.5 ⁇ m away from the interface S on the side of the first alumina layer was defined as a “virtual plane A” (see, for example, FIG. 4).
  • the point at which the atomic ratio of aluminum is 10 at % and which is closer to the substrate is defined as the "interface Q on the substrate side of the first alumina layer" (see FIG. 4).
  • the average value of the atomic ratio of nitrogen in the region (interface region) sandwiched between the interface S and the virtual plane A, and the region sandwiched between the virtual plane A and the interface Q (non-interface region ) were obtained respectively.
  • Such measurements were performed three times, and the average value of the values obtained in each measurement was calculated as the nitrogen content in the interface region of the first alumina layer, and the nitrogen content in the non-interface region of the first alumina layer. as a percentage.
  • Table 6 shows the results.
  • the cutting tools of Samples 1 to 13 had surface quality ranks A to C in cutting evaluation 2, and good results were obtained.
  • the cutting tools of Samples 102 and 103 were rank E in surface quality in cutting evaluation 2.
  • the cutting tool of sample 101 (the cutting tool of the comparative example) had a surface quality of rank C in cutting evaluation 2, but had a cutting time of 4.5 minutes in cutting evaluation 1, and had wear resistance and adhesion resistance. could not be reconciled.
  • Base material 20 First alumina layer 21 Titanium compound layer 22 Second alumina layer 23 Base layer 24 Multilayer structure layer 24a First unit layer 24b Second unit layer, 30 CVD device, 31 substrate setting jig, 32 reaction vessel, 33 temperature control device, 34 gas introduction port, 35 gas introduction pipe, 36 ejection hole, 40 coating, 50 cutting tool, A first alumina Virtual plane A including a point 0.5 ⁇ m away from the interface S between the layer and the titanium compound layer to the first alumina layer side, R: Interface Q, S on the substrate side of the first alumina layer, S: The first alumina layer and the titanium compound Interface S with layer

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  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
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EP21940857.2A EP4144466B1 (en) 2021-05-21 2021-05-21 Cutting tool
PCT/JP2021/019381 WO2022244243A1 (ja) 2021-05-21 2021-05-21 切削工具
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US12202051B2 (en) 2023-06-22 2025-01-21 Sumitomo Electric Hardmetal Corp. Cutting tool
US12226836B2 (en) 2023-06-22 2025-02-18 Sumitomo Electric Hardmetal Corp. Cutting tool
US12404589B1 (en) 2024-03-01 2025-09-02 Sumitomo Electric Hardmetal Corp. Cutting tool

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WO2026022969A1 (ja) * 2024-07-24 2026-01-29 住友電工ハードメタル株式会社 切削工具

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US12202051B2 (en) 2023-06-22 2025-01-21 Sumitomo Electric Hardmetal Corp. Cutting tool
US12226836B2 (en) 2023-06-22 2025-02-18 Sumitomo Electric Hardmetal Corp. Cutting tool
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US12404589B1 (en) 2024-03-01 2025-09-02 Sumitomo Electric Hardmetal Corp. Cutting tool
WO2025182085A1 (ja) 2024-03-01 2025-09-04 住友電工ハードメタル株式会社 切削工具

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