JP7019093B2 - 立方晶窒化硼素焼結体、及び、その製造方法 - Google Patents
立方晶窒化硼素焼結体、及び、その製造方法 Download PDFInfo
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- JP7019093B2 JP7019093B2 JP2021503616A JP2021503616A JP7019093B2 JP 7019093 B2 JP7019093 B2 JP 7019093B2 JP 2021503616 A JP2021503616 A JP 2021503616A JP 2021503616 A JP2021503616 A JP 2021503616A JP 7019093 B2 JP7019093 B2 JP 7019093B2
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- sintered body
- boron nitride
- cubic boron
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- 229910052582 BN Inorganic materials 0.000 title claims description 95
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 95
- 238000004519 manufacturing process Methods 0.000 title claims description 52
- 239000000843 powder Substances 0.000 claims description 191
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 108
- 229910052799 carbon Inorganic materials 0.000 claims description 108
- 239000002245 particle Substances 0.000 claims description 104
- 239000011230 binding agent Substances 0.000 claims description 69
- 238000000034 method Methods 0.000 claims description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 38
- 150000001875 compounds Chemical class 0.000 claims description 35
- 239000011812 mixed powder Substances 0.000 claims description 31
- 239000000126 substance Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 19
- 239000001301 oxygen Substances 0.000 claims description 19
- 229910052760 oxygen Inorganic materials 0.000 claims description 19
- 238000005245 sintering Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 13
- 229910052796 boron Inorganic materials 0.000 claims description 13
- 229910021480 group 4 element Inorganic materials 0.000 claims description 13
- 229910021478 group 5 element Inorganic materials 0.000 claims description 13
- 229910021476 group 6 element Inorganic materials 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 13
- 230000000737 periodic effect Effects 0.000 claims description 12
- 238000009832 plasma treatment Methods 0.000 claims description 9
- 239000006104 solid solution Substances 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 description 38
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 27
- 238000004458 analytical method Methods 0.000 description 25
- 239000000463 material Substances 0.000 description 23
- 238000002360 preparation method Methods 0.000 description 23
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 18
- 239000010936 titanium Substances 0.000 description 16
- 239000007789 gas Substances 0.000 description 13
- 239000011651 chromium Substances 0.000 description 12
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 10
- 239000005416 organic matter Substances 0.000 description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 229910052750 molybdenum Inorganic materials 0.000 description 9
- 239000011733 molybdenum Substances 0.000 description 9
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 8
- 229910052804 chromium Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 229910052735 hafnium Inorganic materials 0.000 description 8
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- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 7
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 7
- 229910052721 tungsten Inorganic materials 0.000 description 7
- 239000010937 tungsten Substances 0.000 description 7
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000013507 mapping Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910010037 TiAlN Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000007872 degassing Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000000691 measurement method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 4
- 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 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- 230000000007 visual effect Effects 0.000 description 4
- 229910000760 Hardened steel Inorganic materials 0.000 description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- NMJKIRUDPFBRHW-UHFFFAOYSA-N titanium Chemical compound [Ti].[Ti] NMJKIRUDPFBRHW-UHFFFAOYSA-N 0.000 description 3
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910026551 ZrC Inorganic materials 0.000 description 2
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- GPBUGPUPKAGMDK-UHFFFAOYSA-N azanylidynemolybdenum Chemical compound [Mo]#N GPBUGPUPKAGMDK-UHFFFAOYSA-N 0.000 description 2
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- -1 hafnium nitride Chemical class 0.000 description 2
- WHJFNYXPKGDKBB-UHFFFAOYSA-N hafnium;methane Chemical compound C.[Hf] WHJFNYXPKGDKBB-UHFFFAOYSA-N 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 description 2
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052702 rhenium Inorganic materials 0.000 description 2
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910003468 tantalcarbide Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- KREHIIWCKNFTNC-UHFFFAOYSA-N [Cr].[Ti].[Ti] Chemical compound [Cr].[Ti].[Ti] KREHIIWCKNFTNC-UHFFFAOYSA-N 0.000 description 1
- QAKIDWGXFZCSRP-UHFFFAOYSA-N [Ti].[Mo].[Ti] Chemical compound [Ti].[Mo].[Ti] QAKIDWGXFZCSRP-UHFFFAOYSA-N 0.000 description 1
- YSTWCCHWWMEAKP-UHFFFAOYSA-N [Ti].[V].[Ti] Chemical compound [Ti].[V].[Ti] YSTWCCHWWMEAKP-UHFFFAOYSA-N 0.000 description 1
- GGPQWIMALBOMEF-UHFFFAOYSA-N [Ti].[Zr].[Ti] Chemical compound [Ti].[Zr].[Ti] GGPQWIMALBOMEF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- DJPURDPSZFLWGC-UHFFFAOYSA-N alumanylidyneborane Chemical compound [Al]#B DJPURDPSZFLWGC-UHFFFAOYSA-N 0.000 description 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- CXOWYMLTGOFURZ-UHFFFAOYSA-N azanylidynechromium Chemical compound [Cr]#N CXOWYMLTGOFURZ-UHFFFAOYSA-N 0.000 description 1
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 description 1
- HGHPQUIZVKPZEU-UHFFFAOYSA-N boranylidynezirconium Chemical compound [B].[Zr] HGHPQUIZVKPZEU-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- CNEOGBIICRAWOH-UHFFFAOYSA-N methane;molybdenum Chemical compound C.[Mo] CNEOGBIICRAWOH-UHFFFAOYSA-N 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- CGZLUZNJEQKHBX-UHFFFAOYSA-N titanium tungsten Chemical compound [Ti][Ti][W] CGZLUZNJEQKHBX-UHFFFAOYSA-N 0.000 description 1
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
前記結合相は、周期律表の第4族元素、第5族元素、第6族元素及びアルミニウムからなる群より選ばれる少なくとも1種の元素と、窒素、炭素、硼素及び酸素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、及び、前記化合物由来の固溶体からなる群より選ばれる少なくとも1種を含み、
TEM-EDXを用いて前記立方晶窒化硼素粒子と前記結合相との界面に垂直な方向に、前記立方晶窒化硼素粒子から前記結合相にわたって炭素含有量を測定した場合、前記結合相の炭素含有量の平均値よりも炭素含有量の大きい第1領域が存在し、前記第1領域内に前記界面が存在し、かつ、前記第1領域の長さは0.1nm以上10nm以下である、立方晶窒化硼素焼結体である。
立方晶窒化硼素粉末に有機物を付着させて、有機物付着立方晶窒化硼素粉末を作製する工程と、
前記有機物付着立方晶窒化硼素粉末と結合材粉末とを混合して、混合粉末を調製する工程と、
前記混合粉末を焼結して、立方晶窒化硼素焼結体を得る工程と、を備え、
前記混合粉末は、20体積%以上80体積%未満の前記有機物付着立方晶窒化硼素粉末と、20体積%超80体積%以下の前記結合材粉末とを含み、
前記結合材粉末は、周期律表の第4族元素、第5族元素、第6族元素及びアルミニウムからなる群より選ばれる少なくとも1種の元素と、窒素、炭素、硼素及び酸素からなる群より選ばれる少なくとも1種の元素とを含む、立方晶窒化硼素焼結体の製造方法である。
近年、機械部品の急速な高機能化に伴い、機械部品となる被削材の難削化が加速している。これに伴い、切削工具の短寿命化によるコスト増という問題が顕在化している。このため、low-cBN焼結体のさらなる改良が望まれる。
[本開示の効果]
最初に本開示の実施態様を列記して説明する。
(1)本開示の立方晶窒化硼素焼結体は、
20体積%以上80体積%未満の立方晶窒化硼素粒子と、20体積%超80体積%以下の結合相と、を備える立方晶窒化硼素焼結体であって、
前記結合相は、周期律表の第4族元素、第5族元素、第6族元素及びアルミニウムからなる群より選ばれる少なくとも1種の元素と、窒素、炭素、硼素及び酸素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、及び、前記化合物由来の固溶体からなる群より選ばれる少なくとも1種を含み、
TEM-EDXを用いて前記立方晶窒化硼素粒子と前記結合相との界面に垂直な方向に、前記立方晶窒化硼素粒子から前記結合相にわたって炭素含有量を測定した場合、前記結合相の炭素含有量の平均値よりも炭素含有量の大きい第1領域が存在し、前記第1領域内に前記界面が存在し、かつ、前記第1領域の長さは0.1nm以上10nm以下である。
立方晶窒化硼素粉末に有機物を付着させて、有機物付着立方晶窒化硼素粉末を作製する工程と、
前記有機物付着立方晶窒化硼素粉末と結合材粉末とを混合して、混合粉末を調製する工程と、
前記混合粉末を焼結して、立方晶窒化硼素焼結体を得る工程と、を備え、
前記混合粉末は、20体積%以上80体積%未満の前記有機物付着立方晶窒化硼素粉末と、20体積%超80体積%以下の前記結合材粉末とを含み、
前記結合材粉末は、周期律表の第4族元素、第5族元素、第6族元素及びアルミニウムからなる群より選ばれる少なくとも1種の元素と、窒素、炭素、硼素及び酸素からなる群より選ばれる少なくとも1種の元素とを含む。
(b)上記酸素は結合力を低下させるため、該酸素を低減させることで、cBN粒子と結合相との結合力を高め得る。
(c)一方、cBN粒子と結合相との界面に存在する炭素の量が多過ぎると、焼結が阻害され、cBN焼結体が低密度となり、cBN焼結体の特性が変化する傾向がある。
本開示の立方晶窒化硼素焼結体は、20体積%以上80体積%未満の立方晶窒化硼素粒子と、20体積%超80体積%以下の結合相と、を備える立方晶窒化硼素焼結体であって、結合相は、周期律表の第4族元素、第5族元素、第6族元素及びアルミニウムからなる群より選ばれる少なくとも1種の元素と、窒素、炭素、硼素及び酸素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、及び、該化合物由来の固溶体からなる群より選ばれる少なくとも1種を含み、TEM-EDXを用いて立方晶窒化硼素粒子と結合相との界面に垂直な方向に、立方晶窒化硼素粒子から結合相にわたって炭素含有量を測定した場合、結合相の炭素含有量の平均値よりも炭素含有量の大きい第1領域が存在し、第1領域内に前記界面が存在し、かつ、第1領域の長さは0.1nm以上10nm以下である。
二値化処理の具体的な方法について、図1~図6を用いて説明する。
cBN粒子は、硬度、強度、靱性が高く、cBN焼結体中の骨格としての役割を果たす。cBN粒子のD50(平均粒径)は特に限定されず、例えば、0.1~10.0μmとすることができる。通常、D50が小さい方がcBN焼結体の硬度が高くなる傾向があり、粒径のばらつきが小さい方が、cBN焼結体の性質が均質となる傾向がある。cBN粒子のD50は、例えば、0.5~4.0μmとすることが好ましい。
結合相は、難焼結性材料であるcBN粒子を工業レベルの圧力温度で焼結可能とする役割を果たす。また、鉄との反応性がcBNより低いため、高硬度焼入鋼の切削において、化学的摩耗及び熱的摩耗を抑制する働きを付加する。また、cBN焼結体が結合相を含有すると、高硬度焼入鋼の高能率加工における耐摩耗性が向上する。
本開示のcBN焼結体は、TEM-EDX(透過型電子顕微鏡(TEM)付帯のエネルギー分散型X線分光法(EDX))を用いて、cBN粒子と結合相との界面に垂直な方向に、cBN粒子から結合相にわたって炭素含有量を測定した場合に、下記(1)~(3)の条件を満たすことを特徴とする。
(1)結合相の炭素含有量の平均値よりも炭素含有量の大きい第1領域が存在する。
(2)第1領域内に界面が存在する。
(3)第1領域の長さは0.1nm以上10nm以下である。
本開示のcBN焼結体は、工具の材料として用いた場合に、工具の長寿命化を可能とすることができる。この理由は、本開示のcBN焼結体では、cBN粒子と結合相との界面に存在する炭素の量及び分布が適切に調整されていることにより、cBN粒子と結合相との結合力が高められているためと推察される。
本開示のcBN焼結体の製造方法について説明する。本開示のcBN焼結体の製造方法は、第1の実施形態に記載のcBN焼結体の製造方法であり、立方晶窒化硼素粉末(以下、「cBN粉末」ともいう。)に有機物を付着させて、有機物付着立方晶窒化硼素粉末(以下、「有機物付着cBN粉末」ともいう。)を作製する工程(以下、「作製工程」ともいう。)と、有機物付着立方晶窒化硼素粉末と結合材粉末とを混合して、混合粉末を調製する工程(以下、「調製工程」ともいう。)と、混合粉末を焼結して、立方晶窒化硼素焼結体を得る工程(以下、「焼結工程」ともいう。)と、を備える。
本工程は、cBN粉末に有機物を付着させて、有機物付着cBN粉末を作製する工程である。
超臨界水を用いる方法について説明する。当該方法においては、例えば、cBN粉末と有機物とを超臨界水に投入する工程が実施される。これにより、有機物付着cBN粉末を作製することができる。なお本明細書において、超臨界水とは、超臨界状態又は亜臨界状態の水を意味する。
プラズマ処理を実施する方法について説明する。当該方法においては、プラズマ処理により立方晶窒化硼素粉末に有機物を付着させる工程が実施される。例えば、プラズマ発生装置内において、cBN粉末を、炭素を含む第1ガス雰囲気に曝した後、アンモニアを含む第2ガス雰囲気下に曝す方法が挙げられる。第1ガスとしては、CF4、CH4、C2H2等を用いることができる。第2ガスとしては、NH3、N2及びH2の混合ガス等を用いることができる。
本工程は、有機物付着cBN粉末と、結合材粉末とを混合して、混合粉末を調製する工程である。有機物付着cBN粉末は、上述の作製工程により得られた有機物付着cBN粉末であり、結合材粉末は、cBN焼結体の結合相の原料である。
本工程は、混合粉末を焼結してcBN焼結体を得る工程である。本工程において、混合粉末が高温高圧条件下に曝されて焼結されることにより、cBN焼結体が製造される。
本開示のcBN焼結体の製造方法によれば、工具の材料として用いた場合に、工具の長寿命化を可能とすることができるcBN焼結体を製造することができる。その理由は、有機物付着cBN粉末の表面にほぼ均一に存在する炭素が触媒機能を発揮し、これにより、cBN粒子と結合相との界面におけるネックグロスの発生が促進され、結果的に、cBN粒子と結合相との界面における結合力に優れたcBN焼結体が得られるためと推察される。
本開示の立方晶窒化硼素焼結体は、工具の材料として用いることができる。工具は、基材として上記cBN焼結体を含むことができる。また工具は、基材となるcBN焼結体の表面に被膜を有していてもよい。
《作製工程》
まず、有機物付着cBN粉末を作製した。具体的には、まず、超臨界水合成装置(株式会社アイテック社製、「MOMI超mini」)を用いて、以下の条件下で超臨界水を作製した。
圧力:35MPa
温度:375℃
流速:2ml/min
結合材粉末を下記の手順で準備した。チタン(Ti)粉末、アルミニウム(Al)粉末、炭化チタン(TiC)粉末を37:22:41(重量%)で混合し、真空雰囲気下で1500℃、30分熱処理を実施して、概略Ti2AlC組成の結合材化合物を得た。該結合材化合物をボールミル法により、平均粒径0.5μmまで粉砕し第1結合材粉末を作製した。また、第2結合材粉末として炭窒化チタン(TiCN)粉末を準備した。第2結合材粉末と第1結合材粉末とを、重量比で1:3で混合し、結合材粉末を得た。
次に、得られた混合粉末を焼結することにより、cBN焼結体を作製した。具体的には、混合粉末を、Ta製の容器に充填して真空シールし、ベルト型超高圧高温発生装置を用いて、6.5GPa、1700℃で15分間焼結した。これにより、cBN焼結体が作製された。
作製工程において、ヘキシルアミン投入速度を1ml/minとし、調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末60:40の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
作製工程において、ヘキシルアミン投入速度を2ml/minとし、調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末70:30の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
作製工程において、ヘキシルアミン投入速度を3ml/minとし、調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末70:30の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
作製工程において、ヘキシルアミン投入速度を0.1ml/minとし、調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末20:80の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
作製工程において、ヘキシルアミン投入速度を3ml/minとし、調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末79:21の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
作製工程において、ヘキシルアミン投入速度を4ml/minとし、調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末30:70の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
作製工程において、ヘキシルアミン投入速度を4ml/minとし、調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末79:21の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
作製工程において、超臨界水を用いる方法に代えて、プラズマ処理を用いた以外は、試料1と同じ製法で作製した。作製工程は、プラズマ改質装置(Dienner社製、低圧プラズマ装置FEMTO)のチャンバー内にcBN粉末をセットし、真空度:30Pa、電力:1500W、周波数:13.56MHzの条件でCF4ガスを導入して30分処理した。続いて、NH3ガスを導入して30分処理した。これにより、炭素及び窒素が導入された、有機物付着cBN粉末を作製した。
作製工程において、CF4ガス導入後の処理時間を60分に変更した以外は、試料9と同じ製法でcBN焼結体を作製した。
作製工程において、NH3ガス導入後の処理時間を15分に変更した以外は、試料9と同じ製法でcBN焼結体を作製した。
調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末50:50の比率で配合した以外は試料9と同じ製法でcBN焼結体を作製した。
調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末15:85の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末80:20の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
作製工程を行わず、cBN粉末と結合材粉末とを、体積%でcBN粉末:結合材粉末85:15の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
<試料16>
調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末30:70の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
<試料17>
調製工程において、有機物付着cBN粉末と結合材粉末とを、体積%で有機物付着cBN粉末:結合材粉末75:25の比率で配合した以外は試料1と同じ製法でcBN焼結体を作製した。
《cBN粒子及び結合相の含有割合》
試料1~試料17のcBN焼結体について、cBN粒子及び結合相のそれぞれの含有割合(体積%)を走査電子顕微鏡(SEM)付帯のエネルギー分散型X線分析装置(EDX)を用いて測定した。具体的な測定方法は第1の実施形態に記載されているため、その説明は繰り返さない。結果を表1の「cBN粒子含有割合(体積%)」、「結合相含有割合(体積%)」の欄に示す。
試料1~試料17のcBN焼結体について、結合相の組成をXRD(X線回折測定)及びICP用いて測定した。具体的な測定方法は第1の実施形態に記載されているため、その説明は繰り返さない。
試料1~試料17のcBN焼結体について、第1領域の長さ(以下、「第1領域の長さ」ともいう。)、第1領域の炭素含有量の最大値、及び、結合相の炭素含有量の平均値を、TEM-EDXによる元素マッピング分析及び元素ライン分析により測定した。具体的な測定方法は第1の実施形態に記載されているため、その説明は繰り返さない。なお、サンプルの厚みは50nmとし、EDXにおけるビーム径は0.2nmとし、スキャン間隔は0.6nmとした。
試料1~試料17のcBN焼結体を用いて切削工具(基材形状:CNGA120408、刃先処理T01215)を作製した。これを用いて、下記の切削条件下で切削試験を実施した。
切削速度:170m/min.
送り速度:0.2mm/rev.
切込み:0.16mm
クーラント:DRY
切削方法:断続切削
旋盤:LB400(オークマ株式会社製)
被削材:SKD11
試料1~試料12のcBN焼結体の製造方法は、実施例に該当する。試料1~試料12のcBN焼結体は実施例に該当する。試料1~試料12のcBN焼結体を用いた工具は、切削距離が長く、工具寿命が長かった。
試料16のcBN焼結体は、第1領域の長さが0.1nm未満であり、比較例に該当する。試料16のcBN焼結体を用いた工具は、切削距離が短く、工具寿命が短かった。
試料17のcBN焼結体は、第1領域の長さが10nm超であり、比較例に該当する。試料17のcBN焼結体を用いた工具は、切削距離が短く、工具寿命が短かった。
Claims (6)
- 20体積%以上80体積%未満の立方晶窒化硼素粒子と、20体積%超80体積%以下の結合相と、を備える立方晶窒化硼素焼結体であって、
前記結合相は、周期律表の第4族元素、第5族元素、第6族元素及びアルミニウムからなる群より選ばれる少なくとも1種の元素と、窒素、炭素、硼素及び酸素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、及び、前記化合物由来の固溶体からなる群より選ばれる少なくとも1種を含み、
TEM-EDXを用いて前記立方晶窒化硼素粒子と前記結合相との界面に垂直な方向に、前記立方晶窒化硼素粒子から前記結合相にわたって炭素含有量を測定した場合、前記結合相の炭素含有量の平均値よりも炭素含有量の大きい第1領域が存在し、前記第1領域内に前記界面が存在し、かつ、前記第1領域の長さは0.1nm以上10nm以下であり、
前記第1領域の炭素含有量の最大値と、前記結合相の炭素含有量の平均値との差は、0.3原子%以上5原子%以下である、立方晶窒化硼素焼結体。 - 前記立方晶窒化硼素粒子の含有割合は、35体積%以上75体積%未満である、請求項1に記載の立方晶窒化硼素焼結体。
- 前記第1領域の長さは、0.1nm以上5nm以下である、請求項1又は請求項2に記載の立方晶窒化硼素焼結体。
- 請求項1から請求項3のいずれか1項に記載の立方晶窒化硼素焼結体の製造方法であって、
立方晶窒化硼素粉末に有機物を付着させて、有機物付着立方晶窒化硼素粉末を作製する工程と、
前記有機物付着立方晶窒化硼素粉末と結合材粉末とを混合して、混合粉末を調製する工程と、
前記混合粉末を焼結して、立方晶窒化硼素焼結体を得る工程と、を備え、
前記混合粉末は、20体積%以上80体積%未満の前記有機物付着立方晶窒化硼素粉末と、20体積%超80体積%以下の前記結合材粉末とを含み、
前記結合材粉末は、周期律表の第4族元素、第5族元素、第6族元素及びアルミニウムからなる群より選ばれる少なくとも1種の元素と、窒素、炭素、硼素及び酸素からなる群より選ばれる少なくとも1種の元素とを含む、立方晶窒化硼素焼結体の製造方法。 - 前記有機物付着立方晶窒化硼素粉末を作製する工程は、前記立方晶窒化硼素粉末と、前記有機物とを、超臨界水に投入する工程を含む、請求項4に記載の立方晶窒化硼素焼結体の製造方法。
- 前記有機物付着立方晶窒化硼素粉末を作製する工程は、プラズマ処理により前記立方晶窒化硼素粉末に前記有機物を付着させる工程を含む、請求項4に記載の立方晶窒化硼素焼結体の製造方法。
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