JP4381790B2 - Composite material and processing method using the same - Google Patents
Composite material and processing method using the same Download PDFInfo
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- JP4381790B2 JP4381790B2 JP2003413359A JP2003413359A JP4381790B2 JP 4381790 B2 JP4381790 B2 JP 4381790B2 JP 2003413359 A JP2003413359 A JP 2003413359A JP 2003413359 A JP2003413359 A JP 2003413359A JP 4381790 B2 JP4381790 B2 JP 4381790B2
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- 239000002131 composite material Substances 0.000 title claims description 87
- 238000003672 processing method Methods 0.000 title description 12
- 238000005498 polishing Methods 0.000 claims description 189
- 239000000463 material Substances 0.000 claims description 99
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 81
- 239000004917 carbon fiber Substances 0.000 claims description 81
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 70
- 239000006061 abrasive grain Substances 0.000 claims description 61
- 238000005520 cutting process Methods 0.000 claims description 41
- 238000000227 grinding Methods 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 31
- 239000002134 carbon nanofiber Substances 0.000 claims description 29
- 239000004065 semiconductor Substances 0.000 claims description 25
- 229920005989 resin Polymers 0.000 claims description 20
- 239000011347 resin Substances 0.000 claims description 20
- 229910052582 BN Inorganic materials 0.000 claims description 19
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 10
- 239000011229 interlayer Substances 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 10
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 10
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 9
- 229910052796 boron Inorganic materials 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 9
- 238000003754 machining Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000010432 diamond Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
- 229910003460 diamond Inorganic materials 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 6
- 238000001069 Raman spectroscopy Methods 0.000 claims description 5
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 5
- 229910021417 amorphous silicon Inorganic materials 0.000 claims description 4
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 4
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 229910052580 B4C Inorganic materials 0.000 claims description 3
- 238000002441 X-ray diffraction Methods 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 claims description 2
- 239000004640 Melamine resin Substances 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 2
- 239000009719 polyimide resin Substances 0.000 claims description 2
- 229920005749 polyurethane resin Polymers 0.000 claims description 2
- 229920002050 silicone resin Polymers 0.000 claims description 2
- 229920006337 unsaturated polyester resin Polymers 0.000 claims description 2
- 239000004643 cyanate ester Substances 0.000 claims 1
- 239000002585 base Substances 0.000 description 37
- 235000012431 wafers Nutrition 0.000 description 27
- 239000010408 film Substances 0.000 description 26
- 239000000758 substrate Substances 0.000 description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 17
- 229910052710 silicon Inorganic materials 0.000 description 17
- 239000010703 silicon Substances 0.000 description 17
- 230000003746 surface roughness Effects 0.000 description 14
- 239000011230 binding agent Substances 0.000 description 12
- 230000003287 optical effect Effects 0.000 description 12
- 238000005259 measurement Methods 0.000 description 11
- 229910052782 aluminium Inorganic materials 0.000 description 10
- 239000000835 fiber Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 238000007517 polishing process Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000004745 nonwoven fabric Substances 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 150000003623 transition metal compounds Chemical class 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910000760 Hardened steel Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- JXOOCQBAIRXOGG-UHFFFAOYSA-N [B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[Al] Chemical compound [B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[Al] JXOOCQBAIRXOGG-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000002173 cutting fluid Substances 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- KZPXREABEBSAQM-UHFFFAOYSA-N cyclopenta-1,3-diene;nickel(2+) Chemical compound [Ni+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KZPXREABEBSAQM-UHFFFAOYSA-N 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
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- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003698 laser cutting Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
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- 238000000206 photolithography Methods 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
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- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
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- 229920000728 polyester Polymers 0.000 description 1
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- 239000005060 rubber Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は、複合材料及びそれを用いた加工方法に関する。例えば砥粒を含むホイールやブレード、ろう付け切削バイト、スローアウェイチップなどの研削、研磨、切削用の複合材、及びそれらを用いた加工方法に関するものである。さらには、固定砥粒方式による半導体ウェハや層間絶縁膜もしくは配線材料等の電子部品を精密研削もしくは研磨する際に使用する研磨用複合材、及びそれを用いた研削用材料又は研磨用材料、並びにそれらを使用した半導体ウェハ等の電子部品の加工方法にも関する。 The present invention relates to a composite material and a processing method using the same. For example, the present invention relates to a composite material for grinding, polishing, and cutting of wheels and blades containing abrasive grains, brazing cutting tools, throw-away tips, and a processing method using them. Further, a polishing composite material used when precision grinding or polishing an electronic component such as a semiconductor wafer, an interlayer insulating film, or a wiring material by a fixed abrasive method, and a grinding material or a polishing material using the same, and The present invention also relates to a method for processing an electronic component such as a semiconductor wafer using the same.
近年、半導体デバイスの高性能化にともない電子回路の高集積化、微細化が進んでいる。半導体基板表面に高度な配線構造を構築するには、回路パターンを形成するフォトリソグラフィーの微細化限界、すなわち焦点深度が浅くなるという制約を軽減するため、結像面である半導体基板表面を平坦化する行程が重要なプロセスとなる。
通常使用されている化学的機械的研磨方法による平坦化においては、砥粒を研磨液に分散させたスラリーを研磨パッドに流すと同時に、キャリアに保持された基板を回転させながら研磨する方法がある。例えば、絶縁膜研磨用スラリーとしては、二酸化ケイ素（例えば以下の特許文献１参照。）や酸化セリウム（例えば以下の特許文献２参照。）などを研磨液に分散させたものがある。これらの方法では、基板を傷つけないために比較的軟質な研磨パッドが用いられるが、砥粒が研磨パッドに保持されていないことにより研磨速度が遅いという問題点がある。また、回路パターンを転写した基板を研磨する場合には、研磨速度が回路配線の間隔により変化し、ディッシングやシニングといった研磨ムラが発生する難点がある。また、使用済みの砥粒の処理などの問題がある。
In recent years, electronic circuits have been highly integrated and miniaturized with higher performance of semiconductor devices. In order to build an advanced wiring structure on the surface of the semiconductor substrate, the semiconductor substrate surface, which is the imaging plane, is flattened in order to reduce the limitation of photolithography miniaturization that forms circuit patterns, that is, the restriction that the depth of focus is shallow. The process to do is an important process.
In flattening by a commonly used chemical mechanical polishing method, there is a method in which a slurry in which abrasive grains are dispersed in a polishing liquid is passed through a polishing pad, and at the same time, polishing is performed while rotating a substrate held by a carrier. . For example, as the insulating film polishing slurry, there is a slurry in which silicon dioxide (for example, see Patent Document 1 below), cerium oxide (for example, see Patent Document 2 below) or the like is dispersed in a polishing liquid. In these methods, a relatively soft polishing pad is used so as not to damage the substrate, but there is a problem that the polishing rate is slow because the abrasive grains are not held on the polishing pad. Further, when polishing a substrate to which a circuit pattern has been transferred, the polishing rate varies depending on the interval between circuit wirings, and there is a problem that uneven polishing such as dishing and thinning occurs. There are also problems such as processing of used abrasive grains.
上記半導体基板の平坦化の問題点を解決するための別の方法として、砥粒を固着した回転盤に基板を押し当て回転、摺動させながら研磨する方法がある（例えば、以下の特許文献３、４、５等参照。）。この方法では砥粒が固定されているので研磨速度が比較的速いという利点がある。 As another method for solving the problem of flattening of the semiconductor substrate, there is a method of polishing while pressing and rotating and sliding the substrate against a rotating plate to which abrasive grains are fixed (for example, Patent Document 3 below). 4, 5, etc.)). This method has an advantage that the polishing rate is relatively fast because the abrasive grains are fixed.
しかしながら先に記載したような固定式砥粒による研磨の方法では、研磨時にスクラッチと呼ばれる微小キズが発生する問題や、砥粒の脱落による深い研磨痕が発生する問題がある。これらのキズは回路短絡の原因になるため、デバイスの歩留まりの低下を招きやすい。
半導体デバイスの高性能化を達成するためには、基板表面の研磨の精度を向上させ、キズや研磨痕の無い基板の提供が必須要件となる。さらに基板のキズだけでなく、デバイスを構成する層間絶縁膜や回路パターンなども精度良く研磨できる手段が必要となる。
However, the method of polishing with fixed abrasive grains as described above has a problem that micro scratches called scratches occur during polishing and a problem that deep polishing marks are generated due to falling off of the abrasive grains. Since these scratches cause a short circuit, the device yield tends to decrease.
In order to achieve high performance of semiconductor devices, it is essential to improve the polishing accuracy of the substrate surface and to provide a substrate free from scratches and polishing marks. Furthermore, not only scratches on the substrate but also means capable of accurately polishing an interlayer insulating film and a circuit pattern constituting the device are required.
切削分野においては高硬度材料を砥粒に用いた切削工具により、高能率な高速切削が進んでいる。近年は環境問題から切削液を使用しない乾式切削加工法が増えつつある。この場合、工具はより高温になるため熱伝導性のよい材料が好ましく、熱伝導の特に高いダイヤモンドや立方晶ボロンナイトライドなどの含有率を高めた材料が有利である。特に難削材、その中でもステンレス鋼、耐熱鋼、高硬度鋳鉄、焼結合金、焼入れ鋼などの鉄系難削材には立方晶ボロンナイトライドが最適な砥粒である。結合材となる母材がメタルの場合は安価で高能率なワイヤーカット放電加工が可能だが、絶縁性のセラミックスを母材とする材料では導電性が劣り、工具をカット加工する際には高価なレーザーカット加工機が必要となる。切削工具材料の場合は、導電性を付与し、安価で高能率なワイヤーカット放電加工機で加工できることが望まれる。
本発明は、上記事情に鑑みなされたものであって、基板や層間絶縁膜、回路パターン等の表面の研磨精度を向上させ、キズや研磨痕の無い基板が得られる研削材や研磨材若しくは研削方法や研磨方法を提供することを目的とする。
具体的には研削、研磨加工時の砥粒の脱落を抑え、研磨痕の発生を抑制すると同時に砥粒の後処理の負担を軽減させ、寿命の長い研削材や研磨材若しくは研削方法や研磨方法を提供することを目的とする。
さらに、被加工物の研削、研磨の精度を向上させるために、研削材や研磨材に摺動性、弾力性、導電性、熱伝導性、耐食性を付与することで、加工時の物理的、化学的要因の影響を低減することができる研磨用複合材を提供することを目的とする。
The present invention has been made in view of the above circumstances, and improves the polishing accuracy of the surface of a substrate, an interlayer insulating film, a circuit pattern, etc., and provides a grinding material, polishing material, or grinding material that can obtain a substrate without scratches or polishing marks. An object is to provide a method and a polishing method.
Specifically, it suppresses the drop of abrasive grains during grinding and polishing, suppresses the generation of polishing marks, and at the same time reduces the burden of post-treatment of abrasive grains. The purpose is to provide.
Furthermore, in order to improve the accuracy of grinding and polishing of the workpiece, the physical properties at the time of processing can be improved by adding slidability, elasticity, conductivity, thermal conductivity, and corrosion resistance to the abrasive and abrasive. An object of the present invention is to provide a polishing composite capable of reducing the influence of chemical factors.
本発明の他の目的は、これら高性能な研磨用複合材を利用した研削材や研磨材を使用して、半導体基板や電子デバイスを構成する層間絶縁膜や回路パターンを研削、研磨する電子部品の加工方法を提供することである。
特に、多結晶シリコン、単結晶シリコン、アモルファスシリコン等のシリコンを研削、研磨するシリコンの加工方法を提供することを目的とする。
Another object of the present invention is to provide an electronic component for grinding and polishing an interlayer insulating film and a circuit pattern constituting a semiconductor substrate or an electronic device using an abrasive or an abrasive using these high-performance polishing composite materials. It is to provide a processing method.
In particular, an object of the present invention is to provide a silicon processing method for grinding and polishing silicon such as polycrystalline silicon, single crystal silicon, and amorphous silicon.
本発明者らは上記課題を解決するために鋭意研究を行った結果、以下の研磨用複合材及び、その研磨用複合材を使用した砥石、研削材料、研磨材料及び切削工具材料を発明した。さらに、それらの砥石、研削材料又は研磨材料を使用した電子部品の加工方法並びにシリコンの加工方法を発明した。
（１）本発明の研磨用複合材は前記事情に鑑みてなされたもので、外径が２０〜２００ｎｍ、アスペクト比が１０〜１００で中心部に中空構造を有する多層構造の炭素繊維と砥粒と母材とを含み、前記炭素繊維が、研磨用複合材中に２〜４０体積％含有されたものである。
（２）本発明の研磨用複合材は前記事情に鑑みてなされたもので、炭素繊維のＢＥＴ比表面積が４ｍ２／ｇ以上であることを特徴とする。
（３）本発明の研磨用複合材は前記事情に鑑みてなされたもので、炭素繊維のＸ線回折における炭素（００２）面の面間隔（ｄ００２）が０．３４５ｎｍ以下であることを特徴とする。
（４）本発明の研磨用複合材は前記事情に鑑みてなされたもので、炭素繊維のラマン散乱スペクトルにおける１３４１〜１３４９ｃｍ−１のバンドのピーク高さ（Ｉｄ）と１５７０〜１５７８ｃｍ−１のバンドのピーク高さ（Ｉｇ）の比（Ｉｄ／Ｉｇ）が１．５以下であることを特徴とする。
As a result of intensive studies to solve the above-mentioned problems, the present inventors have invented the following abrasive composites and grindstones, grinding materials, abrasive materials and cutting tool materials using the abrasive composites. Furthermore, the processing method of the electronic component which used those grindstones, grinding materials, or polishing materials, and the processing method of silicon were invented.
(1) The polishing composite material of the present invention has been made in view of the above circumstances, and has an outer diameter of 20 to 200 nm, an aspect ratio of 10 to 100 , and a multi-layer structure carbon fiber and abrasive having a hollow structure at the center. The carbon fiber is contained in an abrasive composite material in an amount of 2 to 40% by volume, including grains and a base material.
(2) The polishing composite material of the present invention has been made in view of the above circumstances, and is characterized in that the BET specific surface area of the carbon fiber is 4 m 2 / g or more.
(3) The polishing composite material of the present invention has been made in view of the above circumstances, and the interplanar spacing (d002) of the carbon (002) plane in X-ray diffraction of carbon fiber is 0.345 nm or less. To do.
(4) abrasive composite material of the present invention has been made in view of the above circumstances, the peak height of the band 1341～1349Cm -1 in the Raman scattering spectrum of the carbon fiber (Id) and a band of 1570～1578Cm -1 The ratio (Id / Ig) of the peak height (Ig) is 1.5 or less.
（５）本発明の研磨用複合材は前記事情に鑑みてなされたもので、前記炭素繊維が、分岐状気相法炭素繊維を含む炭素繊維であることを特徴とする。
（６）本発明の研磨用複合材は前記事情に鑑みてなされたもので、前記炭素繊維が、その結晶内に０．０１〜５質量％のホウ素を含有することを特徴とする。
（７）本発明の研磨用複合材は前記事情に鑑みてなされたもので、前記砥粒が、酸化セリウム、酸化ケイ素、シリコンカーバイド、ボロンカーバイド、ボロンナイトライド、酸化ジルコニウム、ダイヤモンド、及びサファイヤから選ばれる少なくとも１種の材料であることを特徴とする。
（８）本発明の研磨用複合材は前記事情に鑑みてなされたもので、前記母材が、樹脂、メタル、セラミックスから選ばれる少なくとも１種の材料であることを特徴とする。
（９）本発明は前記事情に鑑みてなされたもので、前記樹脂が、フェノール樹脂、メラミン樹脂、ポリウレタン樹脂、エポキシ樹脂、尿素樹脂、不飽和ポリエステル樹脂、シリコーン樹脂、ポリイミド樹脂、エポキシ樹脂、シアネートエステル樹脂、及びベンゾオキサジン樹脂から選ばれる少なくとも１種を含む樹脂である。
(5) The polishing composite material of the present invention has been made in view of the above circumstances, and the carbon fiber is a carbon fiber containing a branched vapor grown carbon fiber.
(6) The composite material for polishing according to the present invention is made in view of the above circumstances, and the carbon fiber contains 0.01 to 5% by mass of boron in the crystal.
(7) The polishing composite material of the present invention is made in view of the above circumstances, and the abrasive grains are made of cerium oxide, silicon oxide, silicon carbide, boron carbide, boron nitride, zirconium oxide, diamond, and sapphire. It is characterized by being at least one material selected.
(8) The polishing composite material of the present invention has been made in view of the above circumstances, and the base material is at least one material selected from resin, metal, and ceramics.
(9) The present invention has been made in view of the above circumstances, and the resin is a phenol resin, melamine resin, polyurethane resin, epoxy resin, urea resin, unsaturated polyester resin, silicone resin, polyimide resin, epoxy resin, cyanate. It is resin containing at least 1 sort (s) chosen from ester resin and benzoxazine resin.
（１０）本発明の砥石は前記事情に鑑みてなされたもので、先の（１）〜（９）のいずれかに記載の研磨用複合材を成形加工してなることを特徴とする。
（１１）本発明の研削材料は前記事情に鑑みてなされたもので、先の（１）〜（９）のいずれかに記載の研磨用複合材を用いたことを特徴とする。
（１２）本発明の研磨材料は前記事情に鑑みてなされたもので、先の（１）〜（９）のいずれかに記載の研磨用複合材を用いたことを特徴とする。
（１３）本発明の切削工具材料は前記事情に鑑みてなされたもので、先の（１）〜（９）のいずれかに記載の研磨用複合材を用いたことを特徴とする。
（１４）本発明の切削工具材料は前記事情に鑑みてなされたもので、先の（１３）に記載の炭素繊維が、母材中に２０〜４５体積％含有されてなることを特徴とする。
（１５）本発明のワイヤーカット放電加工用材料は前記事情に鑑みてなされたもので、先の（１３）に記載の切削工具材料を用いたことを特徴とする。
（１６）本発明のワイヤーカット放電加工方法は前記事情に鑑みてなされたもので、先の（１３）に記載の切削工具材料を用いることを特徴とする。
（１７）本発明の切削工具の製造方法は前記事情に鑑みてなされたもので、先の（１６）に記載のワイヤーカット放電加工方法を用いたことを特徴とする。
（１８）本発明の電子部品の製造方法は前記事情に鑑みてなされたもので、先の（１）に記載の研磨用複合材を用いて、半導体、層間絶縁膜、及び配線材料から選ばれるし少なくも１種を研削する工程を含むことを特徴とする。
（１９）本発明の電子部品の製造方法は前記事情に鑑みてなされたもので、先の（１）に記載の研磨用複合材を用いて、半導体、層間絶縁膜、及び配線材料から選ばれるし少なくも１種を研磨する工程を含むことを特徴とする。
（２０）本発明の電子部品の製造方法は前記事情に鑑みてなされたもので、先の（１８）または（１９）に記載の半導体が、多結晶シリコン、単結晶シリコン、及びアモルファスシリコンから選ばれる少なくとも１種であることを特徴とする。
(10) The grindstone of the present invention is made in view of the above circumstances, and is characterized by being formed by molding the polishing composite material according to any one of (1) to (9) above.
(11) The grinding material of the present invention has been made in view of the above circumstances, and is characterized by using the polishing composite material according to any one of (1) to (9) above.
(12) The polishing material of the present invention has been made in view of the above circumstances, and is characterized by using the polishing composite material according to any one of (1) to (9) above.
(13) The cutting tool material of the present invention has been made in view of the above circumstances, and is characterized by using the polishing composite material according to any one of (1) to (9) above.
(14) The cutting tool material of the present invention has been made in view of the above circumstances, and the carbon fiber described in (13) above is contained in the base material in an amount of 20 to 45% by volume. .
(15) The wire-cut electric discharge machining material of the present invention has been made in view of the above circumstances, and is characterized by using the cutting tool material described in (13) above.
(16) The wire-cut electric discharge machining method of the present invention has been made in view of the above circumstances, and is characterized by using the cutting tool material described in (13) above.
(17) The cutting tool manufacturing method of the present invention has been made in view of the above circumstances, and is characterized by using the wire-cut electric discharge machining method described in (16) above.
(18) An electronic component manufacturing method of the present invention has been made in view of the above circumstances, and is selected from a semiconductor, an interlayer insulating film, and a wiring material using the polishing composite material described in (1) above. However, the method includes a step of grinding at least one kind.
(19) The electronic component manufacturing method of the present invention has been made in view of the above circumstances, and is selected from a semiconductor, an interlayer insulating film, and a wiring material using the polishing composite material described in (1) above. However, the method includes a step of polishing at least one kind.
(20) The method for manufacturing an electronic component of the present invention has been made in view of the above circumstances, and the semiconductor described in (18) or (19) above is selected from polycrystalline silicon, single crystal silicon, and amorphous silicon. It is characterized by being at least one kind.
本発明の研磨用複合材は、炭素繊維を含み、研削、研磨においては摺動性、弾力性、導電性、熱伝導性及び耐食性に優れているので、砥粒の脱落が抑制され、摩擦抵抗が低減し、研磨ムラが抑えられ、被研磨面が高平坦化し、高精度の研削若しくは研磨加工が可能となる。また、本発明の研磨用複合材を用いることにより、切削工具材料においては導電性、熱伝導性が向上し、より高速、高能率切削が実現でき、ワイヤーカット放電加工が可能となる。これらのことにより安価で能率的な工具加工ができる。
また、本発明の研磨用複合材に使用する砥粒や母材は、特に制限はなく従来公知の材料を使用することが可能である。好ましくは、砥粒は半導体分野の用途には酸化セリウム、酸化ケイ素又は酸化アルミニウムから選ばれる少なくとも１種であり、鉄系難削材を切削する工具材料の場合ではボロンナイトライドのうち高圧相のものがよく、特に立方晶ボロンナイトライドが好ましい。切削工具材の母材はアルミニウムの酸化物、窒化物、ホウ化物が好ましい。
さらに、本発明の加工方法によれば、シリコンをはじめとする各種電子部品の研削、研磨加工において、砥粒の脱落が抑制され、摩擦抵抗が低減し、研磨ムラが抑えられ、被研磨面が高平坦化し、高精度の研削若しくは研磨加工が可能となる。
The polishing composite material of the present invention contains carbon fiber, and is excellent in slidability, elasticity, conductivity, thermal conductivity and corrosion resistance in grinding and polishing, so that the falling of abrasive grains is suppressed, and friction resistance , Polishing unevenness is suppressed, the surface to be polished is flattened, and highly accurate grinding or polishing can be performed. Moreover, by using the composite material for polishing of the present invention, the cutting tool material has improved conductivity and thermal conductivity, can realize high-speed and high-efficiency cutting, and enables wire-cut electric discharge machining. By these things, cheap and efficient tool processing can be performed.
Further, the abrasive grains and the base material used for the polishing composite material of the present invention are not particularly limited, and conventionally known materials can be used. Preferably, the abrasive grains are at least one selected from cerium oxide, silicon oxide, and aluminum oxide for applications in the semiconductor field, and in the case of a tool material that cuts iron-based difficult-to-cut materials, boron nitride has a high-pressure phase. In particular, cubic boron nitride is preferable. The base material of the cutting tool material is preferably an aluminum oxide, nitride, or boride.
Furthermore, according to the processing method of the present invention, in grinding and polishing of various electronic parts including silicon, the falling of abrasive grains is suppressed, the frictional resistance is reduced, the polishing unevenness is suppressed, and the surface to be polished is reduced. High flatness and high-precision grinding or polishing are possible.
以下、本発明について詳細に説明するが、本発明は２００２年１２月１１日付けの米国仮出願第６０／４３２,２４７号及び２００３年１２月４日付けの米国出願の出願内容に基づくものである。
まず、本発明の研磨用複合材は、基板、布、粉体などの母材に砥粒と炭素繊維を固着させたものである。研磨用複合材の形態としては、例えば、砥石や切削工具材料のようにバインダー機能を兼ねた母材自身に砥粒と炭素繊維を混合して成型したものや、研磨用ブレードのように母材となる金属やセラミック製の基板表面に、バインダーを使用して砥粒と炭素繊維を固着させたもの、あるいは研磨パッドのように不織布からなる母材の表面に、バインダーを使用して砥粒と炭素繊維を固着させたもの等の形態が利用できる。
また、本発明において研削とは、切断を含む部材を削除する加工方法を指し、研磨とは部材表面の凹凸を少なくして表面を滑らかにする加工方法を指し、切削とは部材表面をより深く切り削ることを指すものとする。また、研削材料あるいは研磨材料あるいは切削材料とはこれらそれぞれの加工目的に使用する材料を指す。研削材料、研磨材料あるいは切削材料の具体例を挙げれば、砥石、研磨ホイール、研削ブレード、研磨パッド、ドレッサー、切削バイト、スローアウェイチップ、ドリル等が挙げられる。
Hereinafter, the present invention will be described in detail. The present invention is based on the contents of US Provisional Application No. 60 / 432,247 dated December 11, 2002 and the US application dated December 4, 2003. is there.
First, the polishing composite material of the present invention is obtained by fixing abrasive grains and carbon fibers to a base material such as a substrate, cloth or powder. As the form of the composite material for polishing, for example, a base material itself that has a binder function such as a grindstone or a cutting tool material is molded by mixing abrasive grains and carbon fiber, or a base material such as a polishing blade The surface of the base material made of non-woven fabric such as a polishing pad is used to fix the abrasive grains and carbon fiber to the surface of the substrate made of metal or ceramic, using a binder, or Forms such as those in which carbon fibers are fixed can be used.
In the present invention, grinding refers to a processing method that removes a member including cutting, polishing refers to a processing method that smoothes the surface by reducing irregularities on the surface of the member, and cutting deepens the surface of the member. It shall refer to cutting. The grinding material, polishing material, or cutting material refers to a material used for each of these processing purposes. Specific examples of the grinding material, polishing material, or cutting material include a grindstone, a polishing wheel, a grinding blade, a polishing pad, a dresser, a cutting tool, a throw-away tip, a drill, and the like.
（砥粒）
本発明に用いる砥粒の種類としては特に限定されるものではなく、従来から使用されている例えば酸化セリウム、酸化ケイ素、酸化アルミニウム、酸化チタン、酸化ジルコニウム、シリコンカーバイド、タングステンカーバイド、ボロンカーバイド、ボロンナイトライド、ダイヤモンド、サファイヤ、有機微粒子などの中から、目的とする被加工物の種類に応じて用いることができる。特に、半導体分野の用途には酸化セリウム、酸化ケイ素又は酸化アルミニウムから選ばれる少なくとも１種を用いることが好ましい。鉄系難削材を切削する工具材料の場合ではボロンナイトライドのうち高圧相のものがよく、特に立方晶ボロンナイトライドが好ましい。
本発明に用いる砥粒の粒径は、研磨材、研削材の場合被加工物の表面仕上げの程度に応じて０．１〜１００μｍのものを使い分けることができる。好ましくは０．３から５０μｍの粒径のものがよい。粒径が０．１μｍ以下の場合、砥粒の突出部が小さく、研磨速度が非常に遅くなる。一方、粒径が１００μｍ以上では、研磨速度は速くなるが、被加工物表面の研磨痕数が多くなり、さらに深さが深くなる。また、表面粗さも粗くなる。切削材の場合の砥粒の粒径は０．０５〜３０μｍがよい。０．０５μｍ以下では、表面不純物が増えるため焼結性が劣り、３０μｍ以上では複合体組織が緻密にならず強度が劣る。
本発明に用いる砥粒の添加量としては、砥石にする場合には３〜３０体積％が好ましく、より好ましくは５〜２０体積％がよい。砥粒の添加量が３体積％以下では研磨速度が遅く、短時間で十分な平坦性を得ることができない。一方、３０体積％以上では樹脂の接着性が低下し、砥粒の脱落が顕著になり、研磨痕数が増大する。
また母材表面に固着させる場合には、砥粒と炭素繊維との体積比が１対０．５乃至１対１程度となるようにするのが好ましい。
切削工具の場合には通常砥粒は４０〜９０体積％添加されるが、耐摩耗性、熱伝導性を上げるために好ましくは６５〜９０体積％がよい。砥粒の添加量が６５％未満では、母材の特性が強く反映され、熱伝導性が悪く、あるいは硬度が低下するため耐摩耗性が劣ったりする。９０体積％を超えると相対的に剛性の高い砥粒では母材の均一混合が難しい。
(Abrasive grains)
The type of abrasive grains used in the present invention is not particularly limited, and conventionally used, for example, cerium oxide, silicon oxide, aluminum oxide, titanium oxide, zirconium oxide, silicon carbide, tungsten carbide, boron carbide, boron Among nitrides, diamonds, sapphire, organic fine particles, etc., they can be used according to the type of the target workpiece. In particular, it is preferable to use at least one selected from cerium oxide, silicon oxide, and aluminum oxide for applications in the semiconductor field. In the case of a tool material for cutting an iron-based difficult-to-cut material, a boron nitride having a high-pressure phase is preferable, and cubic boron nitride is particularly preferable.
In the case of an abrasive or an abrasive, the grain size of the abrasive used in the present invention may be 0.1 to 100 μm depending on the degree of surface finish of the workpiece. A particle diameter of 0.3 to 50 μm is preferable. When the particle size is 0.1 μm or less, the protruding portion of the abrasive grains is small and the polishing rate becomes very slow. On the other hand, when the particle size is 100 μm or more, the polishing rate is increased, but the number of polishing marks on the surface of the workpiece is increased and the depth is further increased. Further, the surface roughness is also increased. The grain size of the abrasive grains in the case of a cutting material is preferably 0.05 to 30 μm. If it is 0.05 μm or less, the surface impurities increase, so that the sinterability is inferior, and if it is 30 μm or more, the composite structure is not dense and the strength is inferior.
As addition amount of the abrasive grain used for this invention, when using it as a grindstone, 3-30 volume% is preferable, More preferably, 5-20 volume% is good. When the added amount of abrasive grains is 3% by volume or less, the polishing rate is slow, and sufficient flatness cannot be obtained in a short time. On the other hand, if it is 30% by volume or more, the adhesiveness of the resin is lowered, the abrasive grains drop off significantly, and the number of polishing marks increases.
Moreover, when making it adhere to the base material surface, it is preferable to make it the volume ratio of an abrasive grain and carbon fiber be about 1 to 0.5 thru | or 1: 1.
In the case of a cutting tool, usually 40 to 90% by volume of abrasive grains are added, but preferably 65 to 90% by volume in order to increase wear resistance and thermal conductivity. When the added amount of the abrasive grains is less than 65%, the characteristics of the base material are strongly reflected, the thermal conductivity is poor, or the hardness is lowered, so that the wear resistance is inferior. If it exceeds 90% by volume, it is difficult to uniformly mix the base material with abrasive grains having relatively high rigidity.
（母材）
本発明に用いる母材としては、プラスチックやゴムなどの樹脂、セメントやガラス、アルミナ、窒化アルミニウム等のセラミックス、純金属や合金などのメタル等が挙げられ、これらは結合剤（ボンド）としての役割も成しているものであっても良い。また母材に砥粒や炭素繊維を固着させる手段は、使用する結合剤（ボンド）の種類によって、レジノイドボンド、メタルボンド、ビトリファイボンド、電着ボンド等が利用できる。母材が結晶質の場合、母材と砥粒、母材同士、砥粒同士の焼結により炭素繊維を粒界に挟むことも可能である。
本発明に用いる樹脂としては、特に限定されるものではなく、公知の樹脂を用いることができる。例えば、ポリアミド、ポリエーテル、ポリエステル、ポリイミド、ポリスルホン、エポキシ、不飽和ポリエステル、フェノールなどの熱硬化性樹脂またはナイロン、ポリエチレン、ポリカーボネート、ポリアリレートなど熱可塑性樹脂などを用いることができる。さらにそれぞれの樹脂に発泡剤を組み合わせることもできる。また、必要に応じて調泡剤、砥粒の分散、湿潤、濡れ性などを調整するための添加剤、樹脂と砥粒の結合強度を調整するためのカップリング剤などを使用することができる。
樹脂を母材とする場合は、樹脂と砥粒及び炭素繊維を混合して圧縮成型して砥石に加工したものであっても良いし、あるいはまた母材となる樹脂製の基板や不織布の表面に、結合剤を用いて砥粒及び炭素繊維を固着させたものであっても良い。
また、金属やセラミックス製の母材表面に砥粒及び炭素繊維を固着させる場合には、メタルボンドが使用できる。メタルボンドとしては、銅、錫、鉄、ニッケル、コバルトやそれらの合金が利用できる。さらに、ビトリファイボンドは８００〜１０００℃で焼結した磁器、ガラス質の無機結合剤であり、電着ボンドは電気メッキ法で砥粒を固定するものである。
(Base material)
Examples of the base material used in the present invention include resins such as plastic and rubber, ceramics such as cement and glass, alumina and aluminum nitride, metals such as pure metals and alloys, etc., and these serve as binders. It may also be made. Resinoid bonds, metal bonds, vitrified bonds, electrodeposition bonds, and the like can be used as means for fixing abrasive grains and carbon fibers to the base material, depending on the type of binder used. When the base material is crystalline, it is also possible to sandwich the carbon fiber between the base material and abrasive grains, between the base materials, and between the abrasive grains.
The resin used in the present invention is not particularly limited, and a known resin can be used. For example, a thermosetting resin such as polyamide, polyether, polyester, polyimide, polysulfone, epoxy, unsaturated polyester, or phenol, or a thermoplastic resin such as nylon, polyethylene, polycarbonate, or polyarylate can be used. Furthermore, a foaming agent can be combined with each resin. Further, as necessary, a foaming agent, an additive for adjusting the dispersion, wettability, wettability, etc. of the abrasive grains, a coupling agent for adjusting the bond strength between the resin and the abrasive grains, and the like can be used. .
When the resin is used as a base material, the resin, abrasive grains, and carbon fibers may be mixed and compression-molded and processed into a grindstone, or the surface of a resin substrate or non-woven fabric used as the base material Alternatively, the abrasive grains and carbon fibers may be fixed using a binder.
Moreover, when bonding abrasive grains and carbon fibers to the surface of a base material made of metal or ceramics, a metal bond can be used. As the metal bond, copper, tin, iron, nickel, cobalt, or an alloy thereof can be used. Furthermore, vitrify bond is a porcelain and glassy inorganic binder sintered at 800 to 1000 ° C., and electrodeposited bond fixes abrasive grains by electroplating.
（炭素繊維）
本発明で使用する炭素繊維は気相法炭素繊維を用いるのが好ましい。気相法炭素繊維は、一般的には、有機遷移金属化合物を用いて有機化合物を熱分解することにより得ることができる。
気相法炭素繊維の原料となる有機化合物は、トルエン、ベンゼン、ナフタレン、エチレン、アセチレン、エタン、天然ガス、一酸化炭素等のガス及びそれらの混合物も使用可能である。中でもトルエン、ベンゼン等の芳香族炭化水素が好ましい。
有機遷移金属化合物は、触媒となる遷移金属を含むものである。遷移金属としては、周期律表第ＩＶa、Ｖa、ＶＩa、ＶＩＩa、ＶＩＩＩ族の金属を含む有機化合物である。中でもフェロセン、ニッケロセン等の化合物が好ましい。
気相法炭素繊維は、上記有機化合物と有機遷移金属化合物を気化して、予め５００〜１３００℃に加熱した水素などの還元性ガスと混合し、８００〜１３００℃に加熱した反応炉へ供給して反応させて得る。
母材との密着性を上げるために、気相法炭素繊維の表面に付着したタールなどの有機物を除くために不活性雰囲気中で９００〜１３００℃で熱処理をおこなうのが好ましい。
さらに母材との密着性を上げるために、酸化性雰囲気中３００〜４５０℃で熱処理を行ったり、炭酸ガスや水酸化カリウムなどにより賦活し、接着面積を上げる方法も利用できる。
気相法炭素繊維の表面積は、振動ミルやジェットミルなどの乾式粉砕、ビーズミルなどの湿式粉砕により上げることもできる。
母材との親和性を上げるために、気相法炭素繊維の表面もしくは全体をフッ素化、酸化などの処理を施してもよい。
(Carbon fiber)
The carbon fiber used in the present invention is preferably a vapor grown carbon fiber. Vapor grown carbon fiber can be generally obtained by thermally decomposing an organic compound using an organic transition metal compound.
As the organic compound used as a raw material for vapor grown carbon fiber, gases such as toluene, benzene, naphthalene, ethylene, acetylene, ethane, natural gas, carbon monoxide, and mixtures thereof can be used. Of these, aromatic hydrocarbons such as toluene and benzene are preferred.
The organic transition metal compound contains a transition metal serving as a catalyst. The transition metal is an organic compound containing a metal of Group IVa, Va, VIa, VIIa, or VIII of the Periodic Table. Of these, compounds such as ferrocene and nickelocene are preferred.
The vapor-grown carbon fiber vaporizes the organic compound and the organic transition metal compound, mixes with a reducing gas such as hydrogen previously heated to 500 to 1300 ° C., and supplies the mixture to a reactor heated to 800 to 1300 ° C. And react.
In order to improve the adhesion to the base material, it is preferable to perform heat treatment at 900 to 1300 ° C. in an inert atmosphere in order to remove organic substances such as tar adhering to the surface of the vapor grown carbon fiber.
Furthermore, in order to raise the adhesiveness with a base material, the method of heat-processing at 300-450 degreeC in an oxidizing atmosphere, or activating with a carbon dioxide gas, potassium hydroxide, etc. can also utilize the method of raising an adhesion area.
The surface area of the vapor grown carbon fiber can also be increased by dry pulverization such as a vibration mill or jet mill, or wet pulverization such as a bead mill.
In order to increase the affinity with the base material, the surface or the whole of the vapor grown carbon fiber may be subjected to a treatment such as fluorination or oxidation.
また、導電性や熱伝導性などの特性を向上させるために気相法炭素繊維を不活性雰囲気下で２０００〜３５００℃で熱処理を行い、結晶を発達させることができる。さらに結晶を発達させ、導電性を向上させるために、気相法炭素繊維に炭化ホウ素（Ｂ ４ Ｃ）、酸化ホウ素（Ｂ ２ Ｏ ３ ）、元素状ホウ素、ホウ酸（Ｈ ３ ＢＯ ３ ）、ホウ酸塩等のホウ素化合物と混合して不活性雰囲気下で２０００〜３５００℃で熱処理を行なって、炭素結晶中にボロン（Ｂ）を０．０１〜５質量％含有する繊維としてもよい。
使用する熱処理炉は２０００℃以上、好ましくは２３００℃以上の目的とする温度が保持できる炉であればよく、通常の、アチソン炉、抵抗炉、高周波炉他の何れの装置でもよい。また、場合によっては、粉体または気相法炭素繊維を押し固めた成形体に直接通電して加熱する方法も使用できる。
熱処理の雰囲気は非酸化性の雰囲気、好ましくはアルゴン、ヘリウム、ネオン等の１種もしくは２種以上の希ガス雰囲気がよい。熱処理の時間は、生産性の面からは出来るだけ短い方が好ましい。特に長時間加熱していると、燒結して固まってくるので製品収率も悪化する。従って、成形体等の中心部の温度が目標温度に達した後、１時間以下の保持時間で十分である。
Moreover, in order to improve characteristics, such as electroconductivity and heat conductivity, a vapor grown carbon fiber can be heat-processed at 2000-3500 degreeC by inert atmosphere, and a crystal | crystallization can be developed. In order to further develop crystals and improve conductivity, vapor grown carbon fiber is boron carbide (B 4 C), boron oxide (B 2 O 3 ), elemental boron, boric acid (H 3 BO 3 ), It is good also as a fiber which mixes with boron compounds, such as a borate, and heat-processes at 2000-3500 degreeC by inert atmosphere, and contains 0.01-5 mass% of boron (B) in a carbon crystal.
The heat treatment furnace to be used may be a furnace capable of maintaining a target temperature of 2000 ° C. or higher, preferably 2300 ° C. or higher, and may be any ordinary apparatus such as an Atchison furnace, a resistance furnace, or a high frequency furnace. Moreover, depending on the case, the method of heating by energizing directly the compact | molding | casting which pressed the powder or the vapor-grown carbon fiber can also be used.
The atmosphere for the heat treatment is a non-oxidizing atmosphere, preferably an atmosphere of one or more rare gases such as argon, helium and neon. The heat treatment time is preferably as short as possible from the viewpoint of productivity. In particular, when heated for a long time, the product yield deteriorates because it sets and solidifies. Therefore, a holding time of 1 hour or less is sufficient after the temperature of the central part of the molded body or the like reaches the target temperature.
本形態に用いる気相法炭素繊維の外径としては２〜５００ｎｍが好ましい。摺動性や導電性などの機能を十分発揮するためにの炭素繊維の分散を均一にする必要があり、繊維の外径としては１０〜３００ｎｍがより好ましく、さらに２０〜２００ｎｍが一層好ましい。また、気相法炭素繊維は、研磨用複合材表面に分布している割合が多ければ多いほど摺動性が向上する。外径が５ｎｍ未満では研磨用複合材内に炭素繊維を均一に分散させることが困難となり、研磨用複合材に摩擦抵抗のムラが発生して研磨ムラの原因となり、外径が５００ｎｍを越えると研磨用複合材に所望の導電性、熱伝導性を付与するために多量の炭素繊維を添加しなければならなくなり、その結果研磨用複合材の機械的強度が低下し、研磨時に砥粒や炭素繊維の脱落による研磨痕が発生し易くなる。
本形態に用いる気相法炭素繊維のアスペクト比としては５〜１５０００が好ましい。研磨用複合材中への均一な分散性を容易にするためには気相法炭素繊維のアスペクト比は１０〜１００がより好ましい。
アスペクト比が５未満では繊維という形状的特徴が失われ、研磨用複合材に所望の導電性、熱伝導性を付与することができなくなり、アスペクト比が１５０００を越えると繊維が相互に絡み合い、研磨用複合材中に炭素繊維を均一に分散させることが困難となり、その結果砥石に成型直後の砥石表面の平坦性の低下、砥石面内の摩擦抵抗のムラ等が発生し、被加工物の平坦性低下の原因となる。
The outer diameter of the vapor grown carbon fiber used in this embodiment is preferably 2 to 500 nm. In order to sufficiently exhibit functions such as slidability and conductivity, it is necessary to uniformly disperse the carbon fiber, and the outer diameter of the fiber is more preferably 10 to 300 nm, and further preferably 20 to 200 nm. In addition, as the proportion of the vapor grown carbon fiber distributed on the surface of the polishing composite material increases, the slidability improves. If the outer diameter is less than 5 nm, it is difficult to uniformly disperse the carbon fibers in the polishing composite material, causing unevenness in frictional resistance in the polishing composite material, causing uneven polishing. If the outer diameter exceeds 500 nm, A large amount of carbon fiber must be added to give the desired composite conductivity and thermal conductivity to the polishing composite material, resulting in a decrease in the mechanical strength of the polishing composite material. Polishing marks are likely to occur due to fiber dropping.
The aspect ratio of vapor grown carbon fiber used in this embodiment is preferably 5 to 15000. In order to facilitate uniform dispersibility in the polishing composite material, the aspect ratio of the vapor grown carbon fiber is more preferably 10 to 100.
If the aspect ratio is less than 5, the shape characteristic of the fiber is lost, and it becomes impossible to impart the desired electrical conductivity and thermal conductivity to the polishing composite. If the aspect ratio exceeds 15,000, the fibers are entangled with each other and polished. As a result, it becomes difficult to uniformly disperse carbon fibers in the composite material, resulting in a decrease in the flatness of the surface of the grindstone immediately after molding, unevenness in the frictional resistance in the surface of the grindstone, etc. Cause a decline in sex.
また、本発明で使用する炭素繊維は、ＢＥＴ比表面積が４ｍ２ ／ｇ以上であるものが好ましい。
ＢＥＴ比表面積が４ｍ２ ／ｇ未満では母材との接着面積が小さくなり、炭素繊維の捕捉力が低下し、研削、研磨時に研磨用複合材から炭素繊維が脱落してしまい、スクラッチや研磨痕の原因となる。
さらに、本発明で使用する炭素繊維は、Ｘ線回折における炭素（００２）面の面間隔（ｄ００２ ）が０．３４５ｎｍ以下であるものが好ましい。
（ｄ００２ ）値が０．３４５ｎｍを越えると熱伝導性や摺動性が低下し、研磨時に発生する熱の放熱性が低下し、研磨焼けなどの問題が発生する。
また、本発明で使用する炭素繊維は、ラマン散乱スペクトルの１３４１〜１３４９ｃｍ−１のバンドピーク高さ（Ｉｄ）と１５７０〜１５７８ｃｍ−１のピーク高さ（Ｉｇ）の比（Ｉｄ／Ｉｇ）が１.５以下であるものが好ましい。
ここで、ラマンスペクトルのＩｄは炭素構造の乱れの増加と対応しているブロードなバンド領域であり、Ｉｇは完全なグラファイト構造と関連づけられる比較的シャープなバンド領域である。ピークの強度比は、炭素材料の黒鉛化度を示す指標として用いられているが、この強度比をピーク高さ比として示した場合、黒鉛化度が高いほど小さい値となる。
（Ｉｄ／Ｉｇ）の値が１．５を越えるとグラフェンシート面内の結晶が発達していないため、炭素繊維自体の導電性、熱伝導性が低く、研磨用複合材に所望の導電性や熱伝導性を付与することが困難となる場合がある。
The carbon fiber used in the present invention preferably has a BET specific surface area of 4 m 2 / g or more.
When the BET specific surface area is less than 4 m 2 / g, the adhesion area with the base material becomes small, the carbon fiber capturing force decreases, and the carbon fiber falls off from the polishing composite during grinding and polishing, resulting in scratches and polishing marks. Cause.
Furthermore, the carbon fiber used in the present invention preferably has a carbon (002) plane spacing (d002) of 0.345 nm or less in X-ray diffraction.
If the value of (d002) exceeds 0.345 nm, the thermal conductivity and slidability deteriorate, the heat dissipation of the heat generated during polishing decreases, and problems such as polishing burns occur.
The carbon fiber used in the present invention has a ratio (Id / Ig) of the band peak height (Id) of 1341 to 1349 cm −1 and the peak height (Ig) of 1570 to 1578 cm −1 of the Raman scattering spectrum of 1. It is preferable that it is 0.5 or less.
Here, Id of the Raman spectrum is a broad band region corresponding to an increase in the disorder of the carbon structure, and Ig is a relatively sharp band region associated with a complete graphite structure. The intensity ratio of the peak is used as an index indicating the degree of graphitization of the carbon material. When this intensity ratio is indicated as the peak height ratio, the higher the degree of graphitization, the smaller the value.
When the value of (Id / Ig) exceeds 1.5, since the crystal in the graphene sheet plane is not developed, the conductivity and thermal conductivity of the carbon fiber itself are low, and the desired conductivity or It may be difficult to impart thermal conductivity.
本発明で使用する炭素繊維は中心部に中空構造を有する多層構造のものとする。中空構造を有することにより弾力性に富んだものとなり、研磨効率が高まるにもかかわらず研磨痕の発生を抑制することができるようになる。また、多層構造を有することにより潤滑性に富んだものとなり、研磨痕の発生を抑制することができるようになる。このような中心部に中空構造を有する多層構造の炭素繊維は、気相法によって得られる炭素繊維に特有の性質である。
本発明で使用する炭素繊維は分岐状気相法炭素繊維を含むものであっても良い。分岐状気相法炭素繊維は、外径が極細でありながら分岐部が連通した中空構造を有する場合が多い。分岐状気相法炭素繊維を研磨用複合材に添加する場合、通常の気相法炭素繊維に比べて低濃度添加しただけで、効率よく導電や熱伝導ネットワークを形成することができる。換言すれば通常の気相法炭素繊維と同濃度の分岐状気相法炭素繊維を研磨用複合材に添加した場合、より高い導電性、熱伝導性、摺動性、弾力性を得ることができる。
本発明で使用する炭素繊維は、炭素繊維結晶中に０．０１〜５質量％のホウ素が含有されていることが好ましい。
The carbon fiber used in the present invention has a multilayer structure having a hollow structure at the center. By having a hollow structure, it becomes rich in elasticity, and generation of polishing marks can be suppressed despite an increase in polishing efficiency. Further, by having a multilayer structure, it becomes rich in lubricity, and generation of polishing marks can be suppressed. Such a carbon fiber having a multilayer structure having a hollow structure in the center part has a characteristic characteristic of the carbon fiber obtained by the vapor phase method.
The carbon fiber used in the present invention may include a branched vapor grown carbon fiber. In many cases, the branched vapor grown carbon fiber has a hollow structure in which branch portions communicate with each other even though the outer diameter is extremely fine. When the branched vapor grown carbon fiber is added to the polishing composite, a conductive or heat conduction network can be efficiently formed only by adding a low concentration compared to a normal vapor grown carbon fiber. In other words, when a branched vapor grown carbon fiber having the same concentration as a normal vapor grown carbon fiber is added to the polishing composite material, higher conductivity, thermal conductivity, slidability, and elasticity can be obtained. it can.
The carbon fiber used in the present invention preferably contains 0.01 to 5% by mass of boron in the carbon fiber crystal.
炭素繊維中にホウ素が含有されていると、結晶の積層構造が発達するため導電性が向上する。また、結晶性の発達および結晶面内に取り込まれたホウ素の効果により炭素繊維の耐食性が向上したり、表面電荷分布が変化し、母材との濡れ性や摺動性が改善される。これらホウ素を含有する気相法炭素繊維を研磨用複合材に添加することにより、研磨時の摩擦抵抗を減少させ、摩擦熱の発生を抑制することができる。また、母材との密着性が改善されるため研磨時の炭素繊維の脱落を低減することができる。
本発明の研磨用複合材は、基板、布、粉体などの母材に砥粒と炭素繊維を固着させたものである。研磨用複合材の形態としては、例えば砥石や切削工具材料のようにバインダー機能を兼ねた母材自身に砥粒と炭素繊維を混合して成型したものや、研磨用ブレードのように母材となる金属やセラミック製の基材表面に、バインダーを使用して砥粒と炭素繊維を固着させたもの、あるいは研磨パッドのように不織布からなる母材の表面に、バインダーを使用して砥粒と炭素繊維を固着させたもの等の形態が利用できる。
When boron is contained in the carbon fiber, the crystal structure is developed, so that conductivity is improved. In addition, the development of crystallinity and the effect of boron incorporated in the crystal plane improve the corrosion resistance of the carbon fiber, change the surface charge distribution, and improve the wettability and slidability with the base material. By adding these vapor-grown carbon fibers containing boron to the polishing composite material, the frictional resistance during polishing can be reduced and the generation of frictional heat can be suppressed. In addition, since the adhesion with the base material is improved, it is possible to reduce the falling off of the carbon fiber during polishing.
The polishing composite material of the present invention is obtained by fixing abrasive grains and carbon fibers to a base material such as a substrate, cloth or powder. As the form of the composite material for polishing, for example, a base material having a binder function such as a grindstone or a cutting tool material, which is molded by mixing abrasive grains and carbon fiber, or a base material such as a polishing blade is used. The surface of the base material made of metal or ceramic to be bonded to the abrasive grains and carbon fibers using a binder, or the surface of the base material made of a non-woven fabric such as a polishing pad, and the abrasive grains using a binder Forms such as those in which carbon fibers are fixed can be used.
研磨用複合材が砥石の形態を取る場合、本発明で用いる炭素繊維の添加量としては、５〜４０体積％が好ましく、１０〜３０体積％がより好ましい。添加量が５体積％以下であると、研磨用複合材に十分な摺動性、弾力性、導電性、熱伝導性、耐食性を付与することができず、平坦な研磨面を得ることができない。また、添加量が４０体積％以上になると母材との密着性が悪くなり、研磨用複合材の機械的強度が低下する。その結果、研磨時に研磨用複合材から炭素繊維や砥粒の脱落が発生し、研磨用複合材及び被加工物の品質低下を招いてしまう。
研磨用複合材が切削工具材料の形態を取る場合、炭素繊維の添加量としては、２〜１５体積％が好ましく、２〜１０体積％がより好ましい。添加量が２体積％以下であると、研磨用複合材に十分な導電性を付与することができず、ワイヤーカット放電加工ができない。また、添加量が１５体積％以上になると切削時の摩耗が大きくなり、またチッピングが発生しやすくなる。
研磨用複合材が基材表面にバインダーを使用して砥粒と炭素繊維を固着させたもの、あるいは不織布等からなる母材の表面に、バインダーを使用して砥粒と炭素繊維を固着させた形態を取る場合、炭素繊維の使用量は砥粒と炭素繊維との体積比が１対０．５〜１対１程度となるようにするのが好ましい。
When the abrasive composite takes the form of a grindstone, the amount of carbon fiber used in the present invention is preferably 5 to 40% by volume, more preferably 10 to 30% by volume. If the addition amount is 5% by volume or less, the polishing composite material cannot be provided with sufficient slidability, elasticity, conductivity, thermal conductivity, and corrosion resistance, and a flat polished surface cannot be obtained. . On the other hand, when the addition amount is 40% by volume or more, the adhesion with the base material is deteriorated, and the mechanical strength of the polishing composite material is lowered. As a result, carbon fibers and abrasive grains fall off from the polishing composite during polishing, leading to a deterioration in the quality of the polishing composite and the workpiece.
When the abrasive composite takes the form of a cutting tool material, the amount of carbon fiber added is preferably 2 to 15% by volume, more preferably 2 to 10% by volume. When the addition amount is 2% by volume or less, sufficient conductivity cannot be imparted to the polishing composite material, and wire-cut electric discharge machining cannot be performed. Further, when the addition amount is 15% by volume or more, wear during cutting increases, and chipping is likely to occur.
Abrasive composite material in which abrasive grains and carbon fibers are fixed to a substrate surface using a binder, or a base material made of a nonwoven fabric or the like is used to fix abrasive grains and carbon fibers to a surface of a base material. When taking a form, it is preferable that the amount of carbon fiber used is such that the volume ratio of the abrasive grains to the carbon fiber is about 1: 0.5 to 1: 1.
上記のように構成した本発明の研磨用複合材は、炭素繊維を添加することにより、研磨用複合材に弾力性を付与し、被研磨物に過剰な負荷を与えることなく、研磨痕を低減することができる。
被加工物の平坦化には、砥石の平坦性に加え、砥石と被加工物接触面内の圧力分布の均一性が求められる。嵩密度が低く、弾力性に富む炭素繊維、特に気相法炭素繊維を砥石に添加すると砥石の弾性率が大きくなり、研磨圧力を均一化することができ、被加工物面の均一な平坦化を可能とする。さらに過剰な圧力がかかった場合でも、変形による圧力緩和により研磨痕の深さを浅くしたり、数を少なくすることができる。
さらに、摺動性、導電性、熱伝導性、耐食性を向上させることで、加工時の物理的、化学的要因の影響を低減することができるようになる効果を有する。
特にダイヤモンド砥粒を用いて半導体を研削、研磨する場合、大気中の酸素と摩擦熱によるダイヤモンド砥粒の酸化を抑え、研磨材の寿命を延長することができるようになる。
また、半導体ウェハの研磨や、研磨パッドのドレッシング時における研磨材の砥粒の脱落を抑えることができるようになる。
The composite material for polishing of the present invention configured as described above gives elasticity to the composite material for polishing by adding carbon fiber, and reduces polishing marks without applying excessive load to the object to be polished. can do.
In order to flatten the workpiece, in addition to the flatness of the grindstone, the uniformity of the pressure distribution in the contact surface between the grindstone and the workpiece is required. Addition of carbon fiber with low bulk density and high elasticity, especially vapor grown carbon fiber, to the grinding wheel increases the elastic modulus of the grinding wheel and makes it possible to equalize the polishing pressure and evenly flatten the work surface. Is possible. Further, even when excessive pressure is applied, the depth of the polishing mark can be reduced or the number can be reduced by pressure relaxation due to deformation.
Furthermore, by improving slidability, conductivity, thermal conductivity, and corrosion resistance, there is an effect that the influence of physical and chemical factors during processing can be reduced.
In particular, when a semiconductor is ground and polished using diamond abrasive grains, oxidation of the diamond abrasive grains due to atmospheric oxygen and frictional heat can be suppressed, and the life of the abrasive can be extended.
In addition, it is possible to prevent the abrasive grains from falling off during polishing of the semiconductor wafer or dressing of the polishing pad.
半導体ウェハの研磨においては、半導体ウェハと砥粒部分以外との摩擦抵抗を低減させ、被加工物である半導体ウェハの研磨ムラを抑え、表面を高平坦化することができ、発生する摩擦熱を放熱させて研磨焼けを低減することができる効果を発揮する。
さらに、砥石形成時に優れた離型性を付与することができる研磨用複合材となる。
面接触で研磨する砥石の場合、砥石の研磨面の平坦性は、研磨後の被加工物の平坦性に影響を及ぼす。したがって、いかに金型通りに砥石を抜き取るのかが重要になる。砥石形成時の離型性を改善するには、離型剤等を使用することもできる。しかし、本発明の炭素繊維を用いた場合、砥石に摺動性を与え、その結果、優れた離型性と同時に研削、研磨時の砥粒部以外の摩擦抵抗を低減することができる。
In polishing a semiconductor wafer, the frictional resistance between the semiconductor wafer and the part other than the abrasive grains is reduced, the unevenness of polishing of the semiconductor wafer as a workpiece can be suppressed, the surface can be flattened, and the generated frictional heat can be reduced. The effect of reducing heat dissipation by dissipating heat is exhibited.
Furthermore, it becomes an abrasive composite material that can impart excellent releasability when forming a grindstone.
In the case of a grindstone that is ground by surface contact, the flatness of the ground surface of the grindstone affects the flatness of the workpiece after polishing. Therefore, it is important how to remove the grindstone according to the mold. In order to improve the releasability at the time of forming the grindstone, a release agent or the like can be used. However, when the carbon fiber of the present invention is used, the grindstone is given slidability, and as a result, the frictional resistance other than the abrasive grains during grinding and polishing can be reduced simultaneously with excellent release properties.
また、砥石に導電性を付与し、研磨後の砥石膜厚を電気的に把握することができ、砥石交換などの管理を行うことができる研磨用複合材となる。
連続研磨による生産を行う場合、一般に研磨時間で研磨量を制御し、平坦化しているため、研磨後の砥石膜厚を把握することは重要である。レーザや光では砥石の残膜量を把握することは難しい。しかし、本発明の炭素繊維を添加した砥石では、炭素繊維が高い導電性を有するため、砥粒、砥石に導電性が付与され、残膜量を電気抵抗で管理することができ、また、導電性を有する基板上に該砥石を設置することで全体が電気的導通となり、この基板の位置を導通検出手段を用いて検出することができ、基板位置を制御手段を用いて制御することで常に同一の研磨環境を再現することができる。
さらに、研磨時に発生する摩擦熱による研磨焼けや砥粒の消耗を抑えるために、研磨時に水などの冷媒を供給する方法があるが、炭素繊維を砥石に添加するとさらに高い放熱、冷却の効果を得ることができるので、砥粒の消耗を抑えることが可能となる。
Further, the grinding stone can be provided with conductivity, the grinding wheel thickness after polishing can be electrically grasped, and the grinding composite material can be managed such as grinding wheel replacement.
In the case of production by continuous polishing, it is important to grasp the grindstone film thickness after polishing because the polishing amount is generally controlled by the polishing time and flattened. It is difficult to grasp the remaining film amount of the grindstone with a laser or light. However, in the grindstone to which the carbon fiber of the present invention is added, since the carbon fiber has high conductivity, conductivity is imparted to the abrasive grains and the grindstone, and the amount of the remaining film can be managed by electric resistance. When the grindstone is placed on a substrate having electrical properties, the whole becomes electrically conductive, and the position of the substrate can be detected using the conduction detecting means, and the substrate position is always controlled by using the control means. The same polishing environment can be reproduced.
Furthermore, there is a method of supplying a coolant such as water at the time of polishing in order to suppress polishing burn and abrasive grain consumption due to frictional heat generated at the time of polishing, but adding carbon fiber to the grindstone has a higher heat dissipation and cooling effect. Since it can be obtained, it is possible to suppress wear of the abrasive grains.
以上、被加工物を研削、研磨する場合について説明したが、本発明の複合研磨
材は、研磨パッドのドレッサーにも利用できる。
例えば、スラリーなどの浮遊砥粒方式による半導体ウェハの研磨では、ウェハ研磨と次のウェハ研磨の間に研磨パッドの清浄化を行う。例えば化学的機械的研磨では研磨パッドとして発泡ポリウレタンがよく用いられている。ウェハを研磨した後にパッドを電子顕微鏡で観察すると、パッド表面の凹部に砥粒や被加工物の削り屑が堆積したり、スラリーに含まれるエッチャントと呼ばれる添加剤の影響などにより凹部が閉塞されていることが観察される。凹部が閉塞すると研磨速度が低下したり、堆積した砥粒により研磨痕が増大するという問題がある。したがって、ウェハ研磨後にパッドをドレッシングして余分な砥粒を除去し、閉塞した凹部を回復する必要がある。しかし、パッド表面はスラリー中のエッチャントにより酸性またはアルカリ性であることが多く、そのためドレッサー表面は化学的に安定であることが望まれる。炭素繊維を砥石に添加することで酸やアルカリと接触する面積を減らすことができ、化学的に安定となって砥粒の脱落などを抑えることができる。
Although the case where the workpiece is ground and polished has been described above, the composite abrasive of the present invention can also be used as a dresser for a polishing pad.
For example, in polishing a semiconductor wafer by a floating abrasive method such as slurry, the polishing pad is cleaned between the wafer polishing and the next wafer polishing. For example, in chemical mechanical polishing, polyurethane foam is often used as a polishing pad. When the pad is observed with an electron microscope after polishing the wafer, abrasive grains or workpiece shavings accumulate in the recesses on the pad surface, or the recesses are blocked due to the influence of an additive called an etchant contained in the slurry. Observed. When the concave portion is closed, there is a problem that the polishing rate is lowered or the polishing marks are increased due to the accumulated abrasive grains. Therefore, after polishing the wafer, it is necessary to dress the pad to remove excess abrasive grains and recover the closed recess. However, the pad surface is often acidic or alkaline due to the etchant in the slurry, and therefore it is desirable that the dresser surface be chemically stable. By adding carbon fiber to the grindstone, the area in contact with the acid or alkali can be reduced, and it becomes chemically stable and can prevent the abrasive grains from dropping off.
次に、本発明の研磨用複合材を使用した砥石や研削材、研磨材を使用して電子部品を研削、研磨加工する方法について説明する。
電子部品の一例として半導体集積回路を例に挙げて説明すると、鏡面加工されたシリコンウエハの表面に絶縁層を形成し、その絶縁層の上にアルミニウム等の金属薄膜からなる回路パターンを形成する。近年の集積回路では高機能を負荷するため、絶縁層と回路パターンを複数層積層した多層集積回路が多用されている。回路パターンの形成は、導体薄膜表面に形成したフォトレジスト膜に回路パターンを露光により転写し、エッチングすることにより微細なパターンを形成している。そのため転写面の平坦性が確保されないと精密な回路パターンを形成することはできない。このような多層の半導体集積回路を形成する場合には、シリコンウエハの鏡面研磨をはじめとして、層間絶縁膜や回路パターン形成用の金属薄膜も高精度に研磨して平坦性を確保することが重要となる。
本発明の電子部品の加工方法は、シリコンウエハをじめとする半導体の切断を含む研削加工、研磨加工や、層間絶縁膜若しくは回路パターンとなる金属薄膜の研磨加工が対象となる。これらの電子部品の加工方法において本発明の研磨用複合材を使用した砥石や研削材、研磨材を使用すれば、デイッシングやシニングといった研磨ムラが無く、微小キズや研磨痕の無い高度に平坦性を有する精密加工された加工面を得ることができる。
特に、本発明の砥石は多結晶シリコン、単結晶シリコンあるいはアモルファスシリコン等のシリコンの研削加工若しくは研磨加工に際して有用である。
Next, a method for grinding and polishing an electronic component using a grindstone, an abrasive, or an abrasive using the abrasive composite of the present invention will be described.
A semiconductor integrated circuit will be described as an example of an electronic component. An insulating layer is formed on the surface of a mirror-finished silicon wafer, and a circuit pattern made of a metal thin film such as aluminum is formed on the insulating layer. In recent years, in order to load a high function in an integrated circuit, a multilayer integrated circuit in which a plurality of insulating layers and circuit patterns are stacked is often used. The circuit pattern is formed by transferring the circuit pattern to a photoresist film formed on the surface of the conductive thin film by exposure and etching to form a fine pattern. Therefore, a precise circuit pattern cannot be formed unless the flatness of the transfer surface is ensured. When forming such a multi-layer semiconductor integrated circuit, it is important to ensure flatness by polishing the interlayer insulating film and the metal thin film for circuit pattern formation with high precision, including mirror polishing of silicon wafers. It becomes.
The electronic component processing method of the present invention is intended for grinding and polishing processes including cutting of semiconductors including silicon wafers, and polishing processes for metal thin films that form interlayer insulating films or circuit patterns. In the processing method of these electronic parts, if the grindstone, abrasive, or abrasive using the abrasive composite material of the present invention is used, there is no unevenness of polishing such as dishing or thinning, and there is no fine scratches or traces. It is possible to obtain a precisely machined surface having
In particular, the grindstone of the present invention is useful when grinding or polishing silicon such as polycrystalline silicon, single crystal silicon, or amorphous silicon.
以下に本発明について実施例を示し、本発明をさらに具体的に説明する。なお、これらは説明のための単なる例示であって、本発明はこれらに何等制限されるものではない。なお、下記の例における各特性の測定方法は以下の通りである。
（１）ＢＥＴ比表面積
Quantachrome社製、ＮＯＶＡ１２００を使用し、液体窒素温度における窒素の吸着等温線より、ＢＥＴ法およびＢＪＨ法を用いて算出した。なお、窒素の吸着量は相対圧力（Ｐ／Ｐ０ ）を０.０１〜１.０として測定した。
（２）ラマン散乱スペクトル
励起光として波長５１４．５ｎｍのアルゴン（Ａｒ）レーザを使用し、検出器としてＣＣＤ（ Charge Coupled Device ）を使用し、スリット間隔は５００μｍ、露光時間は６０秒で炭素繊維のラマン散乱スペクトルを測定した。
（３）表面電気抵抗
ダイヤモンドビト砥石＃325/400にて平面研削仕上げした材料表面を４端子法で５点測定し平均値を求めた。
（４）ワイヤーカット放電加工機（WEDM）
ファナック製 ROBOCUT α-0C
（５）切削性能試験
工具形状：SNGN120308 被削材：鉄系焼結合金（ＨRC 45）
V=150m/min f=0.15mm/rev d=0.5mm 切削長 1200m
摩耗量はフランク摩耗ＶＢmaxで表示
Examples of the present invention will be shown below, and the present invention will be described more specifically. Note that these are merely illustrative examples, and the present invention is not limited thereto. In addition, the measuring method of each characteristic in the following example is as follows.
(1) BET specific surface area
Using NOVA1200 manufactured by Quantachrome, it was calculated from the adsorption isotherm of nitrogen at the liquid nitrogen temperature using the BET method and the BJH method. The amount of nitrogen adsorbed was measured at a relative pressure (P / P0) of 0.01 to 1.0.
(2) Raman scattering spectrum An argon (Ar) laser having a wavelength of 514.5 nm is used as excitation light, a CCD (Charge Coupled Device) is used as a detector, a slit interval is 500 μm, an exposure time is 60 seconds, and carbon fiber Raman scattering spectrum was measured.
(3) Surface electrical resistance The surface of the material that was surface ground with a diamond bit grindstone # 325/400 was measured at five points by the 4-terminal method, and the average value was obtained.
(4) Wire cut electric discharge machine (WEDM)
FANUC ROBOCUT α-0C
(5) Cutting performance test Tool shape: SNGN120308 Work material: Sintered iron alloy (HRC 45)
V = 150m / min f = 0.15mm / rev d = 0.5mm Cutting length 1200m
Wear amount is indicated by Frank wear V B max
（実施例１）
フェノール樹脂に平均粒径０．５μｍの酸化セリウムを１０体積％と、平均繊維径２００ｎｍ、アスペクト比１００、ＢＥＴ比表面積が１０ｍ２／ｇ、ｄ００２が０．３３９ｎｍ、Ｉｄ／Ｉｇが０．１で、中心部が中空で積層構造を有する気相法炭素繊維を３０体積％混合し、金型温度１６０℃、成形圧力９８０．６ｋＰで１５分間加圧成形して、直径５０ｍｍ、厚さ１０ｍｍの砥石を作製した。研磨は絶縁膜を被覆したシリコンウェハに水を流しながら砥石に４９ｋＰの荷重をかけて３分間行った。このとき、シリコンウエハ及び砥石は、相対速度が１０ｃｍ／ｓｅｃになるようにそれぞれ同方向に回転させながら行った。研磨速度は研磨前と研磨後の膜厚を光干渉式膜厚計で測定して求めた。研磨後の表面粗さは触針式粗さ計で計測した。研磨痕の測定は光学顕微鏡観察により実施した。
研磨速度３００ｎｍ／ｍｉｎ、表面粗さ２．０ｎｍという実用上十分な研磨速度及び表面粗さを得ることができた。また、研磨面を光学顕微鏡で観察した結果、ウェハ表面に研磨痕が全く発生していないことを確認した。
Example 1
10% by volume of cerium oxide having an average particle diameter of 0.5 μm in a phenol resin, an average fiber diameter of 200 nm, an aspect ratio of 100, a BET specific surface area of 10 m 2 / g, d002 of 0.339 nm, and Id / Ig of 0.1 30% by volume of vapor-grown carbon fiber with a hollow center part and a laminated structure is mixed and pressure-molded at a mold temperature of 160 ° C. and a molding pressure of 980.6 kP for 15 minutes. Was made. Polishing was performed for 3 minutes by applying a load of 49 kP to the grindstone while flowing water through the silicon wafer coated with the insulating film. At this time, the silicon wafer and the grindstone were rotated while rotating in the same direction so that the relative speed was 10 cm / sec. The polishing rate was determined by measuring the film thickness before and after polishing with an optical interference film thickness meter. The surface roughness after polishing was measured with a stylus type roughness meter. The measurement of the polishing marks was performed by observation with an optical microscope.
A practically sufficient polishing rate and surface roughness of 300 nm / min and a surface roughness of 2.0 nm could be obtained. Further, as a result of observing the polished surface with an optical microscope, it was confirmed that no polishing mark was generated on the wafer surface.
（実施例２）
フェノール樹脂に平均粒径０．５μｍの酸化セリウムを１０体積％と、平均繊維径２０ｎｍ、アスペクト比１００、ＢＥＴ比表面積が１００ｍ２／ｇ、ｄ００２が０．３４１ｎｍ、Ｉｄ／Ｉｇが０．２で、中心部が中空で積層構造を有するある気相法炭素繊維を３０体積％混合し、金型温度１６０℃、成形圧力９８０．６ｋＰで１５分間加圧成形して、直径５０ｍｍ、厚さ１０ｍｍの砥石を作製した。研磨は絶縁膜を被覆したシリコンウェハに水を流しながら砥石に４９ｋＰの荷重をかけて３分間行った。このとき、シリコンウエハ及び砥石は、相対速度が１０ｃｍ／ｓｅｃになるようにそれぞれ同方向に回転させながら行った。研磨速度は研磨前と研磨後の膜厚を光干渉式膜厚計で測定して求めた。研磨後の表面粗さは触針式粗さ計で計測した。研磨痕の測定は光学顕微鏡観察により実施した。
研磨速度２８０ｎｍ／ｍｉｎ、表面粗さ１．５ｎｍという実用上十分な研磨速度及び表面粗さを得ることができた。また、研磨面を光学顕微鏡で観察した結果、ウェハ表面に研磨痕が全く発生していないことを確認した。
(Example 2)
10% by volume of cerium oxide having an average particle diameter of 0.5 μm in a phenol resin, an average fiber diameter of 20 nm, an aspect ratio of 100, a BET specific surface area of 100 m 2 / g, d002 of 0.341 nm, and Id / Ig of 0.2 30% by volume of a vapor-grown carbon fiber having a hollow center part and a laminated structure is mixed and pressure-molded at a mold temperature of 160 ° C. and a molding pressure of 980.6 kP for 15 minutes to have a diameter of 50 mm and a thickness of 10 mm. A grindstone was produced. Polishing was performed for 3 minutes by applying a load of 49 kP to the grindstone while flowing water through the silicon wafer coated with the insulating film. At this time, the silicon wafer and the grindstone were rotated while rotating in the same direction so that the relative speed was 10 cm / sec. The polishing rate was determined by measuring the film thickness before and after polishing with an optical interference film thickness meter. The surface roughness after polishing was measured with a stylus type roughness meter. The measurement of the polishing marks was performed by observation with an optical microscope.
A practically sufficient polishing rate and surface roughness of 280 nm / min and a surface roughness of 1.5 nm could be obtained. Further, as a result of observing the polished surface with an optical microscope, it was confirmed that no polishing mark was generated on the wafer surface.
（比較例１）
フェノール樹脂に平均粒径０．５μｍの酸化セリウムを１０体積％混合し、金型温度１６０℃、成形圧力９８０．６ｋＰで１５分間加圧成形して、φ５０ｍｍ、厚さ１０ｍｍの砥石を作製した。研磨は絶縁膜を被覆したシリコンウェハに水を流しながら砥石に４９ｋＰの荷重をかけて３分間行った。このとき、シリコンウエハ及び砥石は、相対速度が１０ｃｍ／ｓｅｃになるようにそれぞれ同方向に回転させながら行った。研磨速度は研磨前と研磨後の膜厚を光干渉式膜厚計で測定して求めた。研磨後の表面粗さは触針式粗さ計で計測した。研磨痕の測定は光学顕微鏡観察により実施した。
研磨速度４００ｎｍ／ｍｉｎという十分な研磨速度を得ることができたが、表面粗さは１０．０ｎｍまでしか至らなかった。また、研磨面を光学顕微鏡で観察した結果、ウェハ表面に研磨痕が１３個／ｃｍ２程度で発生していることを確認した。
(Comparative Example 1)
Phenol resin was mixed with 10% by volume of cerium oxide having an average particle size of 0.5 μm, and press-molded for 15 minutes at a mold temperature of 160 ° C. and a molding pressure of 980.6 kP to produce a grinding wheel having a diameter of 50 mm and a thickness of 10 mm. Polishing was performed for 3 minutes by applying a load of 49 kP to the grindstone while flowing water through the silicon wafer coated with the insulating film. At this time, the silicon wafer and the grindstone were rotated while rotating in the same direction so that the relative speed was 10 cm / sec. The polishing rate was determined by measuring the film thickness before and after polishing with an optical interference film thickness meter. The surface roughness after polishing was measured with a stylus type roughness meter. The measurement of the polishing marks was performed by observation with an optical microscope.
Although a sufficient polishing rate of 400 nm / min could be obtained, the surface roughness reached only 10.0 nm. Further, as a result of observing the polished surface with an optical microscope, it was confirmed that polishing marks were generated at about 13 pieces / cm 2 on the wafer surface.
（比較例２）
フェノール樹脂に平均粒径０．５μｍの酸化セリウムを１０体積％と、平均繊維径２０ｎｍ、アスペクト比２、ＢＥＴ比表面積が１３０ｍ２／ｇ、ｄ００２が０．３４１ｎｍ、Ｉｄ／Ｉｇが０．２で、中心部が中空で積層構造を有するある気相法炭素繊維を３０体積％混合し、金型温度１６０℃、成形圧力９８０．６ｋＰで１５分間加圧成形して、直径５０ｍｍ、厚さ１０ｍｍの砥石を作製した。研磨は絶縁膜を被覆したシリコンウェハに水を流しながら砥石に４９ｋＰの荷重をかけて３分間行った。このとき、シリコンウエハ及び砥石は、相対速度が１０ｃｍ／ｓｅｃになるようにそれぞれ同方向に回転させながら行った。研磨速度は研磨前と研磨後の膜厚を光干渉式膜厚計で測定して求めた。研磨後の表面粗さは触針式粗さ計で計測した。研磨痕の測定は光学顕微鏡観察により実施した。
研磨速度３７０ｎｍ／ｍｉｎという十分な研磨速度を得ることができたが、表面粗さは８．５ｎｍまでしか至らなかった。また、研磨面を光学顕微鏡で観察した結果、ウェハ表面に研磨痕が１０個／ｃｍ２程度で発生していることを確認した。
これら実施例及び比較例の加工結果を表１に示す。
(Comparative Example 2)
10% by volume of cerium oxide having an average particle diameter of 0.5 μm in a phenol resin, an average fiber diameter of 20 nm, an aspect ratio of 2, a BET specific surface area of 130 m 2 / g, d002 of 0.341 nm, and Id / Ig of 0.2 30% by volume of a vapor-grown carbon fiber having a hollow center part and a laminated structure is mixed and pressure-molded at a mold temperature of 160 ° C. and a molding pressure of 980.6 kP for 15 minutes to have a diameter of 50 mm and a thickness of 10 mm. A grindstone was produced. Polishing was performed for 3 minutes by applying a load of 49 kP to the grindstone while flowing water through the silicon wafer coated with the insulating film. At this time, the silicon wafer and the grindstone were rotated while rotating in the same direction so that the relative speed was 10 cm / sec. The polishing rate was determined by measuring the film thickness before and after polishing with an optical interference film thickness meter. The surface roughness after polishing was measured with a stylus type roughness meter. The measurement of the polishing marks was performed by observation with an optical microscope.
Although a sufficient polishing rate of 370 nm / min could be obtained, the surface roughness reached only 8.5 nm. Further, as a result of observing the polished surface with an optical microscope, it was confirmed that polishing marks were generated at about 10 pieces / cm 2 on the wafer surface.
Table 1 shows the processing results of these examples and comparative examples.
次に、実施例１，実施例２及び比較例１について、金型から取り出す際の砥石の不良率と摺動性を表１に併記する。
不良率とは、成形用金型から離型する際に破損した砥石や砥石表面の一部が剥がれて成形金型に付着したままとなったものの割合である。
砥石の摺動性はスラスト式摺動試験方法で評価した。２０ｃｍ／ｓｅｃで回転させた砥石の上方から絶縁膜を被覆したシリコンウェハを１４７ｋＰの荷重をかけて６０分間押し当てた。試験後の砥石の摩耗量を測定して、摺動特性評価の指針とした。
Next, for Example 1, Example 2 and Comparative Example 1, the defect rate and slidability of the grindstone when taking out from the mold are shown in Table 1.
The defect rate is the ratio of the grindstone that was damaged when it was released from the molding die or a part of the grindstone surface that was peeled off and remained attached to the molding die.
The slidability of the grindstone was evaluated by a thrust type sliding test method. A silicon wafer coated with an insulating film was pressed from above the grindstone rotated at 20 cm / sec for 60 minutes while applying a load of 147 kP. The amount of wear of the grindstone after the test was measured and used as a guideline for evaluating the sliding characteristics.
表１に示すとおり、本発明による場合には実用的に支障のない研磨速度が得られる上に、表面粗さも細かく研磨痕もない高精度の研磨加工が達成されることが判る。
これに対して炭素繊維を使用しない比較例１では、研磨速度は速いものの、表面粗さが粗く、研磨痕も発生していることが判る。また、比較例２に示すように、炭素繊維を使用してもその直径が細く、アスペクト比が小さい炭素繊維を使用した場合には、表面粗さが粗く、研磨痕も発生していることが判る。
また、砥石に炭素繊維を添加することにより、離型性が改善されることが分かる。また、摩擦試験結果からも炭素繊維の添加により摺動性が改善され、砥石摩耗量の低減効果が確認された。
As shown in Table 1, according to the present invention, it can be seen that a polishing rate with practically no hindrance is obtained, and that a high-precision polishing process with fine surface roughness and no polishing marks is achieved.
On the other hand, in Comparative Example 1 in which no carbon fiber is used, it can be seen that although the polishing rate is high, the surface roughness is rough and polishing marks are also generated. In addition, as shown in Comparative Example 2, when carbon fiber is used, the diameter is thin and the carbon fiber having a small aspect ratio is used, so that the surface roughness is rough and polishing marks are generated. I understand.
Moreover, it turns out that a mold release property is improved by adding carbon fiber to a grindstone. Also, from the friction test results, the slidability was improved by the addition of carbon fiber, and the effect of reducing the amount of grinding wheel wear was confirmed.
（実施例３）
平均粒径３μｍの立方晶ボロンナイトライド８５質量％と平均粒径１０μｍのアルミニウム粉末を１５質量％、アルミニウム粉末に対し３０質量％の平均繊維径１５０ｎｍ、アスペクト比６７、ＢＥＴ比表面積が１３ｍ２／ｇ、ｄ００２が０．３３９ｎｍ、Ｉｄ／Ｉｇが０．１で、中心部が中空で積層構造を有するある気相法炭素繊維を、アセトンを添加して超硬ボールを用いて３時間湿式混合した。乾燥後、温度１４５０℃、圧力５．５ＧＰa、１時間の条件で焼結しφ３０mm、厚さ４mmの研磨用複合体を得た。平面研削盤、ダイヤモンド砥石で厚みを調整し、ワイヤーカット放電加工機で切断し、工具研削盤を用いて１２．７□mm×３．２tmmに仕上加工した。複合体の表面電気抵抗を測定し、焼結合金（硬度ＨＲＣ４５）を削る切削性能試験を実施した。
（実施例４）
実施例３と同じ立方晶ボロンナイトライド、アルミニウム粉末、気相法炭素繊維を用いて、質量比で、立方晶ボロンナイトライド９０％、アルミニウム粉末１０％、炭素繊維の添加量をアルミニウムに対して３０％添加した以外は全て実施例３と同条件で複合体を作製し、測定、試験を行った。複合体はワイヤーカット放電加工機で切断可能であった。
（実施例５）
実施例３と同じ原料を用い、質量比で、立方晶ボロンナイトライド９５％、アルミニウム粉末５％、炭素繊維の添加量をアルミニウムに対して３０％添加した以外は全て実施例３と同条件で複合体を作製し、加工、測定、試験を行った。
(Example 3)
85% by mass of cubic boron nitride having an average particle size of 3 μm, 15% by mass of aluminum powder having an average particle size of 10 μm, an average fiber diameter of 150 nm of 30% by mass with respect to the aluminum powder, an aspect ratio of 67, and a BET specific surface area of 13 m 2 / g, d002 of 0.339 nm, Id / Ig of 0.1, a vapor grown carbon fiber having a hollow center portion and a laminated structure was wet-mixed for 3 hours using cemented carbide balls with addition of acetone. . After drying, sintering was performed under conditions of a temperature of 1450 ° C., a pressure of 5.5 GPa, and 1 hour to obtain a polishing composite having a diameter of 30 mm and a thickness of 4 mm. The thickness was adjusted with a surface grinder and a diamond grindstone, cut with a wire cut electric discharge machine, and finished to 12.7 □ mm × 3.2 t mm using a tool grinder. The surface electrical resistance of the composite was measured, and a cutting performance test for cutting a sintered alloy (hardness HRC45) was performed.
(Example 4)
Using the same cubic boron nitride, aluminum powder and vapor grown carbon fiber as in Example 3, the mass ratio of cubic boron nitride 90%, aluminum powder 10%, and the amount of carbon fiber added to aluminum Except for the addition of 30%, a composite was prepared under the same conditions as in Example 3, and measured and tested. The composite could be cut with a wire cut electric discharge machine.
(Example 5)
The same raw materials as in Example 3 were used under the same conditions as in Example 3 except that 95% of cubic boron nitride, 5% of aluminum powder, and 30% of the amount of carbon fiber added to aluminum were added by mass ratio. A composite was produced and processed, measured, and tested.
（実施例６）
立方晶ボロンナイトライド、アルミニウム粉末の質量比は実施例３と同じ８５：１５とし、炭素繊維の添加量をアルミニウムに対して２５質量％添加し、以下実施例３と同条件で複合体を得、測定、試験を行った。
（実施例７）
立方晶ボロンナイトライド、アルミニウム粉末の質量比は実施例４と同じ９０：１０とし、炭素繊維の添加量をアルミニウムに対して５０質量％添加し、以下実施例３と同条件で複合体を得、測定、試験を行った。
（参考例１）
立方晶ボロンナイトライド、アルミニウム粉末の質量比は実施例３と同じ８５：１５とし、炭素繊維の添加量をアルミニウムに対して２０質量％添加し、以下実施例３と同条件で複合体を得、測定、試験を行った。ワイヤーカット放電加工機では切断できなかった。
（参考例２）
立方晶ボロンナイトライド、アルミニウム粉末の質量比は実施例４と同じ９０：１０とし、炭素繊維の添加量をアルミニウムに対して２０質量％添加し、以下実施例３と同条件で複合体を得、測定、試験を行った。ワイヤーカット放電加工機では切断できなかった。
（参考例３）
立方晶ボロンナイトライド、アルミニウム粉末の質量比は実施例５と同じ９５：５とし、炭素繊維の添加量をアルミニウムに対して２０質量％添加し、以下実施例３と同条件で複合体を得、測定、試験を行った。ワイヤーカット放電加工機では切断できなかった。
（参考例４）
立方晶ボロンナイトライド、アルミニウム粉末の質量比は実施例５と同じ９５：５とし、炭素繊維の添加量をアルミニウムに対して１００質量％添加し、以下実施例３と同条件で複合体を得、測定、試験を行った。ワイヤーカット放電加工機では切断できたが、切削性能試験において工具は欠損した。
（比較例３）
市販のアルミニウム化合物を結合材とする立方晶ボロンナイトライド工具で測定、試験を行った。
以上の結果を以下の表２に示す。
(Example 6)
The mass ratio of cubic boron nitride and aluminum powder was 85:15, which was the same as in Example 3, and the addition amount of carbon fiber was 25% by mass with respect to aluminum. Hereinafter, a composite was obtained under the same conditions as in Example 3. Measurements and tests were conducted.
(Example 7)
The mass ratio of cubic boron nitride and aluminum powder was 90:10, the same as in Example 4, and 50% by mass of carbon fiber was added to aluminum, and a composite was obtained under the same conditions as in Example 3 below. Measurements and tests were conducted.
(Reference Example 1)
The mass ratio of cubic boron nitride and aluminum powder was 85:15, the same as in Example 3, and 20% by mass of carbon fiber was added to aluminum, and a composite was obtained under the same conditions as in Example 3 below. Measurements and tests were conducted. It could not be cut with a wire cut electric discharge machine.
(Reference Example 2)
The mass ratio of cubic boron nitride and aluminum powder was 90:10, the same as in Example 4, and 20% by mass of carbon fiber was added to aluminum, and a composite was obtained under the same conditions as in Example 3 below. Measurements and tests were conducted. It could not be cut with a wire cut electric discharge machine.
(Reference Example 3)
The mass ratio of cubic boron nitride and aluminum powder was 95: 5, the same as in Example 5, 20% by mass of carbon fiber was added to aluminum, and a composite was obtained under the same conditions as in Example 3 below. Measurements and tests were conducted. It could not be cut with a wire cut electric discharge machine.
(Reference Example 4)
The mass ratio of cubic boron nitride and aluminum powder was 95: 5, which was the same as in Example 5, and the amount of carbon fiber added was 100% by mass with respect to aluminum, and a composite was obtained under the same conditions as in Example 3 below. Measurements and tests were conducted. Although the wire-cut electric discharge machine was able to cut, the tool was missing in the cutting performance test.
(Comparative Example 3)
Measurements and tests were conducted with a cubic boron nitride tool using a commercially available aluminum compound as a binder.
The above results are shown in Table 2 below.
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| JP2007138048A (en) * | 2005-11-18 | 2007-06-07 | Bussan Nanotech Research Institute Inc | Polishing material |
| JP2008229761A (en) * | 2007-03-19 | 2008-10-02 | Disco Abrasive Syst Ltd | Dry type grinding stone |
| JP5385653B2 (en) * | 2009-03-25 | 2014-01-08 | 株式会社アドマテックス | Polishing pad and polishing method |
| CN103639910B (en) * | 2013-12-04 | 2015-10-14 | 江苏锋芒复合材料科技集团有限公司 | A kind of high accuracy lapping tape and manufacture method thereof |
| CN104312190A (en) * | 2014-10-14 | 2015-01-28 | 荣成复合材料有限公司 | Composite material for lift pedals and cages |
| JP6351134B2 (en) * | 2017-05-29 | 2018-07-04 | 株式会社東京精密 | Sharpening tools |
| CN113927494B (en) * | 2021-10-29 | 2023-03-17 | 北京国瑞升科技股份有限公司 | Grinding belt and preparation method thereof |
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