WO2009151120A1 - アルミニウム酸化物粒子及びそれを含有する研磨用組成物 - Google Patents
アルミニウム酸化物粒子及びそれを含有する研磨用組成物 Download PDFInfo
- Publication number
- WO2009151120A1 WO2009151120A1 PCT/JP2009/060766 JP2009060766W WO2009151120A1 WO 2009151120 A1 WO2009151120 A1 WO 2009151120A1 JP 2009060766 W JP2009060766 W JP 2009060766W WO 2009151120 A1 WO2009151120 A1 WO 2009151120A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- aluminum oxide
- oxide particles
- polishing
- particles
- polishing composition
- Prior art date
Links
- 239000002245 particle Substances 0.000 title claims abstract description 170
- 238000005498 polishing Methods 0.000 title claims abstract description 141
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000000203 mixture Substances 0.000 title claims description 64
- 239000000758 substrate Substances 0.000 claims abstract description 41
- 239000011164 primary particle Substances 0.000 claims abstract description 35
- 239000011163 secondary particle Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 claims description 6
- 229910000510 noble metal Inorganic materials 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 abstract description 10
- 239000006061 abrasive grain Substances 0.000 abstract description 4
- LBDSXVIYZYSRII-IGMARMGPSA-N alpha-particle Chemical compound [4He+2] LBDSXVIYZYSRII-IGMARMGPSA-N 0.000 abstract 1
- -1 nickel-phosphorus) Chemical compound 0.000 description 30
- 229910052782 aluminium Inorganic materials 0.000 description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 19
- 230000007423 decrease Effects 0.000 description 19
- 235000002639 sodium chloride Nutrition 0.000 description 14
- 230000003746 surface roughness Effects 0.000 description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 6
- 239000003082 abrasive agent Substances 0.000 description 6
- 229910001593 boehmite Inorganic materials 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000002950 deficient Effects 0.000 description 6
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 6
- 239000007800 oxidant agent Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 229910052783 alkali metal Inorganic materials 0.000 description 5
- 150000007522 mineralic acids Chemical class 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- WDJHALXBUFZDSR-UHFFFAOYSA-N acetoacetic acid Chemical compound CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000004220 glutamic acid Substances 0.000 description 3
- 235000013922 glutamic acid Nutrition 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000010363 phase shift Effects 0.000 description 3
- 239000001103 potassium chloride Substances 0.000 description 3
- 235000011164 potassium chloride Nutrition 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 229910052594 sapphire Inorganic materials 0.000 description 3
- 239000010980 sapphire Substances 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229920003169 water-soluble polymer Polymers 0.000 description 3
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 229910001680 bayerite Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 229910001679 gibbsite Inorganic materials 0.000 description 2
- 159000000014 iron salts Chemical class 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 150000002815 nickel Chemical class 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- QBYIENPQHBMVBV-HFEGYEGKSA-N (2R)-2-hydroxy-2-phenylacetic acid Chemical compound O[C@@H](C(O)=O)c1ccccc1.O[C@@H](C(O)=O)c1ccccc1 QBYIENPQHBMVBV-HFEGYEGKSA-N 0.000 description 1
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 description 1
- QLCAGXDTDCDEGN-UHFFFAOYSA-N 3-sulfanylcarbonylhexanedioic acid Chemical compound OC(=O)CCC(C(O)=S)CC(O)=O QLCAGXDTDCDEGN-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
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- IWYDHOAUDWTVEP-UHFFFAOYSA-N R-2-phenyl-2-hydroxyacetic acid Natural products OC(=O)C(O)C1=CC=CC=C1 IWYDHOAUDWTVEP-UHFFFAOYSA-N 0.000 description 1
- 229910000929 Ru alloy Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- LEVVHYCKPQWKOP-UHFFFAOYSA-N [Si].[Ge] Chemical compound [Si].[Ge] LEVVHYCKPQWKOP-UHFFFAOYSA-N 0.000 description 1
- RUSUZAGBORAKPY-UHFFFAOYSA-N acetic acid;n'-[2-(2-aminoethylamino)ethyl]ethane-1,2-diamine Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCNCCNCCN RUSUZAGBORAKPY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 1
- 239000005354 aluminosilicate glass Substances 0.000 description 1
- 229940063656 aluminum chloride Drugs 0.000 description 1
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 1
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- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
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- 239000003054 catalyst Substances 0.000 description 1
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- 239000002537 cosmetic Substances 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
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- 150000004985 diamines Chemical class 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
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- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
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- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 description 1
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- 239000007937 lozenge Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
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- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
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- 230000001590 oxidative effect Effects 0.000 description 1
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- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
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- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
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- 239000011780 sodium chloride Substances 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
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- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/11—Lapping tools
- B24B37/20—Lapping pads for working plane surfaces
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/39—Particle morphology extending in three dimensions parallelepiped-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Definitions
- the present invention relates to aluminum oxide particles comprising an aluminum oxide comprising alumina such as ⁇ -alumina and transition alumina, and alumina hydrate such as boehmite, and a polishing composition containing the same.
- Aluminum oxide particles are used as abrasive grains in applications for polishing substrates used for electronic components such as semiconductor device substrates, substrates for displays, hard disk substrates, sapphire substrates for LEDs, and the like. Since these substrates are required to have high smoothness and low defects, the particle size of the aluminum oxide particles used is relatively small (for example, Patent Documents 1 and 2).
- the polishing composition containing aluminum oxide particles as free abrasives generally has a higher polishing rate (removal rate) of the substrate than the polishing composition containing colloidal silica as free abrasives.
- the polishing rate of the substrate by the polishing composition generally decreases as the particle size of the aluminum oxide particles decreases.
- it becomes difficult to remove the aluminum oxide particles attached to the surface of the substrate after polishing by cleaning that is, the cleaning properties of the aluminum oxide particles decrease). .
- the present invention contains aluminum oxide particles and aluminum oxide particles that can be suitably used as abrasive grains without causing adverse effects such as a decrease in polishing speed and a decrease in washability even if the particle size is small.
- An object of the present invention is to provide a polishing composition.
- aluminum oxide particles are provided in which the primary particles are hexahedral in shape and the primary particles have an aspect ratio of 1 to 5.
- the average primary particle size of the aluminum oxide particles is preferably 0.01 to 0.6 ⁇ m.
- the alpha conversion rate of the aluminum oxide particles is preferably 5 to 70%.
- the average secondary particle size of the aluminum oxide particles is preferably 0.01 to 2 ⁇ m, and the value obtained by dividing the 90% particle size of the aluminum oxide particles by the 10% particle size is 3 or less Is preferred.
- a polishing composition comprising the above-described aluminum oxide particles and water.
- the present invention contains aluminum oxide particles and aluminum oxide particles that can be suitably used as abrasives without causing adverse effects such as a decrease in polishing speed and a decrease in washability even if the particle size is small.
- a polishing composition is provided.
- the scanning electron micrograph which shows an example of the aluminum oxide particle of one Embodiment of this invention.
- the two scanning electron micrographs which show another example of the aluminum oxide particle of the same embodiment.
- the primary particles have a hexahedral shape.
- the primary particles of the aluminum oxide particles are preferably parallelepipeds surrounded by two squares facing each other and four rectangles or squares, or parallelepipeds surrounded by two lozenges facing each other and four rectangles or squares It has an external shape similar to An example of the former is shown in FIG. 1 and an example of the latter is shown in FIG.
- the aspect ratio of the primary particles of the aluminum oxide particles is in the range of 1 to 5.
- the aspect ratio is a when the length of the longest side of the three sides extending from one vertex of the aluminum oxide primary particle having a hexahedral shape is a and the length of the shortest side is c. It is defined as the divided value.
- the length b of one remaining side is preferably approximately equal to the length a of the longest side.
- the aspect ratio of primary particles is preferably as small as possible.
- the aspect ratio of the primary particles of the aluminum oxide particles is preferably 3 or less, more preferably 2 or less, and still more preferably 1.5 or less.
- the aluminum oxide particles of the present embodiment include, for example, metals (including simple metals such as copper, aluminum, tungsten, platinum, palladium, and ruthenium, and metallic alloys such as nickel-phosphorus), semiconductors (such as germanium and silicon) Semiconductor, Compound semiconductors such as germanium silicon, gallium arsenide, indium phosphide, gallium nitride, and oxide semiconductors such as sapphire) or insulators (glass such as aluminosilicate glass), urethane resin, acrylic resin, polycarbonate resin, etc. Used as an abrasive in the application which grind
- metals including simple metals such as copper, aluminum, tungsten, platinum, palladium, and ruthenium, and metallic alloys such as nickel-phosphorus
- semiconductors such as germanium and silicon
- Semiconductor Compound semiconductors such as germanium silicon, gallium arsenide, indium phosphi
- aluminum oxide particles are obtained by polishing the wiring of a semiconductor device substrate made of a base metal such as aluminum or copper or a noble metal such as platinum, palladium, or ruthenium, or on the surface of a nickel-phosphorus plated hard disk substrate. It is used in polishing, polishing of glass disk substrate, polishing of plastic lens for glasses, polishing of color filter substrate for liquid crystal display, and polishing of sapphire substrate for LED.
- Aluminum oxide particles may be used as free abrasives or as fixed abrasives.
- the aluminum oxide particles of the present embodiment when used as abrasive particles, have the preferred ranges described below with regard to the average primary particle size, the average secondary particle size, the particle size distribution, and the degree of conversion.
- the average primary particle size of the aluminum oxide particles is preferably 0.01 ⁇ m or more, more preferably 0.03 ⁇ m or more, and still more preferably 0.05 ⁇ m or more.
- the average primary particle diameter is defined as an average value of the lengths of the longest sides among the three sides extending from one vertex of the aluminum oxide primary particles having a hexahedral shape.
- the polishing rate removal rate
- the polishing rate should be improved to a practically suitable level. Becomes easy.
- the average primary particle size of the aluminum oxide particles is preferably 0.6 ⁇ m or less, more preferably 0.35 ⁇ m or less, and particularly preferably 0.25 ⁇ m or less.
- the average primary particle size of the aluminum oxide particles decreases, the number of scratches and the surface roughness of the object to be polished after polishing with the aluminum oxide particles decrease.
- the average primary particle diameter of the aluminum oxide particles is 0.6 ⁇ m or less, more specifically 0.35 ⁇ m or less or 0.25 ⁇ m or less, the number of scratches and the surface roughness are particularly suitable for practical use. It is easy to reduce the average primary particle diameter of the aluminum oxide particles.
- the average secondary particle size of the aluminum oxide particles is preferably 0.01 ⁇ m or more, more preferably 0.03 ⁇ m or more, and still more preferably 0.05 ⁇ m or more.
- the average secondary particle diameter is finally integrated when the volumes of aluminum oxide particles are integrated in the order of smaller particle diameter by the laser confusion method until it becomes 50% or more of the integrated volume of all the particles of aluminum oxide particles Is equal to the particle size of the aluminum oxide particles.
- the polishing rate of the object to be polished by the aluminum oxide particles is improved.
- the polishing rate and the cleaning property are particularly suitable for practical use. It becomes easy to improve.
- the average secondary particle diameter of the aluminum oxide particles is preferably 2 ⁇ m or less, more preferably 1 ⁇ m or less, and still more preferably 0.5 ⁇ m or less.
- the average secondary particle size of the aluminum oxide particles decreases, the number of scratches and the surface roughness of the object to be polished after polishing with the aluminum oxide particles decrease.
- the average secondary particle diameter of the aluminum oxide particles is 2 ⁇ m or less, more preferably 1 ⁇ m or less or 0.5 ⁇ m or less, the number of scratches and the surface roughness are reduced to a practically suitable level. Becomes easy.
- the value D90 / D10 obtained by dividing 90% particle size (D90) of aluminum oxide particles by 10% particle size (D10) is preferably 3 or less, more preferably 2.5 or less More preferably, it is 2.2 or less, and particularly preferably 2.0 or less.
- the 90% particle diameter is finally integrated when the volume of aluminum oxide particles is integrated in the order of smaller particle diameter by the laser confusion method until it becomes 90% or more of the integrated volume of all the particles of aluminum oxide particles.
- the volume of aluminum oxide particles is integrated in the order of smaller particle diameter by the laser confusion method until the particle diameter of aluminum oxide particles is equal to 10% and the particle diameter is 10% or more of the integrated volume of all particles of aluminum oxide particles.
- the scratch number and the surface roughness are particularly preferable practically. It is easy to reduce it to such a level and to improve the washability to a practically suitable level.
- the lower limit of the value D90 / D10 is not particularly limited, but is preferably 1.1 or more, more preferably 1.2 or more, and particularly preferably 1.3 or more.
- the aluminum oxide particles may have any crystal form, for example, alumina hydrate such as boehmite, transition alumina such as ⁇ -alumina, ⁇ -alumina, ⁇ -alumina, And any of ⁇ -alumina may be used.
- the aluminum oxide particles preferably contain at least a part of ⁇ -alumina.
- the alpha conversion rate of the aluminum oxide particles is preferably 5% or more, more preferably 10% or more, and still more preferably 20% or more.
- the rate of ⁇ -conversion is a value determined by X-ray diffraction based on comparison with corundum.
- the polishing rate of the object to be polished by the aluminum oxide particles is improved as the degree of alpha conversion of the aluminum oxide particles is increased.
- the alpha conversion ratio of the aluminum oxide particles is 5% or more, more specifically 10% or more or 20% or more, it becomes easy to improve the polishing rate to a practically suitable level in practice. .
- the alpha conversion ratio of the aluminum oxide particles is preferably 70% or less, more preferably 50% or less, and particularly preferably 30% or less.
- the number of scratches and the surface roughness of the object to be polished after polishing by the aluminum oxide particles decrease as the degree of alpha conversion of the aluminum oxide particles decreases.
- the alpha conversion ratio of the aluminum oxide particles is 70% or less, more preferably 50% or less or 30% or less, the number of scratches and the surface roughness are reduced to a practically suitable level in practice. Becomes easy.
- the aluminum oxide particles of this embodiment are used, for example, in the form of a slurry-like polishing composition prepared by mixing at least with water.
- a polishing composition for polishing the surface of a nickel-phosphorus plated hard disk comprises aluminum oxide particles, preferably together with a polishing accelerator, and more preferably water, together with a polishing accelerator, a cleaning accelerator and an oxidizing agent. Mixed and prepared.
- the polishing composition for polishing a display substrate is prepared, for example, by mixing aluminum oxide particles with water.
- the polishing composition for polishing the wiring of the semiconductor device substrate is prepared by mixing aluminum oxide particles, preferably together with a polishing accelerator and an oxidizing agent, in water.
- the content of aluminum oxide particles in the polishing composition is preferably 0.01% by mass or more, and more preferably 0.1% by mass or more.
- the polishing rate of the object to be polished by the polishing composition is improved as the content of the aluminum oxide particles is increased.
- the polishing rate is set to a practically suitable level in practice. It becomes easy to improve.
- the content of aluminum oxide particles in the polishing composition is preferably 30% by mass or less, more preferably 15% by mass or less. As the content of the aluminum oxide particles decreases, the dispersibility of the aluminum oxide particles in the polishing composition is improved. In this respect, when the content of the aluminum oxide particles in the polishing composition is 30% by mass or less, more preferably 15% by mass or less, the dispersibility of the aluminum oxide particles in the polishing composition is It becomes easy to improve to the level especially suitable practically.
- the polishing accelerator is added to the polishing composition as needed in order to improve the polishing rate of the object to be polished by the polishing composition.
- a polishing accelerator that can be added to the polishing composition for example, organic acids and salts thereof, inorganic acids and salts thereof, alkali compounds (including alkali metal hydroxides, ammonia, amines, and quaternary ammonium compounds) Can be mentioned.
- organic acid examples include citric acid, maleic acid, maleic anhydride, malic acid, glycolic acid, succinic acid, itaconic acid, malonic acid, iminodiacetic acid, gluconic acid, lactic acid, mandelic acid, tartaric acid, crotonic acid, Nicotinic acid, acetic acid, thiomalic acid, formic acid, oxalic acid, carboxyethyl thiosuccinic acid can be mentioned.
- Ammonium salts, alkali metal salts, transition metal salts (including iron salts, nickel salts and aluminum salts) of these organic acids can also be used as polishing accelerators.
- the inorganic acid examples include hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid.
- Ammonium salts, alkali metal salts, transition metal salts (including iron salts, nickel salts and aluminum salts) of these inorganic acids can also be used as polishing accelerators.
- alkali metal hydroxide examples include potassium hydroxide, sodium hydroxide and lithium hydroxide.
- amine examples include monoamines such as methylamine and ethylamine, diamines such as ethylene diamine, and alkanolamines such as monoethanolamine and triethanolamine.
- quaternary ammonium compounds include tetraalkyl ammonium compounds such as tetramethyl ammonium compounds, tetraethyl ammonium compounds and tetrapropyl ammonium compounds.
- the polishing accelerator used in the polishing composition for polishing the surface of a nickel-phosphorus plated hard disk substrate is preferably an inorganic acid salt, in particular an inorganic aluminum salt such as aluminum nitrate, aluminum sulfate, aluminum chloride It is.
- an inorganic aluminum salt such as aluminum nitrate, aluminum sulfate, aluminum chloride It is.
- the polishing rate by the polishing composition is particularly greatly improved without causing the increase in the number of scratches and the surface roughness of the substrate after polishing by the polishing composition.
- the polishing accelerator used in the polishing composition for polishing the wiring of the semiconductor device substrate is preferably an inorganic acid or an organic acid, particularly nitric acid, sulfuric acid or citric acid.
- Polishing accelerators used in other polishing compositions are preferably alkali metal salts of inorganic acids, in particular potassium chloride, sodium chloride, potassium nitrate, sodium nitrate, sodium sulfate, potassium sulfate, sodium sulfate. These alkali metal salts promote aggregation of aluminum oxide particles in the polishing composition, and as a result, the polishing rate by the polishing composition is particularly greatly improved.
- the cleaning accelerator is added to the polishing composition as needed for the purpose of improving the cleaning properties of the aluminum oxide particles. It is also possible to use any chelating compound as a washing accelerator. Specific washing accelerators include diethylenetriaminepentaacetic acid, hydroxyethylethylenediaminetriacetic acid, triethylenetetramine hexaacetic acid, glutamic acid diacetic acid, and alkali metal salts and ammonium salts of these acids.
- the oxidizing agent is added to the polishing composition as needed in order to improve the polishing rate of the object to be polished by the polishing composition.
- any substance having an oxidizing action can be used as an oxidizing agent, hydrogen peroxide which is easy to handle, or a persulfate such as ammonium persulfate, sodium persulfate or potassium persulfate is preferably used.
- raw material particles consisting of alumina hydrate in which the shape of the primary particles is hexahedral can be maintained so that the shape of the primary particles of the raw material particles is substantially maintained. It can be manufactured by baking.
- Aluminum oxide particles mainly composed of ⁇ -alumina are produced by calcinating raw material particles consisting of transition alumina in which the shape of the primary particles is hexahedron so that the shape of the primary particles of the raw material particles is substantially maintained.
- the primary particle of the raw material particle has an outer shape close to a parallelepiped surrounded by two squares facing each other and four rectangles or squares, or a parallelepiped surrounded by two rhombuses facing each other and four rectangles or squares It is preferable to have
- the alumina hydrate may be any of gibbsite, bayerite, nostrandite, and boehmite.
- the calcination temperature is, for example, 500 to 1250 ° C.
- Aluminum oxide particles mainly composed of boehmite are prepared by hydrothermally treating a slurry containing 1 to 30% by mass of gibbsite particles or bayerite particles having an average primary particle diameter of 10 ⁇ m or less at 200 ° C. for 4 hours in an autoclave It can be manufactured.
- the embodiment may be modified as follows.
- the aluminum oxide particles of the embodiment may be used in applications such as fillers for resins, pigments, coating agents, cosmetics, catalysts, ceramic raw materials, etc. in addition to applications as abrasive grains.
- the polishing composition of the embodiment may further contain a surfactant, if necessary. In this case, the number of scratches on the object to be polished after polishing is reduced.
- the polishing composition of the embodiment may further contain a water-soluble polymer, if necessary. In this case, the number of scratches on the object to be polished after polishing is reduced.
- Specific examples of the water-soluble polymer include polysaccharides such as hydroxyethyl cellulose, pullulan and carrageenan, and synthetic water-soluble polymers such as polyvinyl alcohol and polyvinyl pyrrolidone.
- the polishing composition of the embodiment may be prepared by diluting a stock solution of the polishing composition with water.
- the present invention will be more specifically described by way of examples and comparative examples.
- any of aluminum compound particles represented by “A” to “P” in Table 1 can be treated with aluminum nitrate nonahydrate or aluminum chloride hexahydrate
- the polishing composition was prepared by mixing it with water together with tetrasodium glutamic acid diacetate (cleaning accelerator) and hydrogen peroxide (oxidizing agent).
- tetrasodium glutamic acid diacetate cleaning accelerator
- hydrogen peroxide oxidizing agent
- aluminum nitrate nonahydrate, glutamic acid diacetic acid tetrasodium salt and hydrogen peroxide were mixed in water to prepare a polishing composition.
- the shape shown in the “Primary particle shape” column in Table 1 is based on the result of observing the primary particle shape of each aluminum compound particle using a scanning electron microscope “S-4700” manufactured by Hitachi High-Technologies Corporation.
- Each numerical value shown in the “aspect ratio” column in Table 1 is an average value of the aspect ratio measured with 200 aluminum compound particles based on observation with a scanning electron microscope “S-4700”.
- Each numerical value shown in the "alpha conversion ratio” column of Table 1 is alpha conversion of each aluminum compound particle determined based on comparison with corundum using an X-ray diffractometer "Mini Flex II” manufactured by Rigaku Corporation. It is a rate.
- Each numerical value shown in the "average primary particle diameter” column in Table 1 is the average primary particle diameter of each aluminum compound particle measured based on observation with a scanning electron microscope "S-4700".
- Each numerical value shown in the "average secondary particle diameter” column in Table 1 is the value of each aluminum compound particle measured using a laser diffraction / scattering particle size distribution measuring device "LA-950" manufactured by Horiba, Ltd. It is an average secondary particle diameter.
- Each numerical value shown in the "D90 / D10" column in Table 1 is the 90% particle size and 10% particle size of each aluminum compound particle measured using a laser diffraction / scattering particle size distribution measuring apparatus "LA-950". It is the value D90 / D10 calculated from the diameter.
- the aluminum compound particles represented by "A” to “R” in Table 1 are alumina particles mainly composed of alumina, the aluminum compound particles represented by “S” are boehmite particles mainly composed of boehmite, "T”
- the substrate is rinsed with pure water and rinsed, and then arithmetic mean roughness Ra of the substrate surface after polishing is performed using “Micro XAM” manufactured by Phase Shift.
- arithmetic mean roughness Ra of the substrate surface after polishing is performed using “Micro XAM” manufactured by Phase Shift.
- the results of measuring the surface roughness of the substrate after polishing using the “Arithmetic average roughness Ra” column in Table 2 and “Opti Flat” manufactured by Phase Shift, Inc. are shown in Table 2.
- the arithmetic mean swell Wa is shown in the column.
- the number of scratches on the substrate surface after being polished using the polishing composition of each example and then rinsed with pure water was measured. Specifically, the number of scratches was visually measured while irradiating the surface of the substrate with the light of the surface inspection lamp “F100Z” manufactured by Funakoshi Pharmaceutical Co., Ltd. Excellent ( ⁇ ) if the number of scratches measured is less than 30; good ( ⁇ ) if it is 30 or more and less than 50; OK (50) if 50 or more and less than 75; 75 or more and less than 100 In the case of 1, the results evaluated as somewhat defective ( ⁇ ) and in the case of 100 or more as defective ( ⁇ ) are shown in the “scratch number” column of Table 2.
- the polishing composition was prepared by mixing any of the aluminum compound particles shown by "A”, “B”, “D”, “Q”, “S” and “T” in Table 1 with water.
- the types and contents of aluminum compound particles contained in the polishing composition of each example and the pH of the polishing composition of each example are as shown in Table 4.
- the polishing rate when the surface of the acrylic resin substrate for a display was polished under the conditions shown in Table 5 was determined based on the difference in substrate thickness before and after polishing. This is shown in the column "Polishing rate" of No.
- the substrate is rinsed with pure water and rinsed, and then arithmetic mean roughness Ra of the substrate surface after polishing is performed using “Micro XAM” manufactured by Phase Shift. The results of measurement of are shown in the "arithmetic mean roughness Ra" column of Table 4.
- the number of scratches on the substrate surface after being polished using the polishing composition of each example and then rinsed with pure water was measured. Specifically, the number of scratches was visually measured while irradiating the surface of the substrate with the light of the surface inspection lamp “F100Z” manufactured by Funakoshi Pharmaceutical Co., Ltd. If the number of scratches measured is less than 50, it is good ( ⁇ ), if it is 50 or more and less than 75, it is good ( ⁇ ). If it is 75 or more and less than 100, it is somewhat defective ( ⁇ ). The result of having been evaluated as defective ( ⁇ ) is shown in the “scratch number” column of Table 4.
- Examples 31, 32 and Comparative Example 31 Mix any of the aluminum compound particles shown in “A” and “R” in Table 1 with water, hydrochloric acid (polishing accelerator), potassium chloride (polishing accelerator) and hydrogen peroxide (oxidizing agent) in water.
- a polishing composition was prepared.
- the type and content of the aluminum compound particles contained in the polishing composition of each example and the pH of the polishing composition of each example are as shown in Table 6.
- the content of hydrochloric acid, the content of potassium chloride and the content of hydrogen peroxide in the polishing composition of each example are 1.2 g / L and 18.8 g / L for any of the polishing compositions, respectively. L and 34.2 g / L.
- the polishing rate when polishing the surface of a semiconductor device substrate dotted with pads consisting of 70 ⁇ m ⁇ 70 ⁇ m under the conditions shown in Table 7 is the weight of the substrate before and after polishing.
- the results obtained on the basis of the difference are shown in the "polishing speed" column of Table 6.
- the number of scratches on the substrate surface after being polished using the polishing composition of each example and then rinsed with pure water was measured. Specifically, the number of scratches was visually measured while irradiating the surface of the substrate with the light of the surface inspection lamp “F100Z” manufactured by Funakoshi Pharmaceutical Co., Ltd. If the number of scratches measured is less than 50, it is good ( ⁇ ), if it is 50 or more and less than 75, it is good ( ⁇ ). If it is 75 or more and less than 100, it is somewhat defective ( ⁇ ). The result of having been evaluated as defective ( ⁇ ) is shown in the “scratch number” column of Table 6.
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Abstract
Description
本実施形態のアルミニウム酸化物粒子は、一次粒子の形状が六面体をなしている。アルミニウム酸化物粒子の一次粒子は、好ましくは、向かい合った2つの正方形と4つの長方形又は正方形とで囲まれた平行六面体、あるいは向かい合った2つの菱形と4つの長方形又は正方形とで囲まれた平行六面体に近似した外形形状を有する。前者の例を図1、後者の例を図2に示す。
平均一次粒子径に関して
アルミニウム酸化物粒子の平均一次粒子径は、0.01μm以上であることが好ましく、より好ましくは0.03μm以上、さらに好ましくは0.05μm以上である。ここで平均一次粒子径は、六面体形状を有するアルミニウム酸化物一次粒子の一つの頂点から延びる3辺のうち最も長い辺の長さの平均値として定義される。アルミニウム酸化物粒子の平均一次粒子径が大きくなるにつれて、アルミニウム酸化物粒子による研磨対象物の研磨速度(除去速度)は向上する。この点、アルミニウム酸化物粒子の平均一次粒子径が0.01μm以上、さらに言えば0.03μm以上又は0.05μm以上である場合には、研磨速度を実用上特に好適なレベルにまで向上させることが容易となる。
アルミニウム酸化物粒子の平均二次粒子径は、0.01μm以上であることが好ましく、より好ましくは0.03μm以上、さらに好ましくは0.05μm以上である。ここで平均二次粒子径は、アルミニウム酸化物粒子の全粒子の積算体積の50%以上になるまでレーザー錯乱法による粒子径の小さい順にアルミニウム酸化物粒子の体積を積算したときに最後に積算されるアルミニウム酸化物粒子の粒子径に等しい。アルミニウム酸化物粒子の平均二次粒子径が大きくなるにつれて、アルミニウム酸化物粒子による研磨対象物の研磨速度は向上する。また、アルミニウム酸化物粒子による研磨後の研磨対象物の表面に付着したアルミニウム酸化物粒子を洗浄により除去することが容易になる(すなわち、アルミニウム酸化物粒子の洗浄性が向上する)。この点、アルミニウム酸化物粒子の平均二次粒子径が0.01μm以上、さらに言えば0.03μm以上又は0.05μm以上である場合には、研磨速度及び洗浄性を実用上特に好適なレベルにまで向上させることが容易となる。
アルミニウム酸化物粒子の90%粒子径(D90)を10%粒子径(D10)で除して得られる値D90/D10は3以下であることが好ましく、より好ましくは2.5以下、さらに好ましくは2.2以下、特に好ましくは2.0以下である。ここで90%粒子径は、アルミニウム酸化物粒子の全粒子の積算体積の90%以上になるまでレーザー錯乱法による粒子径の小さい順にアルミニウム酸化物粒子の体積を積算したときに最後に積算されるアルミニウム酸化物粒子の粒子径に等しく、10%粒子径は、アルミニウム酸化物粒子の全粒子の積算体積の10%以上になるまでレーザー錯乱法による粒子径の小さい順にアルミニウム酸化物粒子の体積を積算したときに最後に積算されるアルミニウム酸化物粒子の粒子径に等しい。アルミニウム酸化物粒子の値D90/D10が小さくなるにつれて、アルミニウム酸化物粒子中に含まれるスクラッチ数及び表面粗さの増大の原因となる粗大粒子の割合が少なくなるため、アルミニウム酸化物粒子による研磨後の研磨対象物のスクラッチ数及び表面粗さは低減する。また、アルミニウム酸化物粒子中に含まれる洗浄性の低下の原因となる微小粒子の割合も少なくなるため、研磨後の研磨対象物の表面に付着したアルミニウム酸化物粒子を洗浄により除去することが容易になる。この点、アルミニウム酸化物粒子の値D90/D10が3以下、さらに言えば2.5以下、2.2以下又は2.0以下である場合には、スクラッチ数及び表面粗さを実用上特に好適なレベルにまで低減させること及び洗浄性を実用上特に好適なレベルにまで向上させることが容易となる。
α化率に関して
アルミニウム酸化物粒子は、いずれの結晶形態を有していてもよく、例えば、ベーマイトのようなアルミナ水和物、γ-アルミナやδ-アルミナ、θ-アルミナのような遷移アルミナ、及びα-アルミナのいずれを主とするものであってもよい。ただし、高硬度が要求される場合には、アルミニウム酸化物粒子はα-アルミナを少なくとも一部含有していることが好ましい。アルミニウム酸化物粒子のα化率は5%以上であることが好ましく、より好ましくは10%以上、さらに好ましくは20%以上である。ここでα化率は、X線回折法によりコランダムとの比較に基づいて求められる値である。アルミニウム酸化物粒子のα化率が高くなるにつれて、アルミニウム酸化物粒子による研磨対象物の研磨速度は向上する。この点、アルミニウム酸化物粒子のα化率が5%以上、さらに言えば10%以上又は20%以上である場合には、研磨速度を実用上特に好適なレベルにまで向上させることが容易となる。
アミンの具体例としては、メチルアミン、エチルアミンなどのモノアミン、エチレンジアミンなどのジアミン、モノエタノールアミン、トリエタノールアミンなどのアルカノールアミンが挙げられる。
その他の研磨用組成物で使用される研磨促進剤は、好ましくは無機酸のアルカリ金属塩、特に、塩化カリウム、塩化ナトリウム、硝酸カリウム、硝酸ナトリウム、硫酸カリウム、硫酸ナトリウムである。これらのアルカリ金属塩は、研磨用組成物中のアルミニウム酸化物粒子の凝集を促し、結果として研磨用組成物による研磨速度を特に大きく向上する。
α-アルミナ又は遷移アルミナを主とするアルミニウム酸化物粒子は、一次粒子の形状が六面体をなすアルミナ水和物からなる原料粒子を、原料粒子の一次粒子の形状がほぼ維持されるように、か焼することにより製造することができる。α-アルミナを主とするアルミニウム酸化物粒子は、一次粒子の形状が六面体をなす遷移アルミナからなる原料粒子を、原料粒子の一次粒子の形状がほぼ維持されるように、か焼することにより製造することもできる。原料粒子の一次粒子は、向かい合った2つの正方形と4つの長方形又は正方形とで囲まれた平行六面体、あるいは向かい合った2つの菱形と4つの長方形又は正方形とで囲まれた平行六面体に近似した外形形状を有することが好ましい。アルミナ水和物は、ギブサイト、バイヤライト、ノストランダイト、ベーマイトのいずれであってもよい。か焼温度は、例えば500~1250℃である。
前記実施形態のアルミニウム酸化物粒子は、砥粒としての用途のほかに、樹脂用フィラー、顔料、塗工剤、化粧品、触媒、セラミック原料などの用途で使用されてもよい。
前記実施形態の研磨用組成物は、必要に応じてさらに水溶性高分子を含有してもよい。この場合、研磨後の研磨対象物のスクラッチ数が低減する。水溶性高分子の具体例としては、ヒドロキシエチルセルロース、プルラン、カラギーナンなどの多糖類、ポリビニルアルコール、ポリビニルピロリドンなどの合成水溶性高分子が挙げられる。
次に、実施例及び比較例を挙げて本発明をさらに具体的に説明する。
実施例1~17及び比較例1~5では、表1中の“A”~“P”で示すアルミニウム化合物粒子のいずれかを、硝酸アルミニウム九水和物又は塩化アルミニウム六水和物(研磨促進剤)、グルタミン酸二酢酸四ナトリウム塩(洗浄促進剤)及び過酸化水素(酸化剤)とともに、水に混合して研磨用組成物を調製した。比較例6では、硝酸アルミニウム九水和物、グルタミン酸二酢酸四ナトリウム塩及び過酸化水素を水に混合して研磨用組成物を調製した。各例の研磨用組成物中に含まれるアルミニウム化合物粒子の種類及び含有量並びに研磨促進剤の種類及び含有量はそれぞれ、表2の“アルミニウム化合物粒子の種類”欄、“アルミニウム化合物粒子の含有量”欄、“研磨促進剤の種類”欄及び“研磨促進剤の含有量”欄に示すとおりである。また、各例の研磨用組成物中のグルタミン酸二酢酸の含有量及び過酸化水素の含有量はそれぞれ、いずれの研磨用組成物の場合も0.3g/L及び13g/Lである。
表1中の“A”、“B”、“D”、“Q”、“S”、“T”で示すアルミニウム化合物粒子のいずれかを水に混合して研磨用組成物を調製した。各例の研磨用組成物中に含まれるアルミニウム化合物粒子の種類及び含有量並びに各例の研磨用組成物のpHは表4中に示すとおりである。
表1中の“A”、“R”に示すアルミニウム化合物粒子のいずれかを、塩酸(研磨促進剤)、塩化カリウム(研磨促進剤)及び過酸化水素(酸化剤)とともに、水に混合して研磨用組成物を調製した。各例の研磨用組成物中に含まれるアルミニウム化合物粒子の種類及び含有量並びに各例の研磨用組成物のpHは表6中に示すとおりである。また、各例の研磨用組成物中の塩酸の含有量、塩化カリウムの含有量及び過酸化水素の含有量はそれぞれ、いずれの研磨用組成物の場合も1.2g/L、18.8g/L及び34.2g/Lである。
Claims (9)
- 一次粒子の形状が六面体をなし、一次粒子のアスペクト比が1~5であることを特徴とするアルミニウム酸化物粒子。
- 平均一次粒子径が0.01~0.6μmである請求項1に記載のアルミニウム酸化物粒子。
- α化率が5~70%である請求項1又は2に記載のアルミニウム酸化物粒子。
- 平均二次粒子径が0.01~2μmであり、90%粒子径を10%粒子径で除して得られる値が3以下である請求項1~3のいずれか一項に記載のアルミニウム酸化物粒子。
- 電子部品に用いる基板を研磨する用途で砥粒として使用される請求項1~4のいずれか一項に記載のアルミニウム酸化物粒子。
- ニッケル-リンめっきされた研磨対象物の表面を研磨する用途で砥粒として使用される請求項1~4のいずれか一項に記載のアルミニウム酸化物粒子。
- 貴金属からなる研磨用組成物を研磨する用途で砥粒として使用される請求項1~4のいずれか一項に記載のアルミニウム酸化物粒子。
- 樹脂からなる研磨対象物を研磨する用途で砥粒として使用される請求項1~4のいずれか一項に記載のアルミニウム酸化物粒子。
- 請求項1~4のいずれか一項に記載のアルミニウム酸化物粒子と水を含有することを特徴とする研磨用組成物。
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US12/997,455 US20110258938A1 (en) | 2008-06-13 | 2009-06-12 | Aluminum oxide particle and polishing composition containing the same |
CN200980130486.8A CN102105266B (zh) | 2008-06-13 | 2009-06-12 | 氧化铝颗粒以及包含该氧化铝颗粒的抛光组合物 |
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Also Published As
Publication number | Publication date |
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KR101268007B1 (ko) | 2013-05-27 |
US20110258938A1 (en) | 2011-10-27 |
KR20110038035A (ko) | 2011-04-13 |
EP2322322A1 (en) | 2011-05-18 |
CN102105266A (zh) | 2011-06-22 |
EP2322322B1 (en) | 2013-03-13 |
TW201000403A (en) | 2010-01-01 |
JP5204226B2 (ja) | 2013-06-05 |
EP2322322A4 (en) | 2011-09-07 |
EP2322322B2 (en) | 2022-10-05 |
CN102105266B (zh) | 2016-01-13 |
TWI417245B (zh) | 2013-12-01 |
JPWO2009151120A1 (ja) | 2011-11-17 |
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