WO2017037798A1 - 表面被覆切削工具およびその製造方法 - Google Patents
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- WO2017037798A1 WO2017037798A1 PCT/JP2015/074507 JP2015074507W WO2017037798A1 WO 2017037798 A1 WO2017037798 A1 WO 2017037798A1 JP 2015074507 W JP2015074507 W JP 2015074507W WO 2017037798 A1 WO2017037798 A1 WO 2017037798A1
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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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23C—MILLING
- B23C5/00—Milling-cutters
- B23C5/16—Milling-cutters characterised by physical features other than shape
- B23C5/20—Milling-cutters characterised by physical features other than shape with removable cutter bits or teeth or cutting inserts
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
-
- 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
- C23C16/029—Graded interfaces
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/44—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 method of coating
- C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B2224/00—Materials of tools or workpieces composed of a compound including a metal
- B23B2224/04—Aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B2224/00—Materials of tools or workpieces composed of a compound including a metal
- B23B2224/28—Titanium carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B2224/00—Materials of tools or workpieces composed of a compound including a metal
- B23B2224/36—Titanium nitride
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- 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
- B23B2228/04—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner applied by chemical vapour deposition [CVD]
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23C—MILLING
- B23C2224/00—Materials of tools or workpieces composed of a compound including a metal
- B23C2224/04—Aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23C—MILLING
- B23C2224/00—Materials of tools or workpieces composed of a compound including a metal
- B23C2224/28—Titanium carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23C—MILLING
- B23C2224/00—Materials of tools or workpieces composed of a compound including a metal
- B23C2224/36—Titanium nitride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23C—MILLING
- B23C2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
- B23C2228/04—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner applied by chemical vapour deposition [CVD]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23C—MILLING
- B23C2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
- B23C2228/10—Coating
Definitions
- the present invention relates to a surface-coated cutting tool and a manufacturing method thereof.
- Patent Document 1 proposes a cutting tool including a cemented carbide base material and an ⁇ -Al 2 O 3 layer having a (006) texture. .
- Patent Document 2 ⁇ -Al 2 O 3 which has a (0012) texture and contains 100 ppm or more of sulfur on a cemented carbide base material. Cutting tools with layers have been proposed.
- JP 2008-246664 A European Patent Application Publication No. 2705510
- the present invention has been made in view of the above circumstances, and a surface-coated cutting tool capable of achieving a long life by forming a film having excellent slidability as well as excellent wear resistance and production thereof It aims to provide a method.
- the surface-coated cutting tool includes a base material and a coating formed on the base material, the coating including an ⁇ -Al 2 O 3 layer, and the ⁇ -Al 2 O 3 layer.
- the layer includes a plurality of ⁇ -Al 2 O 3 crystal grains and sulfur, and TC (006) exceeds 5 in the orientation index TC (hkl), and the sulfur includes the ⁇ -Al 2 O 3 layer.
- TC 006
- TC (006) exceeds 5 in the orientation index TC (hkl)
- the sulfur includes the ⁇ -Al 2 O 3 layer.
- the density distribution decreases in the direction away from the substrate side.
- FIG. 5 is a drawing-substituting photograph showing the measurement points in the ⁇ -Al 2 O 3 layer used for measuring the sulfur (S) content by EDS on a micrograph.
- a surface-coated cutting tool includes a base material and a coating formed on the base material, and the coating includes an ⁇ -Al 2 O 3 layer, and the ⁇ -Al
- the 2 O 3 layer includes a plurality of ⁇ -Al 2 O 3 crystal grains and sulfur, and TC (006) exceeds 5 in the orientation index TC (hkl), and the sulfur includes the ⁇ -Al 2 In the thickness direction of the O 3 layer, it has a concentration distribution in which the concentration decreases in the direction away from the substrate side.
- the surface-coated cutting tool having such a configuration can exhibit excellent slidability as well as excellent wear resistance.
- the surface or the interface is parallel to the surface of the ⁇ -Al 2 O 3 layer or the surface of the ⁇ -Al 2 O 3 layer adjacent to the side opposite to the substrate.
- the ⁇ -Al 2 O 3 crystal grains having a particle size of 0.2 to 2 ⁇ m preferably occupy 20 to 80 area%. Thereby, abrasion resistance can be improved.
- the TC (006) preferably exceeds 6. This effectively improves the wear resistance and slidability of the tool.
- the TC (006) is more preferably more than 7. Thereby, the wear resistance and slidability of the tool are more effectively improved.
- the maximum sulfur concentration Csmax in the concentration distribution is a region from the interface with the base material or the interface with the layer adjacent to the base material side to 1 ⁇ m in the thickness direction of the ⁇ -Al 2 O 3 layer.
- the minimum sulfur concentration Csmin in the concentration distribution is the surface of the ⁇ -Al 2 O 3 layer or the substrate side of the ⁇ -Al 2 O 3 layer in the thickness direction of the ⁇ -Al 2 O 3 layer. Appears in the region from the interface with the adjacent layer on the opposite side to 1 ⁇ m, the Csmax is 0.005 to 1 atomic%, the Csmin is 0.001 to 0.1 atomic%, and Csmax> It is preferable to satisfy the relationship of Csmin. Thereby, abrasion resistance can be improved.
- the maximum sulfur concentration Csmax in the concentration distribution is preferably 0.005 to 1 atomic%. Thereby, especially slidability can be improved.
- the ⁇ -Al 2 O 3 layer preferably has an average layer thickness of 1 to 15 ⁇ m. Thereby, both wear resistance and chipping resistance can be achieved.
- an outermost surface layer mainly composed of Ti carbide, nitride, or boride is disposed on the surface of the coating. Thereby, identification of the corner part of a tool becomes easy.
- the coating has an intermediate layer between the ⁇ -Al 2 O 3 layer and the base material, and the intermediate layer contains acicular TiCNO or acicular TiBN and has an average layer thickness. Is preferably 0.3 to 1 ⁇ m, and the difference between the maximum thickness and the minimum thickness of the intermediate layer is preferably 0.3 ⁇ m or more. Thereby, the adhesiveness in the coating of the ⁇ -Al 2 O 3 layer can be improved.
- a method for producing a surface-coated cutting tool includes a step of forming the coating film including the ⁇ -Al 2 O 3 layer on the base material by a CVD method,
- the amount of H 2 S gas contained in the raw material gas at the initial stage of formation of the ⁇ -Al 2 O 3 layer is set to 0.5 to 5% by volume, and the amount is instantaneously increased to 0.65 to 7% by volume. .
- a surface-coated cutting tool that can exhibit excellent slidability as well as excellent wear resistance can be manufactured.
- the surface-coated cutting tool of this embodiment includes a base material and a coating film formed on the base material.
- the coating preferably covers the entire surface of the substrate. However, even if a part of the substrate is not coated with this coating or the configuration of the coating is partially different, it does not depart from the scope of the present invention.
- the surface-coated cutting tool of the present embodiment includes a drill, an end mill, a cutting edge replaceable cutting tip for a drill, a cutting edge replaceable cutting tip for an end mill, a cutting edge replaceable cutting tip for milling, a cutting edge replaceable cutting tip for turning, a metal saw, It can be suitably used as a cutting tool such as a gear cutting tool, reamer, or tap.
- any substrate can be used as long as it is conventionally known as this type of substrate.
- cemented carbide for example, WC-based cemented carbide, including WC, including Co or containing carbonitride such as Ti, Ta, Nb), cermet (TiC, TiN, TiCN, etc.) Main component
- high-speed steel ceramics (titanium carbide, silicon carbide, silicon nitride, aluminum nitride, aluminum oxide, etc.), cubic boron nitride sintered body, or diamond sintered body Is preferred.
- a cemented carbide particularly a WC-based cemented carbide, or select a cermet (particularly a TiCN-based cermet).
- These base materials are particularly excellent in the balance between hardness and strength at high temperatures, and have excellent characteristics as base materials for surface-coated cutting tools for the above applications.
- the base material includes those having a chip breaker and those having no chip breaker.
- the edge of the edge of the blade edge is sharp edge (the ridge where the rake face and flank face intersect), honing (the sharp edge is given a radius), negative land (the chamfered), honing and negative land. Any combination of these is included.
- the coating includes an ⁇ -Al 2 O 3 layer.
- the coating can be composed of a plurality of layers including one or more ⁇ -Al 2 O 3 layers and further including other layers.
- TiCNO layer TiBN layer, TiC layer, TiN layer, TiAlN layer, TiSiN layer, AlCrN layer, TiAlSiN layer, TiAlNO layer, AlCrSiCN layer, TiCN layer, TiSiC layer, CrSiN layer, AlTiSiCO layer, TiSiCN layer Etc.
- atomic ratio when a compound is represented by a chemical formula as described above, when the atomic ratio is not particularly limited, any conventionally known atomic ratio is included, and is not necessarily limited to the stoichiometric range.
- a metal element such as titanium (element symbol: Ti), aluminum (element symbol: Al), silicon (element symbol: Si), zirconium (element symbol: Zr), or chromium (element symbol: Cr).
- nonmetallic elements such as nitrogen (element symbol: N), oxygen (element symbol: O), and carbon (element symbol: C) do not necessarily have to have a stoichiometric composition.
- the coating has an average layer thickness of 3 to 35 ⁇ m (3 ⁇ m or more and 35 ⁇ m or less.
- the average layer thickness of the coating is preferably 5 to 20 ⁇ m. If this average layer thickness is less than 3 ⁇ m, the wear resistance may be insufficient. If this average layer thickness exceeds 35 ⁇ m, peeling or destruction of the coating film may occur frequently when a large stress is applied between the coating film and the substrate in the intermittent processing.
- the ⁇ -Al 2 O 3 layer includes a plurality of ⁇ -Al 2 O 3 crystal grains (aluminum oxide whose crystal structure is ⁇ -type) and sulfur (element symbol: S).
- ⁇ -Al 2 O 3 layer contains the ⁇ -Al 2 O 3 of containing crystal grains of a plurality of ⁇ -Al 2 O 3 polycrystal. Usually, this crystal grain has a grain size of about 0.1 to 2 ⁇ m.
- ⁇ -Al 2 O 3 layer In the ⁇ -Al 2 O 3 layer, many ⁇ -Al 2 O 3 crystal grains are (006) -oriented.
- the ⁇ -Al 2 O 3 layer has a TC (006) exceeding 5 in the orientation index TC (hkl) represented by the following formula (1).
- I (hkl) represents the X-ray diffraction intensity of the (hkl) reflecting surface
- I 0 (hkl) represents the standard intensity according to ICDD PDF card number 00-010-0173.
- n in Formula (1) shows the number of reflection used for calculation, and is 8 in this embodiment.
- the (hkl) plane used for reflection is (012), (104), (110), (006), (113), (024), (116), and (300).
- ICDD International Center for Diffraction Data (International Diffraction Data Center).
- PDF registered trademark
- Powder Diffraction File is an abbreviation for Powder Diffraction File.
- the TC (006) of the ⁇ -Al 2 O 3 layer of the present embodiment can be expressed by the following formula (2).
- TC (006) exceeds 5 in the orientation index TC (hkl) means that the numerical value obtained by the above equation (2) obtained by substituting TC (006) into the above equation (1) exceeds 5. means.
- the ⁇ -Al 2 O 3 layer having a TC (006) value of more than 5 contributes to improved wear resistance because the hardness and Young's modulus are superior to the impact and vibration associated with severe cutting conditions. Can do.
- the value of TC (006) is preferably more than 6, more preferably more than 7. As the value of TC (006) is larger, the wear resistance can be effectively improved. Although the upper limit of the value of TC (006) is not limited, since there are eight reflecting surfaces used for the calculation, it may be set to 8 or less.
- TC (hkl) is, for example, as follows using SmartLab (registered trademark) (scanning speed: 21.7 ° / min, step: 0.01 °, scan range: 15 to 140 °) manufactured by Rigaku Corporation. It can be measured under conditions.
- SmartLab registered trademark
- scan range 15 to 140 °
- XRD result the result of TC (hkl) measurement using an X-ray diffractometer.
- the “concentration distribution in which the concentration decreases in the direction away from the substrate side in the thickness direction of the ⁇ -Al 2 O 3 layer” of sulfur refers to the sulfur concentration in the thickness direction of the ⁇ -Al 2 O 3 layer. It means that the portion where the concentration decreases in the direction away from the substrate side may be included.
- the interface between the base material of the ⁇ -Al 2 O 3 layer (if there is a layer adjacent to the substrate side of the ⁇ -Al 2 O 3 layer is the interface between the layer) to just above the point X
- the Y point is directly below the surface of the ⁇ -Al 2 O 3 layer (if there is a layer adjacent to the side opposite to the substrate side of the Al 2 O 3 layer)
- the concentration distribution is such that the S content at the X point> the S content at the Y point.
- the concentration of S in the direction away from the substrate side is There may be a constant part. Further, there may be a portion where the concentration increases in a direction away from the substrate side, or there may be a portion not containing sulfur.
- the maximum sulfur concentration Csmax in the above concentration distribution is the interface between the ⁇ -Al 2 O 3 layer and the substrate side of the ⁇ -Al 2 O 3 layer in the thickness direction of the ⁇ -Al 2 O 3 layer. It preferably appears in a region of 1 ⁇ m from the interface with the adjacent layer.
- the minimum sulfur concentration Csmin in the above concentration distribution is adjacent to the surface of the ⁇ -Al 2 O 3 layer or the side opposite to the substrate side of the ⁇ -Al 2 O 3 layer in the thickness direction of the ⁇ -Al 2 O 3 layer. Preferably, it appears in a region from the interface with the layer to 1 ⁇ m.
- Csmax is preferably 0.005 to 1 atomic%
- Csmin is preferably 0.001 to 0.1 atomic%, and preferably satisfies the relationship Csmax> Csmin.
- Csmax may appear directly above the interface or ⁇ -Al 2 O 3 layer a layer adjacent to the substrate side of the base material of the ⁇ -Al 2 O 3 layer.
- Csmin is the substrate side of the ⁇ -Al 2 O 3 layer surface or ⁇ -Al 2 O 3 layer may appear immediately below the interface between the layer adjacent to the opposite side.
- the difference between Csmax and Csmin is more preferably 0.1 atomic% or more.
- the upper limit of the difference between Csmax and Csmin may be 0.9 atomic%. If the difference is larger than this, coarse grains may be generated.
- Csmax is preferably 0.005 to 1 atomic%, more preferably 0.05 to 1 atomic%, and further preferably 0.1 to 0.7 atomic%. Thereby, slidability can be improved. If Csmax is less than 0.005 atomic%, the slidability becomes insufficient, and the welding of the work material may easily proceed during cutting. If Csmax exceeds 1 atomic%, the chipping resistance may be lowered.
- Csmin is preferably 0.001 to 0.01 atomic%. Even if Csmin is less than 0.001 atomic%, it is difficult to obtain higher wear resistance.
- the content of S contained in the ⁇ -Al 2 O 3 layer is represented by atomic%.
- the content of S is the sum of the number of Al atoms, the number of O atoms, the number of C atoms, the number of chlorine (element symbol: Cl) atoms, the number of Ti atoms and the number of S atoms as the denominator.
- the atomic composition percentage [S / (Al + O + C + Cl + Ti + S) ⁇ 100] with the number of S atoms as a molecule.
- the S content is determined by polishing the cross section of the coating parallel to the cross section in the thickness direction of the ⁇ -Al 2 O 3 layer by ion milling, and the polished surface is subjected to energy dispersive X-ray analysis using a field emission scanning electron microscope. It can be measured by analyzing with an apparatus (EDS: Energy Dispersive X-ray Spectroscopy). Further, the S content can be measured in more detail by using a WDS (Wavelength Dispersive X-ray Spectroscopy) analysis method.
- EDS Energy Dispersive X-ray Spectroscopy
- the conditions of said ion milling process are as follows, for example. Accelerating voltage: 6kV Irradiation angle: 0-5 ° from normal Irradiation time: 300 minutes
- the S content was measured by EDS using a SU6600 (model number) field emission scanning electron microscope manufactured by Hitachi High-Technologies Corporation. At the time of measurement, the acceleration voltage of the field emission scanning electron microscope was set to 15 kV. EDS conditions were set to 150 frames and selected atoms: C, O, Al, S, Cl, and Ti, respectively. As shown in FIG.
- the ⁇ -Al 2 O 3 layer 1 is formed at a predetermined interval in the thickness direction from the interface (TiCNO layer 3) with the base layer (TiCN layer 2) to the coating surface side. -The content of S in the Al 2 O 3 layer 1 was measured and its distribution was analyzed.
- FIG. 1 the measurement points in the ⁇ -Al 2 O 3 layer 1 used for measuring the S content by EDS are shown on a micrograph.
- a TiCN layer 2 is formed on a substrate, a TiCNO layer 3 is laminated on the TiCN layer 2, and an ⁇ -Al 2 O 3 layer 1 is laminated on the TiCNO layer 3.
- measurement points were measured at predetermined intervals (for example, every 1.0 ⁇ m) in the thickness direction from directly above the TiCNO layer 3 which is the interface between the ⁇ -Al 2 O 3 layer 1 and the TiCN layer 2 to the coating surface side. 4 (first measurement point 41, second measurement point 42, third measurement point 43, fourth measurement point 44, fifth measurement point 45) was set. Then, the S content at each measurement point from the first measurement point 41 to the fifth measurement point 45 was measured.
- ⁇ Grain size of ⁇ -Al 2 O 3 crystal grains contained in ⁇ -Al 2 O 3 layer is measured parallel to the interface with the adjacent layer on the surface or on the side opposite to the substrate side and located at a depth of 0.5 ⁇ m from the surface or the interface.
- ⁇ -Al 2 O 3 crystal grains having a grain size of 0.2 to 2 ⁇ m occupy 20 to 80 area%. If the grain size of ⁇ -Al 2 O 3 occupying 20 to 80 area% on this measurement surface is less than 0.2 ⁇ m, the fracture resistance may be lowered. If this particle diameter exceeds 2 ⁇ m, the wear resistance may be reduced.
- the upper limit of the particle diameter is preferably 1.85 ⁇ m or less.
- the lower limit of the particle size is 0.2 ⁇ m, and can be said to be a preferable value unless it is less than 0.2 ⁇ m. This is because, within such a particle size range, it is possible to improve wear resistance as well as fracture resistance.
- the proportion of ⁇ -Al 2 O 3 crystal grains having a grain size of 0.2 to 2 ⁇ m on the measurement surface is less than 20 area% or 80 area% or more, the chipping resistance In addition, it is not preferable because the wear resistance cannot be improved.
- a more preferable ratio of ⁇ -Al 2 O 3 crystal grains having a grain size of 0.2 to 2 ⁇ m is 50 to 70 area%.
- the measurement of the grain size of the ⁇ -Al 2 O 3 crystal grains on the measurement surface of the ⁇ -Al 2 O 3 layer is performed by measuring the fracture surface parallel to the cross section in the thickness direction of the ⁇ -Al 2 O 3 layer. It was done in. Specifically, on the fracture surface, from the surface of the ⁇ -Al 2 O 3 layer (if there is a layer adjacent to the side opposite to the substrate side of the Al 2 O 3 layer, the interface with that layer) A portion 0.5 ⁇ m away from the ⁇ -Al 2 O 3 layer was observed with a field emission scanning electron microscope. The particle diameter of the ⁇ -Al 2 O 3 crystal grains can be measured from the microscopic image using a section method. Further, the fracture surface can be polished by ion milling, and the particle size of ⁇ -Al 2 O 3 crystal grains can be measured from EBSD analysis using a microscopic image of the polished surface.
- the ⁇ -Al 2 O 3 layer desirably has an average layer thickness of 1 to 15 ⁇ m. Thereby, both wear resistance and chipping resistance can be achieved. If the average layer thickness of the ⁇ -Al 2 O 3 layer is less than 1 ⁇ m, wear may easily proceed. When the average layer thickness exceeds 15 ⁇ m, the chipping resistance may be lowered.
- the coating can include other layers in addition to the ⁇ -Al 2 O 3 layer.
- An example of such another layer is a TiCN layer. Since this TiCN layer is excellent in wear resistance, it is possible to impart suitable wear resistance to the coating.
- the TiCN layer is particularly preferably formed by MT-CVD (medium temperature CVD).
- the MT-CVD method can form a film at a relatively low temperature among the CVD methods of about 800 to 1000 ° C., and can reduce damage to the substrate due to heating during film formation.
- the TiCN layer can be disposed, for example, between the ⁇ -Al 2 O 3 layer and the substrate.
- the TiCN layer preferably has an average layer thickness of 2 to 20 ⁇ m. If the average thickness of the TiCN layer is less than 2 ⁇ m, there is a possibility that the wear easily proceeds. If this average layer thickness exceeds 20 ⁇ m, the chipping resistance may be lowered.
- outermost surface layer In addition, the outermost surface layer, intermediate
- ⁇ Outermost surface layer> It is preferable that an outermost surface layer mainly composed of any one of Ti carbide, nitride or boride is disposed on the surface of the coating.
- the outermost surface layer is a layer disposed on the most surface side in the coating. However, it may not be formed in the region including the edge of the cutting edge. For example, when no other layer is formed on the ⁇ -Al 2 O 3 layer, the outermost surface layer is disposed directly on the ⁇ -Al 2 O 3 layer.
- the main component is any one of Ti carbide, nitride, and boride” means that 90% by mass or more of any of Ti carbide, nitride, and boride is included. Further, it preferably means that it consists of any one of Ti carbide, nitride and boride except for inevitable impurities.
- the corner identification (identification of the used part) of the cutting tip after the cutting use is facilitated by the effect of exhibiting a clear color.
- the outermost layer preferably has an average layer thickness of 0.05 to 1 ⁇ m.
- the upper limit of the average layer thickness of the outermost surface layer is preferably 0.8 ⁇ m, more preferably 0.6 ⁇ m.
- the lower limit of the average layer thickness is preferably 0.1 ⁇ m, and more preferably 0.2 ⁇ m. If the average layer thickness is less than 0.05 ⁇ m, when compressive residual stress is applied to the coating, the effect may not be sufficiently obtained, and the fracture resistance may not be improved. When the average layer thickness exceeds 1 ⁇ m, the adhesion with the layer adjacent to the outermost surface layer may be lowered.
- the coating preferably has an intermediate layer between the ⁇ -Al 2 O 3 layer and the substrate.
- the intermediate layer is configured to include acicular TiCNO or acicular TiBN.
- the intermediate layer and the ⁇ -Al 2 O 3 layer is preferably disposed between the TiCN layer disposed between the ⁇ -Al 2 O 3 layer and the substrate, ⁇ -Al 2 O 3 layer More preferably, the Al-Al 2 O 3 layer and the TiCN layer are both in contact with each other between the TiCN layer and the TiCN layer. This is because the adhesion of the ⁇ -Al 2 O 3 layer in the coating is enhanced.
- the intermediate layer can be formed by a known method.
- the intermediate layer preferably has an average layer thickness of 0.3 to 1 ⁇ m. This is because the adhesion of the ⁇ -Al 2 O 3 layer in the coating is further enhanced.
- the average layer thickness of the intermediate layer is more preferably 0.4 to 0.8 ⁇ m.
- the difference between the maximum thickness and the minimum thickness of the intermediate layer is preferably 0.3 ⁇ m or more. Thereby, the adhesion of the ⁇ -Al 2 O 3 layer in the coating can be reliably increased. If the difference between the maximum thickness and the minimum thickness of the intermediate layer is less than 0.3 ⁇ m, the effect of improving the adhesion of the ⁇ -Al 2 O 3 layer may not be sufficiently obtained.
- the upper limit of the difference between the maximum thickness and the minimum thickness of the intermediate layer is 0.9 ⁇ m. If this difference exceeds 0.9 ⁇ m, the ⁇ -Al 2 O 3 crystal grains become non-uniform and the adhesion may be reduced.
- the method for measuring the thickness of the intermediate layer is the same as the method used for measuring the grain size of ⁇ -Al 2 O 3 crystal grains. That is, it can be measured by observing a film cross section parallel to the cross section in the thickness direction of the ⁇ -Al 2 O 3 layer with a field emission scanning electron microscope.
- the average layer thickness of the intermediate layer is measured, for example, at a plurality of locations of the intermediate layer by the above measurement method. It can be determined by calculating the value.
- the maximum thickness and the minimum thickness of the intermediate layer can also be determined by picking up the maximum value and the minimum value from the layer thicknesses at a plurality of locations of the intermediate layer measured by the above measurement method.
- the cross section can be polished by ion milling, and measurement using a microscopic image of the polished surface is also possible.
- the method for producing a surface-coated cutting tool includes a step of forming a film containing an ⁇ -Al 2 O 3 layer on a substrate by a CVD method, and in this step, the formation of the ⁇ -Al 2 O 3 layer is performed.
- the amount of H 2 S gas contained in the raw material gas in the initial stage is set to 0.5 to 5% by volume, and the amount is instantaneously increased to 0.65 to 7% by volume.
- the initial stage of formation of the ⁇ -Al 2 O 3 layer refers to a time when nucleation of crystal grains of Al 2 O 3 is performed.
- the surface-coated cutting tool can be preferably manufactured by forming a film on a substrate by a chemical vapor deposition (CVD) method.
- CVD chemical vapor deposition
- the film forming temperature is 800 to 1200 ° C., which is higher than the physical vapor deposition method, and the adhesion to the substrate is improved.
- other layers other than the ⁇ -Al 2 O 3 layer are formed, these layers can be formed by a conventionally known method.
- the thicknesses of the ⁇ -Al 2 O 3 layer and other layers can be adjusted by appropriately adjusting the film formation time (the film formation rate of each layer is about 0.5 to 2.0 ⁇ m / hour). is there).
- the ⁇ -Al 2 O 3 layer can be formed by the following method using, for example, a CVD method.
- a TiCN layer is formed on the substrate by a known method with or without another layer, and a TiCNO layer is formed on the surface of the TiCN layer. Further, the surface of the TiCNO layer is oxidized to nucleate ⁇ -Al 2 O 3 crystal grains. Subsequently, an ⁇ -Al 2 O 3 layer is formed (a crystal of ⁇ -Al 2 O 3 is grown).
- H 2 S is added to the raw material gas to be introduced.
- the blending amount of the gas is set to a blending amount selected from 0.5 to 5% by volume.
- the compounding amounts of the source gases other than H 2 S gas are as follows: AlCl 3 is 1.3 to 2.5% by volume, HCl is 2.8 to 6% by volume, CO is 1 to 5% by volume, CO 2 is 0.4 to 3% by volume, O 2 is 0.002 to 0.008% by volume, and the balance is H 2 .
- the furnace temperature of the CVD apparatus is 970 to 1020 ° C., and the furnace pressure is 70 to 110 hPa.
- the surface of the TiCNO layer is oxidized by CO, CO 2 and O 2 in the composition of the raw material gas for nucleating ⁇ -Al 2 O 3 crystal grains.
- the H 2 S gas contained in the raw material gas is instantaneously (pulsed) more than the amount selected from 0.5 to 5% by volume. Introduce raw material gas into the increased blending amount. This operation can be performed once or twice or more. That is, first, the blending amount of H 2 S gas is modulated in a pulse shape to nucleate ⁇ -Al 2 O 3 crystal grains, and then ⁇ -Al 2 O is used as a raw material gas having the blending amount of each composition described above. 3 crystal grains are grown to form an ⁇ -Al 2 O 3 layer.
- an ⁇ -Al 2 O 3 layer having a concentration distribution of S in which the concentration decreases in the thickness direction away from the substrate side can be formed.
- the amount to be increased may be adjusted by lowering the amount of H 2 gas that occupies the remainder of the source gas. This is convenient because the blending amount of other gases, the furnace temperature of the CVD apparatus, and the furnace pressure can be made unchanged.
- the blending amount (pulse height) of the H 2 S gas that is instantaneously increased is preferably 130 to 160% with respect to the blending amount selected from 0.5 to 5% by volume. If it is less than 130%, Csmax may be 0.005 atomic% or less. Moreover, when it exceeds 160%, a crystal grain will coarsen and there exists a possibility that the outstanding abrasion resistance may not be obtained.
- the concentration distribution of S as described above can be expressed as ⁇ It can be formed in the thickness direction of the Al 2 O 3 layer.
- Example 1 ⁇ Preparation of substrate> A base material made of a cemented carbide base material (manufactured by Sumitomo Electric Industries) having the shape of CNMG120408 defined in JIS (Japan Industrial Standard) B 4120 (1998) was prepared. The prepared base materials are classified into 7 groups named samples A1 to A7. Moreover, six base materials were prepared for each group. These substrates have a composition consisting of 87.0 wt% WC, 8.0 wt% Co, 2.5 wt% TiC, 1.5 wt% NbC, and 1.0% TaC.
- sample A1 to sample A4 are examples, and sample A5 to sample A7 are comparative examples.
- the nucleation of ⁇ -Al 2 O 3 crystal grains is performed by oxidizing the surface of the TiCNO layer formed on the surface of the TiCN layer.
- An Al 2 O 3 layer was formed.
- the amount of H 2 S gas contained in the introduced raw material gas is set to 0. It was set to 6% by volume.
- the amount of each component gas containing H 2 S gas of the material gas is as shown in Table 2 below.
- H 2 S gas content which had been 0.6% by volume, was instantaneously increased beyond 0.6% by volume. Thereafter, H 2 the amount of S gas was set to 0.6 vol%, H 2 S gas in the raw material gas the amount of each component gas were as shown in Table 2 below containing alpha-Al 2 O 3 crystal grains were grown to form an ⁇ -Al 2 O 3 layer.
- Example 1 the amount of instantaneously elevated H 2 S gas introduced to the sample A1 ⁇ A7 (pulse height) and time for introducing the H 2 S gas in amounts which momentarily increased (Pulse width) was varied. Specifically, with respect to the samples A1 to A4, the pulse height is 150% (that is, 0.9% by volume) of 0.6% by volume of the H 2 S gas, and 0.8 to 1. H 2 S gas was introduced with different pulse widths within a range of 3 minutes. On the other hand, H 2 S gas was not introduced for samples A5 to A6 by increasing the blending amount instantaneously.
- the layer structure of the coating formed in Samples A1 to A7 is a TiN layer, a TiCN layer, a TiCNO layer, an ⁇ -Al 2 O 3 layer, a TiC layer, and a TiN layer in order from the substrate side.
- Table 3 shows the layer structure and the layer thickness ( ⁇ m) of Samples A1 to A7.
- Example 1 ⁇ Content of the test>
- six samples A1 to A7 are prepared.
- the flank face was irradiated with X-rays, and the TC (006) of the ⁇ -Al 2 O 3 layer was measured.
- the S content in the ⁇ -Al 2 O 3 layer was measured.
- the particle diameter of ⁇ -Al 2 O 3 crystal grains was measured for the third piece.
- the slidability was evaluated for the fourth piece.
- the wear resistance was evaluated for the fifth piece. Fracture resistance was evaluated for the sixth piece.
- the content of S of ⁇ -Al 2 O 3 layer is measured point set from just above the interface between the TiCNO layer adjacent to the substrate side of the ⁇ -Al 2 O 3 layer in the coating section in 1 ⁇ m per the film surface Measurement was performed at (first measurement point to fifth measurement point) (see FIG. 1). Also, alpha-Al 2 O 3 crystal grains having a grain size is, Al 2 and the base side of the O 3 layer from the interface between the TiC layer adjacent the opposite side to the alpha-Al 2 O 3 layer side 0. Measurements were taken at 5 ⁇ m away.
- Wear resistance is evaluated by observing the wear width (Vb) formed on the flank of the cutting tool after setting the cutting tool on an NC lathe and cutting the work material for a predetermined time. It can be evaluated that the smaller the value of the wear width (Vb), the better the wear resistance.
- Defect resistance is evaluated by setting the cutting tool on an NC lathe, cutting the work material, and measuring the time until chipping or chipping occurs in the cutting tool. Therefore, it can be evaluated that the longer the time until chipping or chipping, the better the chipping resistance.
- the coefficient of friction ( ⁇ ) was measured by performing the pin-on-disk method under a load of 10N and room temperature. It can be said that the smaller the value of the coefficient of friction ( ⁇ ), the smoother it is, and the better the slidability.
- AA Excellent wear resistance, chipping resistance and sliding property (Vb is 0.165 or less, time to chipping is 6 minutes or more, and friction coefficient ( ⁇ ) is 0.35 or less)
- Vb Chipping resistance and sliding property
- ⁇ friction coefficient
- A Excellent wear resistance, fracture resistance, and slidability (two of the requirements that Vb is 0.165 or less, the time to fracture is 6 minutes or more, and the coefficient of friction ( ⁇ ) is 0.35 or less.
- the TC (006) of the ⁇ -Al 2 O 3 layer was more than 5.
- S content a Csmax of 0.05 to 0.330 atomic% was obtained on the TiCNO layer side of the ⁇ -Al 2 O 3 layer, which is the first measurement point.
- concentration of S decreases in the direction away from the TiCNO layer, and a Csmin of 0.003 to 0.005 atomic% is obtained on the TiC layer side of the ⁇ -Al 2 O 3 layer which is the fifth measurement point. It was.
- the concentration distribution of S in the example has a concentration distribution in which the concentration decreases in the direction away from the substrate side in the thickness direction of the ⁇ -Al 2 O 3 layer.
- the difference between Csmax and Csmin was 0.047 to 0.325.
- the particle diameter of ⁇ -Al 2 O 3 crystal grains at a location 0.5 ⁇ m away from the interface with the TiC layer toward the ⁇ -Al 2 O 3 layer was 1.85 ⁇ m or less.
- ⁇ Discussion> That is, in this example, in addition to the introduction of H 2 S gas with a compounding amount of 0.6% by volume, at a predetermined pulse width (0.8 to 1.3 minutes) and pulse height (150%). H 2 S gas was introduced three times to form an ⁇ -Al 2 O 3 layer.
- This ⁇ -Al 2 O 3 layer had TC (006) of more than 5, and had a concentration distribution of S in which the concentration decreased in the direction away from the substrate side in the thickness direction.
- the cutting tool of the example provided with such a coating containing the ⁇ -Al 2 O 3 layer showed the performance that Vb was 0.168 or less and the time to failure was 5.9 minutes or more, and had excellent resistance. It had wear and fracture resistance. Further, the coefficient of friction ( ⁇ ) also showed a value of 0.38 or less, and it was revealed that it has excellent slidability at the same time. Therefore, the cutting tool of the embodiment can achieve a long life.
- Example 2> ⁇ Preparation of substrate>
- the base material which consists of the cemented carbide base material (made by Sumitomo Electric Industries) which has the shape of CNMG120408 similar to Example 1 was prepared.
- the prepared base materials are classified into three groups named Samples B1 to B3. Moreover, six base materials were prepared for each group.
- This base material is composed of 92.5 wt% WC, 6.0 wt% Co, and 1.5 wt% NbC.
- sample B1 is an example
- samples B2 to B3 are comparative examples.
- Example 2 ⁇ Formation of coating> Under the same conditions as in Example 1, the base materials of Samples B1 to B3 were honed and set in a chemical vapor deposition apparatus, and a film was formed on each of the surfaces by the CVD method. In Example 2, the TiN layer was not included in the coating composition.
- the nucleation of ⁇ -Al 2 O 3 crystal grains is performed by oxidizing the surface of the TiCNO layer formed on the surface of the TiCN layer.
- An Al 2 O 3 layer was formed.
- the amount of H 2 S gas contained in the introduced source gas is set to 1. It was set to 7% by volume.
- the amount of each component gas containing H 2 S gas of the material gas is as shown in Table 5 below.
- H 2 S-gas is set to 1.7 vol%, H 2 S gas in the raw material gas the amount of each component gas were as shown in Table 5 below containing the ⁇ -Al 2 O 3 crystals The grains were grown to form an ⁇ -Al 2 O 3 layer.
- the cycle (pulse cycle) for introducing the H 2 S gas by instantaneously increasing the blending amount was different for the samples B1 to B3.
- the pulse period was 3 minutes for sample B1, 7 minutes for sample B2, and 1 minute for sample B3.
- the pulse height is 130% (ie, 2.21% by volume) compared to 1.7% by volume of H 2 S gas, and the pulse for 2 minutes.
- the blending amount was increased instantaneously and H 2 S gas was introduced twice.
- the layer structure of the coating formed from Samples B1 to B3 is a TiN layer, a TiCN layer, a TiCNO layer, an ⁇ -Al 2 O 3 layer, and a TiC layer in order from the substrate side.
- Table 6 below shows the layer structure and the layer thickness ( ⁇ m) of Samples B1 to B3.
- Example 2 ⁇ Content of the test>
- six samples B1 to B3 are prepared.
- the flank face was irradiated with X-rays, and the TC (006) of the ⁇ -Al 2 O 3 layer was measured.
- the S content in the ⁇ -Al 2 O 3 layer was measured.
- the particle diameter of ⁇ -Al 2 O 3 crystal grains was measured for the third piece.
- the slidability was evaluated for the fourth piece.
- the wear resistance was evaluated for the fifth piece. Fracture resistance was evaluated for the sixth piece.
- the content of S of ⁇ -Al 2 O 3 layer was set from just above the interface between the TiCNO layer adjacent to the substrate side of the ⁇ -Al 2 O 3 layer in the coating section in 1.0 ⁇ m per the film surface Measurement was performed at measurement points (first measurement point to fifth measurement point) (see FIG. 1). Also, alpha-Al 2 O 3 crystal grains having a grain size is, Al 2 and the base side of the O 3 layer from the interface between the TiC layer adjacent the opposite side to the alpha-Al 2 O 3 layer side 0. Measurements were taken at 5 ⁇ m away.
- Wear resistance is evaluated by observing the wear width (Vb) formed on the flank of the cutting tool after setting the cutting tool on an NC lathe and cutting the work material for a predetermined time. It can be evaluated that the smaller the value of the wear width (Vb), the better the wear resistance.
- Defect resistance is evaluated by setting the cutting tool on an NC lathe, cutting the work material, and measuring the time until chipping or chipping occurs in the cutting tool. Therefore, it can be evaluated that the longer the time until chipping or chipping occurs, the better the chipping resistance.
- the coefficient of friction ( ⁇ ) was measured by performing the pin-on-disk method under a load of 10N and room temperature. It can be said that the smaller the value of the coefficient of friction ( ⁇ ), the smoother it is, and the better the slidability.
- AA Excellent wear resistance, chipping resistance and sliding property (Vb is 0.165 or less, time to chipping is 6 minutes or more, and friction coefficient ( ⁇ ) is 0.35 or less)
- Vb Chipping resistance and sliding property
- ⁇ friction coefficient
- A Excellent wear resistance, fracture resistance, and slidability (two of the requirements that Vb is 0.165 or less, the time to fracture is 6 minutes or more, and the coefficient of friction ( ⁇ ) is 0.35 or less.
- the TC (006) of the ⁇ -Al 2 O 3 layer was more than 5.
- the S content a Csmax of 0.850 atomic% was obtained on the TiCNO layer side of the ⁇ -Al 2 O 3 layer as the first measurement point.
- the concentration of S decreased in the direction away from the TiCNO layer in the thickness direction, and Csmin of 0.008 atomic% was obtained on the TiC layer side of the ⁇ -Al 2 O 3 layer as the fifth measurement point. Therefore, it was found that the concentration distribution of S in the example had a concentration distribution in which the concentration decreased in the direction away from the substrate side in the thickness direction of the ⁇ -Al 2 O 3 layer.
- the difference between Csmax and Csmin was 0.842.
- the particle diameter of the ⁇ -Al 2 O 3 crystal grains at a location 0.5 ⁇ m away from the interface with the TiC layer toward the ⁇ -Al 2 O 3 layer was 0.83 ⁇ m.
- ⁇ Discussion> That is, in this example, in addition to the introduction of H 2 S gas with a compounding amount of 1.7% by volume, the compounding amount is instantaneously increased at a predetermined pulse period (3 minutes) to increase the H 2 S gas to 2 Introduced twice, an ⁇ -Al 2 O 3 layer was formed.
- This ⁇ -Al 2 O 3 layer had TC (006) of more than 5, and had a concentration distribution of S in which the concentration decreased in the direction away from the substrate side in the thickness direction.
- the cutting tool of the example provided with such a coating containing the ⁇ -Al 2 O 3 layer showed the performance that Vb was 0.156 and the time to failure was 4.2 minutes, and necessary and sufficient wear resistance. And was found to have defect resistance. Further, the coefficient of friction ( ⁇ ) was 0.39, and it was revealed that the friction coefficient ( ⁇ ) had excellent slidability at the same time. Therefore, the cutting tool of the embodiment can achieve a long life.
Abstract
Description
本発明者らは、上記課題を解決するために鋭意検討を重ね、本発明に到達した。α-Al2O3層の核生成時に多量のH2Sをパルス状に変動させながら導入することによって、α-Al2O3層の厚み方向に硫黄の濃度分布を持たせた。具体的には、α-Al2O3層の厚み方向において、基材側から遠ざかる方向に減少していく硫黄の濃度分布を持たせた。これにより、優れた耐摩耗性とともに優れた摺動性を発揮することが可能となることを見出した。
[1]本発明の一態様に係る表面被覆切削工具は、基材と該基材上に形成された被膜とを備え、該被膜は、α-Al2O3層を含み、該α-Al2O3層は、複数のα-Al2O3の結晶粒と硫黄とを含み、かつ配向性指数TC(hkl)においてTC(006)が5を超え、該硫黄は、該α-Al2O3層の厚み方向において、該基材側から遠ざかる方向にその濃度が減少する濃度分布を有している。このような構成の表面被覆切削工具は、優れた耐摩耗性とともに優れた摺動性を発揮することができる。
以下、本発明の実施形態(以下「本実施形態」とも記す)についてさらに詳細に説明する。
本実施形態の表面被覆切削工具は、基材と該基材上に形成された被膜とを備える。被膜は、基材の全面を被覆することが好ましい。しかしながら、基材の一部がこの被膜で被覆されていなかったり被膜の構成が部分的に異なっていたりしていたとしても本発明の範囲を逸脱するものではない。
基材は、この種の基材として従来公知のものであればいずれも使用することができる。たとえば、超硬合金(たとえば、WC基超硬合金、WCのほか、Coを含み、あるいはTi、Ta、Nbなどの炭窒化物を添加したものも含む)、サーメット(TiC、TiN、TiCNなどを主成分とするもの)、高速度鋼、セラミックス(炭化チタン、炭化ケイ素、窒化ケイ素、窒化アルミニウム、酸化アルミニウムなど)、立方晶型窒化ホウ素焼結体、またはダイヤモンド焼結体のいずれかであることが好ましい。
被膜は、α-Al2O3層を含む。たとえば被膜は、α-Al2O3層を1層以上含み、さらに他の層を含んだ複数の層から構成することができる。
α-Al2O3層は、複数のα-Al2O3(結晶構造がα型である酸化アルミニウム)の結晶粒と硫黄(元素記号:S)とを含んでいる。α-Al2O3層は、複数のα-Al2O3の結晶粒を含んだ多結晶のα-Al2O3を含んでいる。通常この結晶粒は、約0.1~2μm程度の大きさの粒径をもつ。
管電圧: 45kV
管電流: 200mA
フィルター: 多層ミラー
光学系: 集中法
X線回折法: θ-2θ法
<α-Al2O3層に含まれる硫黄の濃度分布>
α-Al2O3層に含まれる硫黄(以下、元素記号である「S」で記す場合がある)は、α-Al2O3層の厚み方向において、基材側から遠ざかる方向にその濃度が減少する濃度分布を有している。具体的には、たとえば、α-Al2O3層の厚み方向において、基材側から遠ざかる方向に向けて順にA点、B点、C点を設定し、これらの点のSの含有量を測定すれば、A点のSの含有量>B点のSの含有量>C点のSの含有量となる濃度分布を有している。このようなSの濃度分布の形態により、優れた耐摩耗性が得られるとともに摺動性を飛躍的に向上させることができる。
加速電圧: 6kV
照射角度: 法線から0-5°
照射時間: 300分
本実施形態では、株式会社日立ハイテクノロジーズ社製SU6600(型番)の電界放出型走査電子顕微鏡を用いたEDSによりSの含有量を測定した。測定時には、電界放出型走査電子顕微鏡の加速電圧を15kVに設定した。EDSの条件は、フレーム数:150、選択原子:C、O、Al、S、Cl、Tiにそれぞれ設定した。図1に示すように、α-Al2O3層1の基材側の層(TiCN層2)との界面部(TiCNO層3)から被膜表面側へ向け、厚み方向に所定の間隔でα-Al2O3層1のSの含有量を測定し、その分布を分析した。
α-Al2O3層は、その表面またはその基材側とは反対側に隣接する層との界面に平行であって、かつ該表面または該界面から0.5μmの深さに位置する測定面において、粒径が0.2~2μmであるα-Al2O3の結晶粒が20~80面積%を占めることが好ましい。この測定面において、20~80面積%を占めるα-Al2O3の結晶粒の粒径が0.2μm未満であれば、耐欠損性が低下する恐れがある。この粒径が2μmを超えると、耐摩耗性が低下する恐れがある。
α-Al2O3層は、平均層厚が1~15μmであることが望ましい。これにより、耐摩耗性と耐欠損性とを両立させることができる。α-Al2O3層の平均層厚を1μm未満とすれば、摩耗が進みやすくなる恐れがある。この平均層厚が15μmを超えると耐欠損性が低下する恐れがある。
被膜は上述のとおり、α-Al2O3層以外に他の層を含むことができる。そのような他の層として、たとえばTiCN層をあげることができる。このTiCN層は耐摩耗性に優れるため、被膜により好適な耐摩耗性を付与することができる。TiCN層は、とりわけMT-CVD(medium temperature CVD)法により形成することが好ましい。MT-CVD法は約800~1000℃というCVD法の中でも比較的低温で成膜することができ、成膜時の加熱による基材のダメージを低減することができる。TiCN層は、たとえば、α-Al2O3層と基材との間に配置することができる。
<最表面層>
被膜は、その表面にTiの炭化物、窒化物または硼化物のいずれかを主成分とする最表面層が配置されることが好ましい。最表面層は、被膜において最も表面側に配置される層である。ただし、刃先稜線部を含む領域においては形成されない場合もある。最表面層は、たとえば、α-Al2O3層上に他の層が形成されていない場合、α-Al2O3層の直上に配置される。
被膜は、α-Al2O3層と基材との間に中間層を有することが好ましい。中間層は、針状のTiCNOまたは針状のTiBNを含んで構成される。たとえば、中間層はα-Al2O3層と、α-Al2O3層および基材の間に配置されるTiCN層との間に配置されることが好ましく、α-Al2O3層およびTiCN層の間であって、α-Al2O3層およびTiCN層にいずれも接して配置されることがさらに好ましい。被膜中におけるα-Al2O3層の密着性が高まるからである。中間層は、公知の方法により形成可能である。
本実施形態の表面被覆切削工具の製造方法は、基材上にCVD法でα-Al2O3層を含む被膜を形成する工程を含み、該工程において、α-Al2O3層の形成初期における原料ガスに含まれるH2Sガスの配合量を0.5~5体積%とし、瞬間的に該配合量を0.65~7体積%に高めている。ここで、α-Al2O3層の形成初期とは、Al2O3の結晶粒の核生成を行なう時期をいう。
<基材の調製>
JIS(Japanese Industrial Standard) B 4120(1998)に規定されるCNMG120408の形状を有する超硬合金母材(住友電気工業製)からなる基材を準備した。準備した基材は、試料A1~A7と名付けた7グループに分類される。また、一つのグループごとに基材を6個準備した。これらの基材は、87.0wt%のWCと、8.0wt%のCoと、2.5wt%のTiCと、1.5wt%のNbC、1.0%のTaCとからなる組成を有する。
試料A1~A7の基材を公知の方法でホーニングし、化学気相蒸着装置内にセットし、その表面にそれぞれCVD法で被膜を形成した。被膜の形成条件に関し、α-Al2O3層を除く各層の形成条件を以下の表1に記載した。
実施例1では上述のとおり、それぞれ6個の試料A1~A7を準備している。この6個のうち1個目に対し、逃げ面部にX線を照射してα-Al2O3層のTC(006)を測定した。2個目に対し、α-Al2O3層のSの含有量を測定した。3個目に対してα-Al2O3結晶粒の粒径を測定した。また4個目に対して摺動性を評価した。5個目に対して耐摩耗性を評価した。6個目に対して耐欠損性を評価した。
被削材: SCM435(JIS)
切削速度: 300m/min
送り: 0.3mm/rev
切込み: 2.0mm
切削油: 乾式
切削時間: 15min
評価: 切削時間15min後の逃げ面摩耗幅Vb(mm)を測定。
被削材: SCM435(JIS)溝入材
切削速度: 200m/min
送り: 0.3mm/rev
切込み: 1.5mm
切削油: 湿式
評価: チッピング又は欠損するまでの時間(分)を測定。
また、摩擦係数(μ)を測定することにより摺動性を評価した。摩擦係数(μ)は、ピンオンディスク法を10Nの荷重、室温の条件で行なって測定した。摩擦係数(μ)の値が小さいほど滑らかであるといえ、摺動性に優れると評価することができる。
AA: 耐摩耗性、耐欠損性および摺動性が非常に優れている(Vbが0.165以下、欠損までの時間が6分以上および摩擦係数(μ)が0.35以下)
A: 耐摩耗性、耐欠損性および摺動性が優れている(Vbが0.165以下、欠損までの時間が6分以上および摩擦係数(μ)が0.35以下の要件のうち2つを満たす)
B: 耐摩耗性、耐欠損性および摺動性が必要十分である(Vbが0.165~0.170、欠損までの時間が4~6分および摩擦係数(μ)が0.35~0.54)
C: 耐摩耗性、耐欠損性および摺動性が不十分である(Vbが0.170~0.180または欠損までの時間が4~6分であって、摩擦係数(μ)が0.54超)
D: 不能(粗大粒発生が発生したので、評価不可能)
<評価結果>
表4から理解されるように、試料A1~A4である実施例において、Vb(mm)が0.170以下の性能、かつ欠損までの時間が5分以上である性能を示し、優れた耐摩耗性および耐欠損性を備えると評価することができた。また、摺動性の評価において、実施例の摩擦係数(μ)は0.54以下であって、特に0.38以下の値を示して十分な摺動性を備えることが明らかとなった。
すなわち本実施例では、その配合量を0.6体積%としたH2Sガスの導入の他に、所定のパルス幅(0.8~1.3分)およびパルス高さ(150%)でH2Sガスを3回導入し、α-Al2O3層を形成した。このα-Al2O3層は、TC(006)が5を超え、かつ、その厚み方向において、基材側から遠ざかる方向にその濃度が減少するSの濃度分布を有していた。このようなα-Al2O3層を含む被膜を備えた実施例の切削工具は、Vbが0.168以下、かつ欠損までの時間が5.9分以上である性能を示し、優れた耐摩耗性および耐欠損性を有していた。また、摩擦係数(μ)も0.38以下の値を示して優れた摺動性を同時に有することが明らかとなった。したがって、実施例の切削工具は、長寿命化を果たすことができる。
<基材の調製>
実施例1と同様のCNMG120408の形状を有する超硬合金母材(住友電気工業製)からなる基材を準備した。準備した基材は、試料B1~B3と名付けた3グループに分類される。また、一つのグループごとに基材を6個準備した。この基材は、92.5wt%のWCと、6.0wt%のCoと、1.5wt%のNbCとから構成されている。なお、後述のとおり、試料B1は実施例となり、試料B2~B3は比較例となるものである。
実施例1と同様な条件で、試料B1~B3の基材をホーニングし、化学気相蒸着装置内にセットし、その表面にそれぞれCVD法で被膜を形成した。なお、実施例2では被膜の構成にTiN層を含めることをしなかった。
実施例2では上述のとおり、それぞれ6個の試料B1~B3を準備している。この6個のうち1個目に対し、逃げ面部にX線を照射してα-Al2O3層のTC(006)を測定した。2個目に対し、α-Al2O3層のSの含有量を測定した。3個目に対してα-Al2O3結晶粒の粒径を測定した。また4個目に対して摺動性を評価した。5個目に対して耐摩耗性を評価した。6個目に対して耐欠損性を評価した。
被削材: FCD700(JIS)
切削速度: 120m/min
送り: 0.3mm/rev
切込み: 2.0mm
切削油: 湿式
切削時間: 10min
評価: 切削時間10min後の逃げ面摩耗幅Vb(mm)を測定。
被削材: FCD450(JIS)溝入材
切削速度: 250m/min
送り: 0.2mm/rev
切込み: 1.5mm
切削油: 湿式
評価: チッピングまたは欠損するまでの時間(分)を測定。
また、摩擦係数(μ)を測定することにより摺動性を評価した。摩擦係数(μ)は、ピンオンディスク法を10Nの荷重、室温の条件で行なって測定した。摩擦係数(μ)の値が小さいほど滑らかであるといえ、摺動性に優れると評価することができる。
AA: 耐摩耗性、耐欠損性および摺動性が非常に優れている(Vbが0.165以下、欠損までの時間が6分以上および摩擦係数(μ)が0.35以下)
A: 耐摩耗性、耐欠損性および摺動性が優れている(Vbが0.165以下、欠損までの時間が6分以上および摩擦係数(μ)が0.35以下の要件のうち2つを満たす)
B: 耐摩耗性、耐欠損性および摺動性が必要十分である(Vbが0.165~0.170、欠損までの時間が4~6分および摩擦係数(μ)が0.35~0.54)
C: 耐摩耗性、耐欠損性および摺動性が不十分である(Vbが0.170~0.180または欠損までの時間が4~6分であって、摩擦係数(μ)が0.54超)
D: 不能(粗大粒発生が発生したので、評価不可能。)
<評価結果>
表7から理解されるように、試料B1である実施例においてVb(mm)が0.156の性能、かつ欠損までの時間が4.2分である性能を示し、優れた耐摩耗性および耐欠損性を備えると評価することができた。また、摺動性の評価において、実施例の摩擦係数(μ)は0.39の値を示して十分な摺動性を備えることが明らかとなった。
すなわち本実施例では、その配合量を1.7体積%としたH2Sガスの導入の他に、所定のパルス周期(3分)で配合量を瞬間的に高めてH2Sガスを2回導入し、α-Al2O3層を形成した。このα-Al2O3層は、TC(006)が5を超え、かつ、その厚み方向において、基材側から遠ざかる方向にその濃度が減少するSの濃度分布を有していた。このようなα-Al2O3層を含む被膜を備えた実施例の切削工具は、Vbが0.156、欠損までの時間が4.2分である性能を示し、必要十分な耐摩耗性および耐欠損性を有することが分かった。また、摩擦係数(μ)は0.39を示して優れた摺動性を同時に有することが明らかとなった。したがって、実施例の切削工具は、長寿命化を果たすことができる。
Claims (10)
- 基材と該基材上に形成された被膜とを備えた表面被覆切削工具であって、
前記被膜は、α-Al2O3層を含み、
前記α-Al2O3層は、複数のα-Al2O3の結晶粒と硫黄とを含み、かつ配向性指数TC(hkl)においてTC(006)が5を超え、
前記硫黄は、前記α-Al2O3層の厚み方向において、前記基材側から遠ざかる方向にその濃度が減少する濃度分布を有する、表面被覆切削工具。 - 前記α-Al2O3層の表面または前記α-Al2O3層の前記基材側とは反対側に隣接する層との界面に平行であって、かつ該表面または該界面から0.5μmの深さに位置する測定面において、粒径が0.2~2μmである前記α-Al2O3の結晶粒が20~80面積%を占める、請求項1に記載の表面被覆切削工具。
- 前記TC(006)が6を超える、請求項1または請求項2に記載の表面被覆切削工具。
- 前記TC(006)が7を超える、請求項1~請求項3のいずれか1項に記載の表面被覆切削工具。
- 前記濃度分布における前記硫黄の最大濃度Csmaxは、前記α-Al2O3層の厚み方向において前記基材との界面または前記基材側に隣接する層との界面から1μmまでの領域に現れ、
前記濃度分布における前記硫黄の最小濃度Csminは、前記α-Al2O3層の厚み方向において前記α-Al2O3層の表面または前記α-Al2O3層の基材側とは反対側に隣接する層との界面から1μmまでの領域に現れ、
前記Csmaxは0.005~1原子%であり、前記Csminは0.001~0.1原子%であり、かつCsmax>Csminの関係を満たす、請求項1~請求項4のいずれか1項に記載の表面被覆切削工具。 - 前記濃度分布における前記硫黄の最大濃度Csmaxは、0.005~1原子%である、請求項1~請求項5のいずれか1項に記載の表面被覆切削工具。
- 前記α-Al2O3層は、平均層厚が1~15μmである、請求項1~請求項6のいずれか1項に記載の表面被覆切削工具。
- 前記被膜は、その表面にTiの炭化物、窒化物または硼化物のいずれかを主成分とする最表面層が配置されている、請求項1~請求項7のいずれか1項に記載の表面被覆切削工具。
- 前記被膜は、前記α-Al2O3層と前記基材との間に、中間層を有し、
前記中間層は、針状のTiCNOまたは針状のTiBNを含み、かつ平均層厚が0.3~1μmであり、
前記中間層の最大厚みと最小厚みとの差が0.3μm以上である、請求項1~請求項8のいずれか1項に記載の表面被覆切削工具。 - 請求項1~請求項9のいずれか1項に記載の表面被覆切削工具の製造方法であって、
前記基材上にCVD法で前記α-Al2O3層を含む前記被膜を形成する工程を含み、
該工程において、前記α-Al2O3層の形成初期における原料ガスに含まれるH2Sガスの配合量を0.5~5体積%とし、瞬間的に前記配合量を0.65~7体積%に高める、表面被覆切削工具の製造方法。
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CN106660139A (zh) | 2017-05-10 |
JP5872746B1 (ja) | 2016-03-01 |
KR20180045764A (ko) | 2018-05-04 |
EP3342511A4 (en) | 2018-07-11 |
CN106660139B (zh) | 2020-02-18 |
KR102216097B1 (ko) | 2021-02-15 |
US20170209936A1 (en) | 2017-07-27 |
JPWO2017037798A1 (ja) | 2017-08-31 |
EP3342511B1 (en) | 2021-12-29 |
EP3342511A1 (en) | 2018-07-04 |
US10058924B2 (en) | 2018-08-28 |
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