WO2022244242A1 - 切削工具 - Google Patents
切削工具 Download PDFInfo
- Publication number
- WO2022244242A1 WO2022244242A1 PCT/JP2021/019380 JP2021019380W WO2022244242A1 WO 2022244242 A1 WO2022244242 A1 WO 2022244242A1 JP 2021019380 W JP2021019380 W JP 2021019380W WO 2022244242 A1 WO2022244242 A1 WO 2022244242A1
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- WIPO (PCT)
- Prior art keywords
- layer
- alumina layer
- titanium compound
- alumina
- cutting tool
- Prior art date
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- 238000005520 cutting process Methods 0.000 title claims abstract description 147
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 182
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 103
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000000576 coating method Methods 0.000 claims abstract description 49
- 239000011248 coating agent Substances 0.000 claims abstract description 46
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 39
- 239000010936 titanium Substances 0.000 claims abstract description 31
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000758 substrate Substances 0.000 claims description 63
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 19
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 abstract description 55
- 239000010410 layer Substances 0.000 description 346
- 239000007789 gas Substances 0.000 description 75
- 238000005259 measurement Methods 0.000 description 37
- 238000000034 method Methods 0.000 description 28
- 238000005229 chemical vapour deposition Methods 0.000 description 27
- 239000000203 mixture Substances 0.000 description 23
- 238000011156 evaluation Methods 0.000 description 16
- 239000002344 surface layer Substances 0.000 description 16
- 239000002994 raw material Substances 0.000 description 15
- 229910002091 carbon monoxide Inorganic materials 0.000 description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 239000000470 constituent Substances 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 6
- 238000005422 blasting Methods 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000012159 carrier gas Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000000992 sputter etching Methods 0.000 description 3
- 238000012935 Averaging Methods 0.000 description 2
- 229910000997 High-speed steel Inorganic materials 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910009043 WC-Co Inorganic materials 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- -1 carbonitrides Chemical class 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000011195 cermet Substances 0.000 description 2
- 239000010730 cutting oil Substances 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910033181 TiB2 Inorganic materials 0.000 description 1
- 229910010060 TiBN Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
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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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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0664—Carbonitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0676—Oxynitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—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
- 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
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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
- C23C16/34—Nitrides
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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
- C23C28/042—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 including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
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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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- 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
- C23C28/048—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 with layers graded in composition or physical properties
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 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 11 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 layer of titanium carbonitride oxide adjacent to the first alumina layer.
- 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 adhesion 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 11 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 layer of titanium carbonitride oxide adjacent to the first alumina layer.
- the above-described cutting tool is improved in wear resistance and adhesion resistance by being provided with the configuration described above.
- wear resistance means resistance to abrasion of the coating when used for cutting.
- adhesion resistance means resistance to adhesion between a cutting tool and a work material, resulting in peeling 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 adhesion resistance.
- 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 11.5 ⁇ 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 ⁇ m or more and 21 ⁇ 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 adhesion 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 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.
- the notation of the form "X to Z” means the upper and lower limits of the range (that is, X to Z or less). and the unit of Z are the same.
- 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.
- 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 11 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 layer of titanium carbonitride oxide adjacent to the first alumina 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 11 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 layer of titanium carbonitride oxide adjacent to the first alumina layer), and furthermore, the titanium compound The layer can be endowed with certain mechanical properties.
- 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 ⁇ m or more and 21 ⁇ 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 layer of titanium carbonitride oxide (TiCNO) adjacent to the first alumina layer.
- TiCNO titanium carbonitride oxide
- the titanium carbonitride oxide layer is provided directly above the first alumina layer.
- the titanium compound layer may be composed only of a layer of titanium carbonitride oxide adjacent to the first alumina layer, or may be composed of a layer of titanium carbonitride oxide adjacent to the first alumina layer and another titanium compound. It may be composed of layers.
- the layer of titanium carbonitride oxide may be composed only of titanium carbonitride oxide, or may be composed of titanium carbonitride oxide and unavoidable impurities. Examples of the inevitable impurities include oxygen and chlorine.
- the thickness of the titanium compound layer is preferably 1 ⁇ m or more and 11.5 ⁇ 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 thickness of the titanium carbonitride oxide layer is preferably 1 ⁇ m or more and 11.5 ⁇ m or less, more preferably 1.5 ⁇ m or more and 9.5 ⁇ m or less, and 3.0 ⁇ m or more and 8.0 ⁇ m or less. is more preferred.
- the thickness of the titanium carbonitride oxide layer can be confirmed by observing vertical cross sections of the base material and the coating using an SEM in the same manner as described above.
- 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 oxide
- 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 impart 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 “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 titanium carbonitride oxide layer is formed directly on the first alumina layer.
- 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 titanium carbonitride oxide layer is formed directly on the first alumina layer.
- a mixed gas of TiCl 4 , CH 4 , N 2 , and CO, for example, is used as the raw material gas for the titanium carbonitride oxide layer.
- 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 3.5 to 5.5% by volume.
- a preferred flow rate for TiCl 4 is 1.4-4.9 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 L/min.
- the content of N 2 in the source gas is preferably 5 to 35% by volume, more preferably 7.5 to 30% by volume, even more preferably 10 to 25% by volume.
- a preferred flow rate for N 2 is 3.5 to 24.5 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 950-1000.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.
- a layer of titanium nitride, titanium carbide, titanium carbonitride, or the like may be formed as a layer constituting a titanium compound layer in addition to the titanium carbonitride oxide layer in the third step. good.
- ⁇ 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 (11.5)/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 (11.5 ⁇ 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 then the subsequent third step was performed.
- 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” (early stage) and “crystal growth” (middle stage) without using the raw material 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 titanium carbonitride oxide layer was formed directly on the first alumina 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.
- the compositions of the titanium compound layers are listed in order from the first alumina layer.
- the notation "TiCNO (6.0)/TiN (1.0)" means a TiCNO layer (thickness 6.0 ⁇ m) and a TiN layer (thickness 1 .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.
- 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 12 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 13.5 minutes in cutting evaluation 1, and had wear resistance and adhesion resistance. could not be reconciled.
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Abstract
Description
基材と上記基材の上に設けられている被膜とを備える切削工具であって、
上記被膜は、
上記基材の上に設けられている第一アルミナ層と、
上記第一アルミナ層の直上に設けられているチタン化合物層と、
上記チタン化合物層の直上に設けられている第二アルミナ層と、を含み、
上記第一アルミナ層において上記チタン化合物層に隣接する部分は界面領域を成し、
上記第一アルミナ層において上記界面領域ではない部分は非界面領域を成し、
上記界面領域における窒素の含有割合は、0.2at%以上11at%以下であり、
上記非界面領域における窒素の含有割合は、0at%以上0.15at%以下であり、
上記チタン化合物層は、上記第一アルミナ層に隣接する炭窒酸化チタンの層を含む。
特許文献1及び特許文献2では、上記のような構成の被膜を有することにより、耐摩耗性、及び酸化アルミニウム層と当該酸化アルミニウム層に接する他の層との間の密着性が向上し、以って切削工具の寿命が長くなることが期待されている。
本開示によれば、耐摩耗性及び耐溶着性が向上した切削工具を提供することが可能になる。
最初に本開示の実施態様を列記して説明する。
基材と上記基材の上に設けられている被膜とを備える切削工具であって、
上記被膜は、
上記基材の上に設けられている第一アルミナ層と、
上記第一アルミナ層の直上に設けられているチタン化合物層と、
上記チタン化合物層の直上に設けられている第二アルミナ層と、を含み、
上記第一アルミナ層において上記チタン化合物層に隣接する部分は界面領域を成し、
上記第一アルミナ層において上記界面領域ではない部分は非界面領域を成し、
上記界面領域における窒素の含有割合は、0.2at%以上11at%以下であり、
上記非界面領域における窒素の含有割合は、0at%以上0.15at%以下であり、
上記チタン化合物層は、上記第一アルミナ層に隣接する炭窒酸化チタンの層を含む。
上記切削工具は旋削加工等の切削加工に用いられるが、旋削加工で一番高温になるのは、切削工具のエッジ部分(刃先稜線部)ではなくてエッジから少し離れた部分(切りくずが接触する部分)であることが知られている。この場合、エッジ部分は高硬度が求められるが、エッジから少し離れた部分では耐熱性、耐溶着性が求められる。しかし、切削工具のエッジと、エッジから離れた部分それぞれに求められる性質を考慮して被膜を設計したことはこれまでになかった。本開示では、第一アルミナ層の更に上にチタン化合物層と第二アルミナ層とを設けることで、切削工具のエッジと、エッジから離れた部分それぞれに求められる性質を両立することに成功した。
以下、本開示の一実施形態(以下「本実施形態」と記す。)について説明する。ただし、本実施形態はこれに限定されるものではない。本明細書において「X~Z」という形式の表記は、範囲の上限下限(すなわちX以上Z以下)を意味し、Xにおいて単位の記載がなく、Zにおいてのみ単位が記載されている場合、Xの単位とZの単位とは同じである。さらに、本明細書において、例えば「TiC」等のように、構成元素の組成比が限定されていない化学式によって化合物が表された場合には、その化学式は従来公知のあらゆる組成比(元素比)を含むものとする。このとき上記化学式は、化学量論組成のみならず、非化学量論組成も含むものとする。例えば「TiC」の化学式には、化学量論組成「Ti1C1」のみならず、例えば「Ti1C0.8」のような非化学量論組成も含まれる。このことは、「TiC」以外の化合物の記載についても同様である。
本開示に係る切削工具は、
基材と上記基材の上に設けられている被膜とを備える切削工具であって、
上記被膜は、
上記基材の上に設けられている第一アルミナ層と、
上記第一アルミナ層の直上に設けられているチタン化合物層と、
上記チタン化合物層の直上に設けられている第二アルミナ層と、を含み、
上記第一アルミナ層において上記チタン化合物層に隣接する部分は界面領域を成し、
上記第一アルミナ層において上記界面領域ではない部分は非界面領域を成し、
上記界面領域における窒素の含有割合は、0.2at%以上11at%以下であり、
上記非界面領域における窒素の含有割合は、0at%以上0.15at%以下であり、
上記チタン化合物層は、上記第一アルミナ層に隣接する炭窒酸化チタンの層を含む。
本実施形態の基材は、この種の基材として従来公知のものであればいずれの基材も使用することができる。例えば、上記基材は、超硬合金(例えば、炭化タングステン(WC)基超硬合金、WCの他にCoを含む超硬合金、WCの他にCr、Ti、Ta、Nb等の炭窒化物を添加した超硬合金等)、サーメット(TiC、TiN、TiCN等を主成分とするもの)、高速度鋼、セラミックス(炭化チタン、炭化珪素、窒化珪素、窒化アルミニウム、酸化アルミニウム等)、立方晶型窒化硼素焼結体(cBN焼結体)及びダイヤモンド焼結体からなる群より選ばれる少なくとも1種を含むことが好ましく、超硬合金、サーメット及びcBN焼結体からなる群より選ばれる少なくとも1種を含むことがより好ましい。
本実施形態に係る被膜40は、上記基材10の上に設けられている第一アルミナ層20と、上記第一アルミナ層20の直上に設けられているチタン化合物層21と、上記チタン化合物層21の直上に設けられている第二アルミナ層22と、を含む(図2参照)。「被膜」は、上記基材の少なくとも一部(例えば、切削加工時に被削材と接するすくい面等)を被覆することで、切削工具における耐欠損性、耐摩耗性、耐溶着性等の諸特性を向上させる作用を有するものである。上記被膜は、上記基材の一部に限らず上記基材の全面を被覆することが好ましい。しかしながら、上記基材の一部が上記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実施形態の範囲を逸脱するものではない。
本実施形態における第一アルミナ層20は、上記基材10の上に設けられている。ここで「基材の上に設けられている」とは、基材の直上に設けられている態様(図2参照)に限られず、他の層を介して基材の上に設けられている態様(図3参照)も含まれる。すなわち、上記第一アルミナ層は、本開示の効果が奏する限りにおいて、上記基材の直上に設けられていてもよいし、後述する下地層等の他の層を介して上記基材の上に設けられていてもよい。
上記第一アルミナ層において上記チタン化合物層に隣接する部分は界面領域を成す。また、上記第一アルミナ層において上記界面領域ではない部分は非界面領域を成す。上記第一アルミナ層の上記界面領域は、上記チタン化合物層との界面Sと、上記界面Sから厚さ方向に0.5μm離れた地点を通る上記界面Sに平行な仮想平面Aとに挟まれた領域であることが好ましい(図4)。上記第一アルミナ層の上記非界面領域は、上記仮想平面Aと、上記第一アルミナ層の基材側の界面Qとに挟まれた領域であることが好ましい(図4)。なお、上記第一アルミナ層において、上記界面領域と上記非界面領域との間には、明確な境界が存在していてもよいし、存在していなくてもよい。
本開示では、第一アルミナ層の界面領域に窒素原子が偏在することでチタン化合物層(特に第一アルミナ層に隣接する炭窒酸化チタンの層)との密着性が向上し、さらに当該チタン化合物層に所定の機械的特性を付することができる。
(AES法の測定条件)
測定加速電圧:10kV
測定電流 :10mA
試料傾斜角度:30°
スパッタ電圧:1kV
本実施形態に係るチタン化合物層21は、上記第一アルミナ層20の直上に設けられている(図2)。上記チタン化合物層は、上記第一アルミナ層に隣接する炭窒酸化チタン(TiCNO)の層を含む。本実施形態の一側面において、上記炭窒酸化チタンの層は、上記第一アルミナ層の直上に設けられていると把握することもできる。上記チタン化合物層は、上記第一アルミナ層に隣接する炭窒酸化チタンの層のみから構成されていてもよいし、上記第一アルミナ層に隣接する炭窒酸化チタンの層と他のチタン化合物の層とから構成されていてもよい。上記炭窒酸化チタンの層は、炭窒酸化チタンのみから構成されていてもよいし、炭窒酸化チタン及び不可避不純物から構成されていてもよい。上記不可避不純物としては、例えば、酸素、塩素等が挙げられる。チタン化合物層の厚さは、1μm以上11.5μm以下であることが好ましく、1.5μm以上9.5μm以下であることがより好ましく、2.5μm以上8.5μm以下であることが更に好ましい。上記チタン化合物層は、従来よりも厚さが薄い。しかし、後述するように上記チタン化合物層は所定の残留応力を有するため、十分な硬度を有する層となっている。チタン化合物層の厚さは、上述したのと同様の方法で、SEMを用いて基材と被膜の垂直断面を観察することにより確認することができる。
装置 :SmartLab(株式会社リガク製)
X線 :Cu/Kα/45kV/200mA
カウンタ:D/teX Ultra250(株式会社リガク製)
測定回折面:(331)面
走査範囲:72°~74°(傾斜法)
本実施形態における第二アルミナ層22は、上記チタン化合物層21の直上に設けられている。上記第二アルミナ層は、その上に表面層等の他の層が設けられていてもよい。また、上記第二アルミナ層は、上記被膜の最表面であってもよい。上記第二アルミナ層は、酸化アルミニウム(Al2O3)のみから構成されていてもよいし、酸化アルミニウム及び不可避不純物から構成されていてもよい。上記不可避不純物としては、例えば、塩素、硫黄等が挙げられる。上記酸化アルミニウムは、α型の酸化アルミニウム(α-Al2O3)であることが好ましい。上記第二アルミナ層は、上記第一アルミナ層と組成が同じであってもよいし、異なっていてもよい。第二アルミナ層の厚さは、0.2μm以上6.5μm以下であることが好ましく、0.5μm以上5μm以下であることがより好ましく、1μm以上4.5μm以下であることが更に好ましい。上記第二アルミナ層は、従来よりも厚さが薄い。しかし、上記第二アルミナ層が薄いことで、後述するように第二アルミナ層を形成した後にブラスト処理を行うことで上記チタン化合物層に所定の残留応力を付与することが可能になる。第二アルミナ層の厚さは、上述したのと同様の方法で、SEMを用いて基材と被膜の垂直断面を観察することにより確認することができる。
上記被膜40は、上記基材10と上記第一アルミナ層20との間に設けられている下地層23を更に含むことが好ましい(図3参照)。上記下地層23は、窒化チタン(TiN)、炭窒化チタン(TiCN)又は炭窒酸化チタン(TiCNO)を含むことが好ましい。上記TiN、TiCN及びTiCNOそれぞれは、立方晶であることが好ましい。
上記被膜は、上記第二アルミナ層上に設けられている表面層を更に含むことが好ましい。上記表面層は、チタン元素と、C、N及びBからなる群より選ばれる少なくとも1種の元素とからなる化合物を含むことが好ましい。
本実施形態に係る切削工具が奏する効果を損なわない範囲において、上記被膜は、他の層を更に含んでいてもよい。上記他の層は、上記第一アルミナ層、上記チタン化合物層、上記第二アルミナ層、上記下地層又は上記表面層とは組成が異なっていてもよいし、同じであってもよい。他の層に含まれる化合物としては、例えば、TiN、TiCN、TiBN及びAl2O3等を挙げることができる。なお、上記他の層は、その積層の順も特に限定されない。上記他の層の厚さは、本実施形態の効果を損なわない範囲において、特に制限はないが例えば、0.1μm以上20μm以下が挙げられる。
本実施形態に係る切削工具の製造方法は、
上記基材を準備する第1工程(以下、単に「第1工程」という場合がある。)と、
化学気相蒸着法で、上記基材上に上記第一アルミナ層を形成する第2工程(以下、単に「第2工程」という場合がある。)と、
化学気相蒸着法で、上記第一アルミナ層の直上に上記チタン化合物層を形成する第3工程(以下、単に「第3工程」という場合がある。)と、
化学気相蒸着法で、上記チタン化合物層の直上に上記第二アルミナ層を形成する第4工程(以下、単に「第4工程」という場合がある。)と、
を含み、
上記第2工程の終盤において、アルミニウムを構成元素として含むガス、窒素を構成元素として含むガス及び酸素を構成元素として含むガスを含む原料ガスを用いて、上記第一アルミナ層を形成させ、
上記第3工程において、上記第一アルミナ層の直上に炭窒酸化チタンの層を形成させる。
第1工程では基材を準備する。例えば、基材として超硬合金基材が準備される。超硬合金基材は、市販品を用いてもよく、一般的な粉末冶金法で製造してもよい。一般的な粉末冶金法で製造する場合、例えば、ボールミル等によってWC粉末とCo粉末等とを混合して混合粉末を得る。該混合粉末を乾燥した後、所定の形状に成形して成形体を得る。さらに該成形体を焼結することにより、WC-Co系超硬合金(焼結体)を得る。次いで該焼結体に対して、ホーニング処理等の所定の刃先加工を施すことにより、WC-Co系超硬合金からなる基材を製造することができる。第1工程では、上記以外の基材であっても、この種の基材として従来公知の基材であればいずれも準備可能である。
第2工程では、化学気相蒸着法(CVD法)で、上記基材上に第一アルミナ層を形成する。また、上記第2工程の終盤において、アルミニウムを構成元素として含むガス、窒素を構成元素として含むガス及び酸素を構成元素として含むガスを含む原料ガスを用いて、上記第一アルミナ層を形成させる。
第3工程では、化学気相蒸着法で、上記第一アルミナ層の直上に上記チタン化合物層を形成する。上記第3工程において、上記第一アルミナ層の直上に炭窒酸化チタンの層を形成させる。
第4工程では、化学気相蒸着法で、上記チタン化合物層の直上に第二アルミナ層を形成する。
本実施形態に係る製造方法では、上述した工程の他にも、本実施形態の効果を損なわない範囲で追加工程を適宜行ってもよい。上記追加工程としては例えば、上記第二アルミナ層上に表面層を形成する工程、及び被膜にブラスト処理を行う工程等が挙げられる。本実施形態において、チタン化合物層の直上にある第二アルミナ層の厚さは、第一アルミナ層の厚さよりも薄い。そのため、上記第4工程の後で、ブラスト処理を行うと上記チタン化合物層に所定の圧縮残留応力を付与することができる。ブラスト処理の条件は、例えば後述する実施例に記載の条件が挙げられる。表面層を形成する方法としては、特に制限はなく、例えば、CVD法等によって形成する方法が挙げられる。
<第1工程:基材を準備する工程>
基材として、TaC(2.0質量%)、NbC(1.0質量%)、Co(10.0質量%)及びWC(残部)からなる組成(ただし不可避不純物を含む。)の超硬合金製切削チップ(形状:CNMG120408N-UX、住友電工ハードメタル株式会社製、JIS B4120(2013))を準備した。
後述の第2工程の前に、準備した基材に対し、CVD装置を用いて、表1に記載の原料ガス組成及び成膜条件で下地層を形成させた。なお、成膜時間は表5に示される厚さとなるように適宜調整した。また、下地層の厚さ及び下地層の組成を表5に示す。表5において、下地層の組成は基材に近い順に記載している。例えば、「TiN(1.0)/TiCN(11.5)/TiCNO(1.5)」との表記は、基材に近い層から順に、TiNの層(厚さ1.0μm)、TiCNの層(厚さ11.5μm)及びTiCNOの層(厚さ1.5μm)が形成されていることを意味する。
準備した基材、又は下地層が形成された基材に対し、CVD装置を用いて、第一アルミナ層を形成させて、後工程の第3工程に移った。第一アルミナ層の形成条件を表2に示す。表2に示されるように、「核生成」(序盤)、「結晶成長」(中盤)、「N含有層形成」(終盤)の各段階に応じて、原料ガスの組成を変化させて第一アルミナ層を成膜した。試料101及び103については、「N含有層形成」(終盤)における原料ガスを用いずに、「核生成」(序盤)、及び「結晶成長」(中盤)の二段階で第一アルミナ層を成膜した。なお、成膜時間は表5に示される厚さとなるように適宜調整した。また、第一アルミナ層の厚さ及び第一アルミナ層の組成を表5に示す。
次に、上記第一アルミナ層が形成された基材に対し、CVD装置を用いて、第一アルミナ層の直上にチタン化合物層を形成した。ここで上記第3工程において、上記第一アルミナ層の直上に炭窒酸化チタンの層を形成させた。チタン化合物層の形成条件を表3に示す。なお、成膜時間は表5に示される厚さとなるように適宜調整した。また、チタン化合物層の厚さ及びチタン化合物層の組成を表5に示す。表5において、チタン化合物層の組成は第一アルミナ層に近い順に記載している。例えば、「TiCNO(6.0)/TiN(1.0)」との表記は、第一アルミナ層に近い層から順に、TiCNOの層(厚さ6.0μm)及びTiNの層(厚さ1.0μm)が形成されていることを意味する。
次に、上記チタン化合物層が形成された基材に対し、CVD装置を用いて、チタン化合物層の直上に第二アルミナ層を形成した。第二アルミナ層の形成条件を表4に示す。なお、成膜時間は表5に示される厚さとなるように適宜調整した。また、第二アルミナ層の厚さ及び第二アルミナ層の組成を表5に示す。
最後に、上記第二アルミナ層が形成された基材に対し、CVD装置を用いて、表面層を形成させた。表面層の形成条件を以下に示す。また、表面層の厚さ及び組成を表5に示す。なお、表5において「-」で示されている箇所は、該当する層が設けられていないことを意味する。
(TiNの場合)
原料ガス組成:TiCl4(7.0vol%)、N2(40.0vol%)、H2(残部)
全ガス流量:60L/min
圧力 :250hPa
温度 :1000℃
(TiCの場合)
原料ガス組成:TiCl4(4.0vol%)、CH4(4.0vol%)、H2(残部)
全ガス流量:50L/min
圧力 :80hPa
温度 :1000℃
最後に、すくい面中央の貫通穴を軸中心として90rpmで、上記切削工具を回転させながら、以下の条件で被膜に対してブラスト処理を行った。
ブラスト処理の条件
メディア:砥粒となる粒径100μmのセラミックス粒子を7体積%含む水溶媒
投射角度:回転軸に対し45°
投射距離:刃先稜線部から10mmの距離
投射圧力:0.05~0.10MPa
投射時間:5~20秒間
投射圧力及び投射時間は、表6に示される残留応力となるように調整した。
上述のようにして作製した試料の切削工具を用いて、以下のように、切削工具の各特性を評価した。ここで、試料1~12は実施例に相当し、試料101~103は比較例に相当する。
被膜を構成する各層の厚さは、電界放出型走査電子顕微鏡(SEM)(株式会社日立ハイテク製、商品名:SU3500)を用いて、基材の表面の法線方向に平行な断面サンプルにおける任意の10点を測定し、測定された10点の厚さの平均値をとることで求めた。このとき上記断面サンプルの測定断面をイオンミリング処理(株式会社日立ハイテク製、商品名:IM4000)により研磨してから測定した。結果を表5、表6に示す。
第一アルミナ層の界面領域及び非界面領域における各元素(酸素、窒素、アルミニウム)の原子割合は、上述の基材の表面の法線方向に平行な断面サンプルに対して、オージェ電子分光法(AES法)によって線分析を行うことで求めた。具体的には、まず、クロスセクションポリッシャ加工によって上記断面サンプルの切断面を研磨した。研磨した切断面に対して、電解放出型走査顕微鏡(FE-SEM)を用いた分析によって下地層、第一アルミナ層及びチタン化合物層における断面SEM像を得た。このときの測定倍率は、50000倍であった。このとき、下地層、及びチタン化合物層が暗い領域として観察され、第一アルミナ層が明るい領域として観察される。次に、上記断面SEM像における視野で、上記チタン化合物層の積層方向に平行な方向でチタン化合物層側から第一アルミナ層側に向かって、上記研磨した切断面に対してAES法によって線分析を行った。このときの測定ピッチは、0.016μmであった。AES法のその他の測定条件は、以下の条件であった。
(AES法の測定条件)
測定装置 :アルバック・ファイ社製、商品名:PHI700
測定加速電圧:10kV
測定電流 :10mA
試料傾斜角度:30°
スパッタ電圧:1kV
上述の2θ-sin2ψ法により、以下の条件でチタン化合物層における残留応力を測定した。結果を表6に示す。表6中、マイナスの数値で表される残留応力は圧縮残留応力を意味し、プラスの数値で表される残留応力は引張残留応力を意味する。
装置 :SmartLab(株式会社リガク製)
X線 :Cu/Kα/45kV/200mA
測定回折面:(331)面
カウンタ:D/teX Ultra250(株式会社リガク製)
走査範囲:72°~74°(傾斜法)
(切削評価1:連続加工試験、耐摩耗性の評価)
上述のようにして作製した試料(試料1~12及び試料101~103)の切削工具を用いて、以下の切削条件により、逃げ面の摩耗量が0.3mmとなるまでの切削時間(分)を測定した。その結果を表6に示す。切削時間が長いほど耐摩耗性に優れる切削工具として評価することができる。
連続加工の切削条件
被削材 :SS400(形状:丸棒)
切削速度:330m/min
送り速度:0.2mm/rev
切込み :1.5mm
切削油 :あり
また上記切削試験において切削加工を開始して1分後における被削材の加工面を目視で観察した。観察した加工面における白濁、むしれの状態を元に図6に示す基準でA~Eのランク付けを行った。結果を表6に示す。ランクA~Cを良好な加工面と評価した。切削評価2を行うことで、切削工具の耐溶着性を評価することができる。
上述のようにして作製した試料(試料1~12及び試料101~103)の切削工具を用いて、以下の切削条件により、溶着による膜剥離を起点としてノーズR部が欠損に至るまでの切削時間(分)を測定した。その結果を表6に示す。切削時間が長いほど耐溶着欠損性に優れる切削工具として評価することができる。
断続加工の切削条件
被削材 :SUS316 断続材(形状:スリット溝付丸棒)
切削速度:120m/min
送り速度:0.15mm/rev
切込み :2.0mm
切削油 :あり
Claims (9)
- 基材と前記基材の上に設けられている被膜とを備える切削工具であって、
前記被膜は、
前記基材の上に設けられている第一アルミナ層と、
前記第一アルミナ層の直上に設けられているチタン化合物層と、
前記チタン化合物層の直上に設けられている第二アルミナ層と、を含み、
前記第一アルミナ層において前記チタン化合物層に隣接する部分は界面領域を成し、
前記第一アルミナ層において前記界面領域ではない部分は非界面領域を成し、
前記界面領域における窒素の含有割合は、0.2at%以上11at%以下であり、
前記非界面領域における窒素の含有割合は、0at%以上0.15at%以下であり、
前記チタン化合物層は、前記第一アルミナ層に隣接する炭窒酸化チタンの層を含む、切削工具。 - 前記第一アルミナ層の厚さは、前記第二アルミナ層の厚さより大きい、請求項1に記載の切削工具。
- 前記チタン化合物層の厚さは、1μm以上11.5μm以下である、請求項1又は請求項2に記載の切削工具。
- 前記第二アルミナ層の厚さは、0.2μm以上6.5μm以下である、請求項1から請求項3のいずれか一項に記載の切削工具。
- 前記第一アルミナ層の厚さは、2μm以上21μm以下である、請求項1から請求項4のいずれか一項に記載の切削工具。
- 前記第一アルミナ層の前記界面領域は、前記チタン化合物層との界面Sと、前記界面Sから厚さ方向に0.5μm離れた地点を通る前記界面Sに平行な仮想平面Aとに挟まれた領域である、請求項5に記載の切削工具。
- 前記第一アルミナ層の前記界面領域における窒素の含有割合は、0.5at%以上10at%以下である、請求項1から請求項6のいずれか一項に記載の切削工具。
- 前記第二アルミナ層の厚さは、0.2μm以上6.5μm以下であり、
前記チタン化合物層の残留応力は、-3GPa以上0GPa以下である、請求項1から請求項7のいずれか一項に記載の切削工具。 - 前記チタン化合物層は、窒化チタン又は炭化チタンの層を更に含む、請求項1から請求項8のいずれか一項に記載の切削工具。
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US20240218504A1 (en) | 2024-07-04 |
JPWO2022244242A1 (ja) | 2022-11-24 |
CN115697600A (zh) | 2023-02-03 |
EP4147809A1 (en) | 2023-03-15 |
EP4147809B1 (en) | 2024-07-03 |
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