CN1673306B - Polishing composition - Google Patents
Polishing composition Download PDFInfo
- Publication number
- CN1673306B CN1673306B CN2005100590654A CN200510059065A CN1673306B CN 1673306 B CN1673306 B CN 1673306B CN 2005100590654 A CN2005100590654 A CN 2005100590654A CN 200510059065 A CN200510059065 A CN 200510059065A CN 1673306 B CN1673306 B CN 1673306B
- Authority
- CN
- China
- Prior art keywords
- substrate
- grinding
- silicon oxide
- oxide particle
- liquid composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 144
- 238000005498 polishing Methods 0.000 title claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 167
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 137
- 238000000034 method Methods 0.000 claims abstract description 78
- 238000004519 manufacturing process Methods 0.000 claims abstract description 37
- 238000000227 grinding Methods 0.000 claims description 247
- 239000002245 particle Substances 0.000 claims description 137
- 239000007788 liquid Substances 0.000 claims description 120
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 112
- 239000011164 primary particle Substances 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- 230000003750 conditioning effect Effects 0.000 claims description 26
- 238000003860 storage Methods 0.000 claims description 26
- 239000002253 acid Substances 0.000 claims description 19
- 239000011521 glass Substances 0.000 claims description 19
- 239000008119 colloidal silica Substances 0.000 claims description 15
- 238000009826 distribution Methods 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- 229910018104 Ni-P Inorganic materials 0.000 claims description 5
- 229910018536 Ni—P Inorganic materials 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims description 5
- 238000007747 plating Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 abstract description 20
- 230000003287 optical effect Effects 0.000 abstract description 16
- 239000012736 aqueous medium Substances 0.000 abstract 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 24
- 239000000126 substance Substances 0.000 description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 18
- -1 phospho Chemical class 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 238000002360 preparation method Methods 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000011156 evaluation Methods 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- 239000002585 base Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000002184 metal Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 230000010354 integration Effects 0.000 description 7
- 150000002500 ions Chemical group 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- JJJOZVFVARQUJV-UHFFFAOYSA-N 2-ethylhexylphosphonic acid Chemical compound CCCCC(CC)CP(O)(O)=O JJJOZVFVARQUJV-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000000280 densification Methods 0.000 description 6
- 239000012467 final product Substances 0.000 description 6
- 238000003801 milling Methods 0.000 description 6
- 102220043159 rs587780996 Human genes 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 230000001186 cumulative effect Effects 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 229910052752 metalloid Inorganic materials 0.000 description 4
- 150000002738 metalloids Chemical class 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 238000001962 electrophoresis Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 238000012797 qualification Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 238000009966 trimming Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 150000001447 alkali salts Chemical class 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000001768 cations Chemical group 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000002296 dynamic light scattering Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 2
- QQVDJLLNRSOCEL-UHFFFAOYSA-N (2-aminoethyl)phosphonic acid Chemical class [NH3+]CCP(O)([O-])=O QQVDJLLNRSOCEL-UHFFFAOYSA-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
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229940123457 Free radical scavenger Drugs 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241001481789 Rupicapra Species 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 125000005263 alkylenediamine group Chemical group 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
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- ZEKANFGSDXODPD-UHFFFAOYSA-N glyphosate-isopropylammonium Chemical compound CC(C)N.OC(=O)CNCP(O)(O)=O ZEKANFGSDXODPD-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 125000003010 ionic group Chemical group 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000011158 quantitative evaluation Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical class Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 229940001516 sodium nitrate Drugs 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- 239000001433 sodium tartrate Substances 0.000 description 1
- 229960002167 sodium tartrate Drugs 0.000 description 1
- 235000011004 sodium tartrates Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 150000003509 tertiary alcohols Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 150000007521 triprotic acids Chemical class 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- ZNRSXPDDVNZGEN-UHFFFAOYSA-K trisodium;chloride;sulfate Chemical compound [Na+].[Na+].[Na+].[Cl-].[O-]S([O-])(=O)=O ZNRSXPDDVNZGEN-UHFFFAOYSA-K 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- 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
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
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- 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
- C09K3/1436—Composite particles, e.g. coated particles
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- 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
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The present invention relates to a polishing composition containing an aqueous medium and silica particles, wherein the silica particles in the polishing composition has a zeta potential of from -15 to 40 mV; a method for manufacturing a substrate including the step of polishing a substrate to be polished with a polishing composition containing an aqueous medium and silica particles, wherein the silica particles in the polishing composition has a zeta potential of from -15 to 40 mV; and a method for reducing scratches on a substrate to be polished with a polishing composition containing an aqueous medium and silica particles, including the step of adjusting a zeta potential of silica particles in the polishing composition to -15 to 40 mV. The polishing composition can be favorably used in polishing the substrate for precision parts, including substrates for magnetic recording media such as magnetic discs, optical discs and opto-magnetic discs; photomask substrates; optical lenses; optical mirrors; optical prisms; semiconductor substrates; and the like.
Description
Technical field
The present invention relates to the Ginding process and the manufacture method of grinding Liquid composition, substrate.
In addition, the invention still further relates to the method (below be also referred to as the method that grinding rate improves) of the grinding rate that improves substrate, the method for using this method to make the method for substrate, grinding Liquid composition and reduce cut.
Background technology
At present, in the manufacturing of various substrates, generally use the operation of various grinding substrates.For example, at semiconductor applications, pair silicon wafer substrate is arranged, the semiconductor wafer substrate of compounds such as gallium arsenide, indium phosphide, gan, the operation that nitrided films such as metallic membrane, silicon nitride, silicon oxide, tantalum nitride, titanium nitride such as the silicon oxide that further forms on wafer (silica), aluminium, copper, tungsten etc. grind; In storage field of hard disks, the operation that has pair aluminium base and glass substrate to grind; In field of display devices such as lens and liquid crystal, the operation that has pair glass to grind.Ground in the grinding step of substrate at these, in order to enhance productivity, grinding rate importantly, for this reason, people have proposed various schemes with regard to the technology that improves mill efficiency.
In storage hard disk drive in recent years, require heavy body and miniaturization, for improving recording density, require to reduce the flying height of magnetic head, reduce the area of unit record.With in the manufacturing process of substrate, desired surface quality is also strict year by year thereupon after grinding at disk, and the countermeasure as reducing the magnetic head floats height must reduce its surfaceness, microcosmic percent ripple, fall (roll-off) and projection; As the countermeasure of the area that reduces unit record, the cut number of each real estate of being allowed will reduce, and the size of cut and the degree of depth become more and more littler.
In addition, at semiconductor applications, to Highgrade integration and the development of high speed aspect, particularly Highgrade integration requires distribution more and more thinner.Consequently, in the manufacturing process of semiconductor substrate, along with the raising to the desired exploring degree of exposure apparatus, the depth of focus during resist exposure shoals, and wishes further to improve the smooth finish and the planeness on surface.
Up to now, in the face of the application of these grindings, the main slip lapping liquid that uses with silicon oxide and cerium oxide particles.Use the slip lapping liquid of silicon oxide particle, its highly versatile uses extensively, but has the low shortcoming of grinding rate.On the other hand, the slip lapping liquid of use cerium oxide particles can be used for the grinding of opticglass, glass storage hard disk, semiconducting insulation film etc., has the fast characteristics of grinding rate, but exists reverse side to be easy to generate the problem of cut.
At these problems, the spy opens the 2002-97459 communique and discloses following abrasive: uses with cerium as the water-dispersion slip of the oxide particle of constituting atom and make the zeta-potential of this particle surface be-10mV or following by giving polished silicon oxide layer, the raising of grinding rate can be sought on the one hand, the generation of cut and dust can be reduced on the other hand.But, surpass with the zeta-potential of this particle surface-situation of 10mV compares, though reduced the generation of cut and dust, grinding rate has also reduced simultaneously, and both can not take into account.
Moreover the spy opens the 2001-329250 communique and discloses following cerium oxide abrasive: by giving SiO
2Insulating films etc. are used by abrasive surface silicon oxide particle are dispersed in slip in the medium, and the zeta-potential of this particle surface is set in-100mV～-10mV, just can carry out the high speed grinding with no damage.But at a high speed the narration of grinding is based on the abrasive that silicon oxide particle constituted by the xenogenesis particle and compares, and the relation between its grinding rate and the zeta-potential is also unclear.
In addition, the spy opens the 2003-193037 communique and discloses the grinding Liquid composition that is intended to improve the surface smoothness of storing hard disk substrate, but the necessary surface smoothness of densification that can not fully obtain storing hard disk substrate.
Summary of the invention
That is, the present invention relates to:
(1) a kind of grinding Liquid composition that comprises water-medium and silicon oxide particle, the zeta-potential of the silicon oxide particle in this grinding Liquid composition is-15～40mV;
(2) Ginding process of the glass substrate of the grinding Liquid composition described in the use above-mentioned (1);
(3) Ginding process of the storage hard disk substrate of the grinding Liquid composition described in the use above-mentioned (1);
(4) a kind of manufacture method of substrate, it comprises the operation of using grinding Liquid composition that quilt grinding substrate is ground, described grinding Liquid composition comprises water-medium and silicon oxide particle, and the zeta-potential of general's silicon oxide particle wherein is adjusted to-15～40mV;
(5) zeta-potential that a kind of method that improves the grinding rate that is ground substrate, its use will comprise the silicon oxide particle in the grinding Liquid composition of water-medium and silicon oxide particle is adjusted to-grinding Liquid composition of 15～40mV;
(6) a kind of manufacture method of substrate, wherein said substrate are that above-mentioned (5) described method is used for being ground substrate;
(7) a kind of minimizing ground substrate and produced the method for cut, and the zeta-potential that its use will comprise the silicon oxide particle in the grinding Liquid composition of water-medium and silicon oxide particle is adjusted to-grinding Liquid composition of 15～40mV.
Embodiment
Densification or the necessary surface smoothness of Highgrade integration that the present inventor just reaches precise part substrates such as storage hard disk substrate and semiconductor substrate require to have carried out research with great concentration, (degree of depth is not less than 10nm but not enough 100nm to " the nanometer cut " that discovery first can not detect so far, width is not less than 5nm but not enough 500nm, length is the trickle scuffing of 100 μ m or above substrate surface) generation hindered densification on the storage hard disk substrate and the Highgrade integration on the semiconductor substrate, thereby finished the present invention.
The abrasive composition that surfaceness is little, the nanometer cut significantly reduces and grinding rate is high of the abrasive material after promptly the present invention relates to grind, and the manufacture method of the substrate that surfaceness is little, the nanometer cut significantly reduces.
In addition, when the present invention relates to improve, improve the method for the grinding rate that is ground substrate, and use this method to make the method for the good and substrate that production efficiency is high of surface smoothness by the surface smoothness of lapped face.
Use grinding Liquid composition of the present invention to produce following effect by for example using in the grinding step of precise part substrate: the surface smoothness height of grinding metacoxa at densification or Highgrade integration, and under higher grinding rate, significantly reduced the trickle nanometer cut that can not detect so far, thereby the present invention can make precise part substrates such as good high-quality storage hard disk substrate of surface texture and semiconductor substrate effectively.
By following explanation, can understand above-mentioned advantage of the present invention and other advantage.
1. abrasive composition
Grinding Liquid composition of the present invention is the grinding Liquid composition that contains water-medium and silicon oxide particle, it is characterized in that: the zeta-potential of the silicon oxide particle in this grinding Liquid composition is-15～40mV, by using this grinding Liquid composition to be ground, can when improving surface smoothness, improve grinding rate to grinding substrate.
The zeta-potential of the present invention by making the silicon oxide particle in the grinding Liquid composition is-15mV～40mV, is preferably-15mV～30mV, can make to be ground substrate and have good surface texture, and can significantly reduce the nanometer cut that causes surface imperfection.Especially, in storage hard disk substrate or semiconductor substrate, this nanometer cut is the rerum natura that densification or Highgrade integration is had vital role.Therefore, the grinding Liquid composition of the application of the invention can be made good high-quality storage hard disk substrate or the semiconductor substrate of surface texture with higher grinding rate.
Although do not plan to stick to theory, but and do not know the minimizing mechanism of this nanometer cut, can know reason by inference is: the zeta-potential of silicon oxide particle is more near iso-electric point, gravitation just becomes big more between the particle between the quartzy particle, thereby causes the oversize particle of cut or the aggregate of fine particle being ground coming off of substrate surface in having suppressed to be considered to grind.
So-called zeta-potential is meant according to principle of electrophoresis among the present invention, when the quartzy particle in grinding Liquid composition applies external electrical field, and the current potential of trying to achieve by the translational speed of this abrasive substance.As the measuring apparatus of zeta-potential, the device of principle of electrophoresis is used in for example preferred " ELS-8000 " (big mound electronics corporation makes), " DELSA 440 SX " (manufacturing of Beckmann Coulter company) and " NICOMP Model1380 " (manufacturing of Particle Sizing Systems company) etc.In addition, also can substitute the device that use " DT 1200 " (Japanese RUFOTO company make) etc. utilizes the ultrasonic wave principle to measure.The mensuration of carrying out according to principle of electrophoresis on the principle of device, concentration that must the dilution silicon oxide particle.The zeta-potential of the silicon oxide particle in this specification sheets in the so-called grinding Liquid composition, be meant by the pH value that is used for will diluting in advance the back grinding Liquid composition be adjusted into dilute before identical zeta-potential adjusting with the aqueous solution (the zeta-potential conditioning agent of grinding Liquid composition and the formed aqueous solution of water.But contain at grinding Liquid composition under the situation of 2 kinds or above zeta-potential conditioning agent, then preparation keeps the aqueous solution of its content ratio), with the zeta-potential of silicon oxide particle concentration adjustment to the grinding Liquid composition of predetermined concentration.In addition, also can use and replace above-mentioned zeta-potential to regulate by the resulting supernatant liquor of the centrifugation of grinding Liquid composition using the aqueous solution.And when stating the zeta-potential measuring apparatus in the use and measuring zeta-potential, be the reliability that improves observed value, same sample is under identical test condition, repeated measurement is 3 times at least, with its mean value as zeta-potential.
The present invention can be adjusted to by the zeta-potential with the silicon oxide particle in the abrasive composition-and 15～40mV improves grinding rate.Consider from the viewpoint that reduces the nanometer cut, wish that this zeta-potential is-15～30mV, be preferably-15～20mV, more preferably-15～10mV, be preferably again-10～10mV, further preferred-5～5mV.
In addition, consider, wish zeta-potential to be adjusted to-15～30mV, be preferably-10～30mV from the viewpoint that reduces cut, more preferably-5～30mV.
In the present invention, the adjusting of the zeta-potential of grinding Liquid composition be there is no special qualification, but preferably before grinding, carry out.In addition, preferably keep the zeta-potential of above-mentioned specified range to finish until grinding.The concrete control method of zeta-potential as described later.
As silicon oxide particle of the present invention, can enumerate colloidal silica particle, pyrolysis method silicon oxide particle etc.Colloidal silica can be by being raw material with silicate base metal-salts such as water glass, carrying out condensation reaction and the soluble glass method of growing silicon oxide particle in the aqueous solution, perhaps by being raw material with tetraethoxysilane etc., carrying out condensation reaction and the organoalkoxysilane method of growing silicon oxide particle obtains in the water that contains water-miscible organic solvents such as alcohol.The pyrolysis method silicon oxide particle can be by being raw material with volatile silicon compound such as silicon tetrachlorides, using oxy-hydrogen burner to carry out vapor phase hydrolysis under 1000 ℃ or above high temperature to obtain.
In addition, as silicon oxide particle of the present invention, also can use the silicon oxide particle of finishing, the silicon oxide particle of composite particlesization etc.The silicon oxide particle of so-called finishing, refer on the silicon oxide particle surface directly or have by coupling agent absorption and/or bonding the silicon oxide particle of metal such as aluminium, titanium, zirconium or their oxide compound, perhaps bonding has silane coupling agent and titanium coupling agent etc. and the silicon oxide particle that forms.The silicon oxide particle of so-called composite particlesization refers to the silicon oxide particle that absorption and/or bonding have nonmetal particle such as polymer particle and silicon oxide particle.These silicon oxide particles can use separately, also can be with its two kinds or above and usefulness.In these silicon oxide particles, consider preferred colloidal silica from the viewpoint that reduces cut.
The median size of the primary particle of silicon oxide particle, irrelevant with the silicon oxide particle that whether mixes one or more, consider its lower limit from the angle that improves grinding rate, and from reducing surfaceness (average surface roughness: Ra, peak-to-valley value: angle Rmax) is considered its upper limit, be preferably and be not less than 1nm but not enough 40nm, more preferably 1～35nm is preferably 3～30nm again, more preferably 5～25nm further is preferably 5～20nm.Moreover, when the primary particle cohesion forms offspring, similarly consider its lower limit from the angle that improves grinding rate, and consider its upper limit from the angle of the surfaceness that reduces substrate, the median size of this offspring is preferably 5～150nm, and more preferably 5～100nm is preferably 5～80nm again, more preferably 5～50nm further is preferably 5～30nm.
In addition, as the size distribution of silicon oxide particle, irrelevant with the silicon oxide particle that whether mixes one or more, from the angle consideration that reduces cut, reduces surfaceness and realize high grinding rate, D90/D50 is preferably 1～5, and more preferably 1～4, more preferably 1～3.
And the median size of the primary particle of silicon oxide particle, begin cumulative size distribution (is benchmark with the number) from small particle size one side of primary particle and reach 50% particle diameter D50 and begin cumulative size distribution (is benchmark with the number) and reach 90% particle diameter D90 from small particle size one side of primary particle, irrelevant with the silicon oxide particle that whether mixes one or more, can obtain by following method.Promptly use the scanner that is connected on the PC to obtain transmission type microscope " the JEM-2000FX " (80kV that makes by JEOL Co., Ltd., 1～50,000 times) view data of photo of observation silicon oxide particle, operational analysis software " WinROOF " (retailer: three paddy business) obtain the diameter of equivalent circle of 1 each and every one silicon oxide particle, with its diameter as silicon oxide particle, after analyzing 1000 or above silicon oxide particle data, use spreadsheet " EXCEL " (Microsoft's manufacturings) to calculate based on this and accumulate size distribution (is benchmark with the number).And the median size of so-called primary particle is represented the identical meaning with D50 here.
The median size of the offspring of silicon oxide particle is irrelevant with the silicon oxide particle that whether mixes one or more, is meant that beginning cumulative size distribution (is benchmark with the volume) from small particle size one side in the measurement of dynamic light scattering method reaches 50% particle diameter.As the measuring apparatus of dynamic light scattering method, suitable use is " ELS-8000 " (big mound electronics corporation makes), " DELSA 440 SX " (manufacturing of Beckmann Coulter company) and " NICOMP Model 1380 " (manufacturing of ParticleSizing Systems company) etc. for example.
Consider from the angle that the improvement of the raising that takes into account grinding rate and surface quality is such, the content of the silicon oxide particle in the above-mentioned grinding Liquid composition is preferably 1～50 weight %, more preferably 2～40 weight % are preferably 3～30 weight % again, more preferably 5～25 weight %.
In addition, so-called water-medium of the present invention is meant water and/or water-miscible organic solvent.Water can be enumerated ion exchanged water, distilled water, ultrapure water etc., as water-miscible organic solvent, can enumerate primary alconol～tertiary alcohol, glycol etc.The content of water-medium be equivalent to deduct silicon oxide particle, zeta-potential conditioning agent the gross weight (100 weight %) from grinding Liquid composition and the content of other composition of adding as required as described later after remaining part.As the content of this medium, be preferably 60～99 weight % of grinding Liquid composition, more preferably 70～98 weight %, further preferred 75～98 weight %.
Can regulate the zeta-potential of the silicon oxide of grinding Liquid composition effectively by in grinding Liquid composition, adding the zeta-potential conditioning agent.So-called zeta-potential conditioning agent is meant the surface that is adsorbed on silicon oxide particle directly or indirectly, and the perhaps character such as acidity or alkalinity of the medium by changing grinding Liquid composition are with the reagent of the surface potential of control particle.For example can enumerate acid, alkali, salt and tensio-active agent.
The zeta-potential conditioning agent for example uses by method as follows.When the zeta-potential on the silicon oxide particle surface of being contained in the grinding Liquid composition surpassed 40mV, as the zeta-potential conditioning agent, preferred acid, acid-salt or the anion surfactant of using made zeta-potential move to negative direction.On the other hand, the zeta-potential when the silicon oxide particle surface of being contained in the grinding Liquid composition is lower than-and during 15mV,, preferably use alkali, basic salt or cats product that zeta-potential is moved to positive dirction as the zeta-potential conditioning agent.In addition, neutral salt, nonionogenic tenside or amphoterics can use under the situation of adjusting zeta-potential in the pH value that does not change grinding Liquid composition.
As acid, can use mineral acid or organic acid.As mineral acid, can enumerate hydrochloric acid, nitric acid, phosphoric acid, Tripyrophosphoric acid, acid amides sulfuric acid (amide sulfuric acid) etc.In addition, as organic acid, can enumerate carboxylic acid, organic phospho acid, amino acid etc.; For example, carboxylic acid can be enumerated monocarboxylic acids such as acetic acid, oxyacetic acid, xitix, di-carboxylic acid such as oxalic acid, tartrate, triprotic acids such as citric acid; Organic phospho acid for example can be enumerated 2-amino-ethyl phosphonic acids, 1-hydroxy ethylene-1,1-di 2 ethylhexyl phosphonic acid (HEDP), amino three (methylene phosphonic acids), ethylene diamine four (methylene phosphonic acid), diethylenetriamine five (methylene phosphonic acid) etc.In addition, as amino acid, can enumerate Padil, L-Ala etc.Wherein, consider preferred mineral acid, carboxylic acid and organic phospho acid from the angle that reduces cut and nanometer cut.For example suitable have hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, Tripyrophosphoric acid, oxyacetic acid, oxalic acid, citric acid, 1-hydroxy ethylene-1,1-di 2 ethylhexyl phosphonic acid, amino three (methylene phosphonic acids), ethylene diamine four (methylene phosphonic acid), a diethylenetriamine five (methylene phosphonic acid).
As alkali, can enumerate ammoniacal liquor, azanol, alkyl azanol, primary～alkyl amine, Alkylenediamine, alkyl ammonium hydroxide etc.Consider from the angle that reduces cut and nanometer cut, preferably ammoniacal liquor, alkanolamine.
In addition,, the salt of above-mentioned acid be can enumerate,, 1A, 2A, the 3B of the long period periodic table of elements, metal and ammonia, azanol or the alkanol ammonium etc. of 8 families preferably belonged to as the positively charged ion that forms its salt as salt.Wherein, as acid-salt, can enumerate ammonium chloride, ammonium nitrate, ammonium sulfate, aluminum nitrate, Tai-Ace S 150, aluminum chloride etc.As basic salt, can enumerate Trisodium Citrate, sodium oxalate, sodium tartrate etc.As neutral salt, can enumerate sodium-chlor, sodium sulfate, SODIUMNITRATE etc.
As tensio-active agent, small molecules type tensio-active agent and high molecular type surfactant are arranged, its absorption or be combined in by chemical bonded refractory on the surface of silicon oxide particle contains same type or 1 dissimilar or above hydrophilic radicals in the molecule.Wherein, can enumerate that to have with ether (oxyethyl group) and hydroxyl be the nonionogenic tenside of the non-ionic group of representative, have with carboxylic acid group, sulfonic group, sulfate group, phosphate-based be the anion surfactant of the anionic group of representative, having with the quaternary ammonium is the cats product of the cation group of representative, has the amphoteric surfactant of anionic group and cation group.
In addition, preferably make up as above-mentioned silicon oxide particle and zeta-potential conditioning agent, as the zeta-potential conditioning agent, preferred hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, Tripyrophosphoric acid, oxyacetic acid, oxalic acid, citric acid, 1-hydroxy ethylene-1,1-di 2 ethylhexyl phosphonic acid, amino three (methylene phosphonic acids), ethylene diamine four (methylene phosphonic acid), diethylenetriamine five (methylene phosphonic acid).More preferably hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, citric acid, 1-hydroxy ethylene-1, the 1-di 2 ethylhexyl phosphonic acid.
In addition, consider, can and use aluminium oxide particles in abrasive composition used in the present invention from the angle that improves grinding rate.Also using under the situation of silicon oxide particle and aluminium oxide particles, as the zeta-potential conditioning agent, preferably sulfuric acid, ammonium sulfate, phosphoric acid, Tripyrophosphoric acid, oxalic acid, citric acid, 1-hydroxy ethylene-1, the 1-di 2 ethylhexyl phosphonic acid, more preferably sulfuric acid, ammonium sulfate, phosphoric acid, Tripyrophosphoric acid, citric acid, 1-hydroxy ethylene-1, the 1-di 2 ethylhexyl phosphonic acid.And the median size of the primary particle of aluminum oxide or offspring preferably with above-mentioned silicon oxide particle in same scope.
In addition, the content of zeta-potential conditioning agent depends on the liquid property of grinding Liquid composition, the character of silicon oxide particle and the zeta-potential of trying to achieve in the grinding Liquid composition, usually can not limit fully, but, for example consider from the angle that reduces cut and nanometer cut, be preferably 0.01～20 weight %, more preferably 0.05～15 weight %.In addition, the zeta-potential conditioning agent can be included in the grinding Liquid composition in advance, also can before being about to grinding it is included in the grinding Liquid composition.
In addition, in the present invention, except silicon oxide particle, can also and with other abrasive substance.As other abrasive substance, can use normally used abrasive substance in the abrasive application, can enumerate metal, metal or metalloid carbide, nitride, oxide compound or boride, diamond etc.Metal or metalloid belong to the element of 2A, 2B, 3A, 3B, 4A, 4B, 5A, 5B, 6A, 7A or the 8th family of the periodic table of elements (long period type).Specific examples as abrasive substance, can enumerate oxide compound (hereinafter referred to as aluminum oxide), silicon carbide, diamond, manganese oxide, magnesium oxide, zinc oxide, titanium oxide, cerium oxide, zirconium white of aluminium etc., in addition, can also enumerate with the surface of these abrasive substances of modified with functional group or to these abrasive substances and carry out surface modification and the material that obtains, make tensio-active agent and abrasive substance become the material etc. of composite particles.From reducing the angle consideration of surfaceness, preferably use in them one or more.
The median size of the primary particle of abrasive substance (except the silicon oxide particle), irrelevant with the abrasive substance that whether mixes one or more, for being not less than 1nm but not enough 40nm, consider from the viewpoint that improves grinding rate, be preferably 3nm or more than, more preferably 5nm or more than, in addition, (average surface roughness: Ra, peak-to-valley value: angle Rmax) is considered from reducing surfaceness, be preferably 35nm or following, more preferably 30nm or following is preferably 25nm or following again, more preferably 20nm or following.Therefore, consider that from the economy angle that reduces surfaceness the particle diameter of this primary particle is preferably 1～35nm, more preferably 3～30nm is preferably 5～25nm, more preferably 5～20nm again.Moreover, form under the situation of offspring through cohesion at primary particle, angle consideration similarly from improving grinding rate and reducing surfaceness, the median size of its offspring is preferably 5～150nm, 5～100nm more preferably, be preferably 5～80nm again, more preferably 5～50nm further is preferably 5～30nm.
The median size of the primary particle of abrasive substance (except the silicon oxide particle), irrelevant with the abrasive substance that whether mixes one or more, use is by the observable image of scanning electron microscope (3000～100000 times is suitable), obtain and begin cumulative size distribution (is benchmark with the number) from small particle size one side of primary particle and reach 50% particle diameter (D50), with its median size as primary particle.Here, the median size of each primary particle adopts 2 average (major diameter and minor axis on average) particle diameters.In addition, the median size of offspring can be measured as volume average particle size by laser diffractometry.
In addition, the size distribution of abrasive substance (except the silicon oxide particle), irrelevant with the abrasive substance that whether mixes one or more, from the angle consideration that reduces the nanometer cut, reduces surfaceness and reach high grinding rate, D90/D50 is preferably 1～5, more preferably 2～5, more preferably 3～5.In addition, so-called D90 is meant and uses by the observable image of scanning electron microscope (3000～100000 times is suitable), begins cumulative size distribution (being benchmark with number) from small particle size one side of primary particle and reach 90% particle diameter.
Consider from the angle that improves grinding rate, the content of the abrasive substance in the grinding Liquid composition (except the silicon oxide particle) be preferably 0.5 weight % or more than, more preferably 1 weight % or more than, be preferably again 3 weight % or more than, more preferably 5 weight % or more than, and from improving the angle consideration of surface quality, this content preferably accounts for 20 weight % or following of grinding Liquid composition, 15 weight % or following more preferably, be preferably 13 weight % or following again, more preferably 10 weight % or following.Promptly consider that from the economy angle that improves surface quality this content is preferably 0.5～20 weight % of grinding Liquid composition, more preferably 1～15 weight % is preferably 3～13 weight % again, more preferably 5～10 weight %.
In addition, in grinding Liquid composition used in the present invention, can mix other composition as required.As this other composition, can enumerate oxygenant, free-radical scavengers, cage compound, rust-preventive agent, defoamer and antiseptic-germicides etc. such as hydrogen peroxide.From the angle of grinding rate,, be preferably 0～10 weight % of grinding Liquid composition, more preferably 0～5 weight % as the content of these other compositions.Above-mentioned grinding Liquid composition can be prepared by said components is suitably mixed.
In addition, the concentration when each component concentrations can be the said composition manufacturing in the above-mentioned grinding Liquid composition, the concentration in the time of also can being to use.In most cases, grinding Liquid composition manufactures the form of concentrated solution usually, in use again with its dilution.
Consider that from the angle of grinding rate, minimizing cut and nanometer cut the pH value of above-mentioned grinding Liquid composition depends on the degree of surface modifications such as employed silicon oxide particle and finishing thereof.Under the situation of colloidal silica, the pH value be preferably 9 or following, more preferably 7 or following, again be preferably 6 or following, more preferably 5 or following, further be preferably 4 or following, more more preferably 3 or following, then be preferably 2.5 or following, then more preferably 2 or below.
Have the grinding Liquid composition of such composition by use, can obtain few cut precise part particularly the nanometer cut, the surface texture excellence very effectively and grind substrate with substrate etc.
So-called nanometer cut is meant that the degree of depth is to be not less than 10nm but not enough 100nm, width are not less than 5nm but not enough 500nm, length are the trickle damage of 100 μ m or above substrate surface among the present invention.Can it be detected by atomic force microscope (AFM), and can carry out quantitative evaluation with the radical of the nanometer cut of being measured by the range estimation proofing unit " MicroMax " described in the embodiment of back.
In addition, so-called cut is meant that the degree of depth is the damage of 10nm or above substrate surface.
In addition, as the surfaceness of surface smoothness yardstick, its evaluation method is also unrestricted, in the present invention, surfaceness is that 10 μ m or the following detectable roughness of shortwave are estimated with the wavelength by AFM (atomic force microscope), and represents with average surface roughness Ra.Specifically, can obtain by the method described in the embodiment of back.
Grinding Liquid composition of the present invention for example can be supplied with to have and keep being ground by the anchor clamps of grinding substrate and the milling apparatus of abrasive cloth, by this method, can when taking into account the surface smoothness of substrate (reducing cut and nanometer cut), improve the grinding rate that is ground substrate.Ground grinding substrate surface by the following method: will keep being ground on the abrasive disk of anchor clamps by the abrasive cloth that is pressed in the foam that posts the organic polymer class, non-foam or non-woven fabrics form of substrate, perhaps will be ground substrate card is posting on the abrasive disk of abrasive cloth, supplied with above-mentioned grinding Liquid composition and apply certain pressure to grinding substrate surface, make abrasive disk or quilt grind substrate simultaneously and move.
From the angle consideration that improves grinding rate and be convenient to control grinding, the grinding load during grinding is preferably 0.5～20kPa, more preferably 1～20kPa, more preferably 3～20kPa.
From the angle consideration that improves grinding rate and reduce the nanometer cut, provided the speed of grinding Liquid composition for every 1cm to grinding substrate
2Substrate is preferably 0.01～3ml/min, more preferably 0.05～2.5ml/min, more preferably 0.1～2ml/min.
The material of the grinding charge that is suitable for using as the present invention, for example can enumerate metal, metalloid or their alloys such as silicon, aluminium, nickel, tungsten, copper, tantalum, titanium, glassy mass such as glass, glassy carbon, decolorizing carbon, stupaliths such as aluminum oxide, silicon-dioxide, silicon nitride, tantalum nitride, titanium carbide, resins such as polyamide resin etc.
Wherein, grinding Liquid composition of the present invention is applicable to that it is the grinding charge of the alloy of principal constituent that metals such as containing aluminium, nickel, tungsten, copper reaches with these metals.For example be applicable to more that plating has in the aluminium alloy base plate of Ni-P and crystallized glass, the hardened glass substrate, is applicable to that further plating has in the aluminium alloy base plate of Ni-P.
In addition, grinding Liquid composition of the present invention just is being applicable at least and is being ground the substrate that contains element silicon in the real estate.For example, be applicable to glass substrates such as crystallized glass, chilled glass, be applicable to that more the surface is formed with the semiconductor substrate of silicon-containing film, be specially adapted to substrates such as crystallized glass, chilled glass.Therefore, the present invention relates to use the Ginding process of the glass substrate of grinding Liquid composition of the present invention.
For the shape of grinding charge and object without particular limitation, that shape that for example have the shape of planar section with discoid, tabular, thick plate-like, prism-shaped etc. and have curvature portions such as lens can become the grinding of using grinding Liquid composition of the present invention.Wherein, especially preferably discoid grinding charge is used for grinding.
Grinding Liquid composition of the present invention is applicable to the grinding of precise part substrate.For example, be applicable in the grinding of precise part substrates such as the substrate that comprises magnetic recording mediums such as the disk of storing hard disk substrate, CD, magneto-optic disk, photomask base plate, optical lens, optical mirror, optical prism, semiconductor substrate.Wherein, because grinding Liquid composition of the present invention can significantly be reduced in densification, the Highgrade integration aspect has the nanometer cut of material impact, so more be applicable in the grinding of disks such as storing hard disk substrate and semiconductor substrate.More be applicable to disk with in the substrate, the grinding of particularly storing hard disk substrate.As the storage hard disk substrate, more preferably glass storage hard disk substrate and plating have the storage hard disk substrate of Ni-P coating.Therefore, the present invention relates to use the Ginding process of the storage hard disk substrate of grinding Liquid composition of the present invention.
The grinding of storage hard disk substrate and semiconductor substrate comprises: for example the planarization operation of the grinding step of silicon wafer (naked wafer), the formation operation that embeds metallic circuit, interlayer dielectric, embed metallic circuit the formation operation, embed the formation operation of electric capacity etc.
In addition, before entering the grinding step that uses grinding Liquid composition of the present invention, the surface texture of substrate is also without particular limitation, and the substrate that for example has Ra and be the surface texture of 1nm is suitable.
Grinding Liquid composition of the present invention has special effect in grinding step, grinding step in addition, and for example polishing (lapping) operation also can be suitable equally.
2. the manufacture method of substrate
The present invention relates to the manufacture method of substrate.
The manufacture method of substrate of the present invention is characterised in that it comprises following operation: use comprise water-medium and silicon oxide particle and the zeta-potential of silicon oxide particle is adjusted to-grinding Liquid composition of 15～40mV, to being ground by the grinding substrate.Owing to have this feature, thereby can obtain following effect, promptly under high grinding rate, the surfaceness of the grinding charge after the grinding is little and obviously reduced the nanometer cut.
In the manufacture method of substrate of the present invention, be fit to use the grinding Liquid composition of the invention described above.
Employed silicon oxide particle in the manufacture method as substrate of the present invention is so long as the material identical with employed silicon oxide particle in the abrasive composition of the invention described above gets final product.
Wherein, consider from the angle that improves grinding rate, the median size of the primary particle of silicon oxide particle be preferably 1nm or more than, more preferably 3nm or more than, more preferably 5nm or more than, and consider from the angle that reduces surfaceness, be preferably not enough 40nm, more preferably 35nm or following is preferably 30nm or following again, more preferably 25nm or following further is preferably 20nm or following.Therefore, consider that from the economy angle that reduces surfaceness the median size of this primary particle is preferably and is not less than 1nm but not enough 40nm, more preferably 1～35nm is preferably 3～30nm again, and more preferably 5～25nm further is preferably 5～20nm.Moreover, form under the situation of offspring through cohesion at primary particle, similarly consider from the angle that improves grinding rate and from the angle of the surfaceness that reduces substrate, the median size of its offspring is preferably 5～150nm, 5～100nm more preferably, be preferably 5～80nm again, more preferably 5～50nm further is preferably 5～30nm.
Employed grinding step in the manufacture method as substrate of the present invention is so long as the operation identical with the grinding step of the grinding Liquid composition that uses the invention described above gets final product.This grinding step is preferably in second operation of a plurality of grinding steps or carry out later on, particularly preferably in carrying out in the last grinding step.At this moment,, also can use other shredder respectively, and when using other shredder respectively for fear of abrasive substance of sneaking into the front operation and grinding Liquid composition, preferably each stage with substrate cleaning.Wherein, there is no special qualification for shredder.
3. improve the method for the grinding rate that is ground substrate
In addition, the present invention relates to improve the method (hereinafter referred to as the method that improves grinding rate) of the grinding rate that is ground substrate.
The method of raising grinding rate of the present invention is characterised in that: the zeta-potential that will comprise the silicon oxide particle in the grinding Liquid composition of water-medium and silicon oxide particle is adjusted to-15～40mV, owing to have this feature, can when taking into account surface smoothness, improve grinding rate.
Employed water-medium, silicon oxide particle in the method as raising grinding rate of the present invention are so long as the material identical with employed material in the grinding Liquid composition of the invention described above gets final product.
Therefore, in the method for raising grinding rate of the present invention, be fit to use grinding Liquid composition of the present invention.
In addition, grinding step so long as the operation identical with the grinding step of aforesaid use grinding Liquid composition of the present invention get final product.
The method of raising grinding rate of the present invention is applicable to the grinding step of precise part substrate.For example be applicable to the substrate that comprises magnetic recording mediums such as the disk of storing hard disk substrate, CD, magneto-optic disk, the grinding of precise part substrates such as photomask base plate, optical lens, optical mirror, optical prism, semiconductor substrate.As the grinding of semiconductor substrate, can enumerate the formation operation of the planarization operation of the grinding step of silicon wafer (naked wafer), the formation operation that embeds metallic circuit, interlayer dielectric, the formation operation that embeds metallic circuit, embedding electric capacity etc.
In addition, as other scheme of the manufacture method of substrate of the present invention, can enumerate the method for the raising grinding rate that uses the invention described above and make the method for substrate.Particularly, the manufacture method of the substrate of this scheme is characterised in that and makes with the following method: promptly use the grinding Liquid composition contain water-medium and silicon oxide particle, the zeta-potential of silicon oxide particle in the said composition is adjusted to-and 15～40mV to be to improve the grinding rate that is ground substrate.Owing to have this feature, can when making full use of the low cut characteristic that silicon oxide has, improve grinding rate, thereby the effect that can obtain to enhance productivity.
By making full use of such feature; manufacturing applicable to recording mediums such as the disk that comprises glass storage hard disk substrate, CD, magneto-optic disks; with the manufacturing of semiconductor substrates such as storage unicircuit, logical integrated circuit or system lsi, perhaps photomask base plate, optical lens, optical mirror, optical prism etc.Wherein, just in time be applicable to the disk that comprises glass storage hard disk substrate and the manufacturing of semiconductor substrate, and be specially adapted to the manufacturing of disks such as glass storage hard disk substrate.
4. reduce the method for the cut that is ground substrate
In addition, the present invention relates to reduce the method (reducing the method for cut) of the cut that is ground substrate that uses grinding Liquid composition.
The method that the present invention reduces cut is characterised in that: the zeta-potential that will comprise the silicon oxide particle in the grinding Liquid composition of water-medium and silicon oxide particle is adjusted to-15～40mV, owing to have this feature, can reduce the cut that is ground substrate.
Employed water-medium, silicon oxide particle in the method as minimizing cut of the present invention are so long as the material identical with employed material in the grinding Liquid composition of the invention described above gets final product.
Therefore, in the method for minimizing cut of the present invention, be fit to use grinding Liquid composition of the present invention.
In addition, grinding step so long as the operation identical with the grinding step that uses grinding Liquid composition of the present invention as mentioned above get final product.
5. the substrate of manufacturing
As mentioned above, use the substrate of the manufacture method manufacturing of grinding Liquid composition of the present invention or substrate of the present invention, can obtain good surface smoothness, for example surfaceness (Ra) is 0.3nm or following, be preferably 0.2nm or following, more preferably 0.15nm or following, more preferably 0.13nm or following.
In addition, the substrate of manufacturing is the few substrate of nanometer cut.Therefore, for example under the situation of storage hard disk substrate, this substrate can reach such requirement, be that recording density is the 120G/ square inch, and then be the storage hard disk substrate of 160G/ square inch, under the situation of semiconductor substrate, this substrate can reach such requirement, be that live width is 65nm, and then be 45nm.
Embodiment
Illustrate further and open the present invention below by embodiment.These embodiment only are illustrations of the present invention, but and do not mean that any qualification of the present invention.
As being ground substrate, use following plating that the aluminium alloy base plate of Ni-P coating is arranged, the lapping liquid of its abrasive substance by containing aluminum oxide has carried out rough grinding in advance, Ra is set at 1nm, thickness is that 1.27mm, periphery are that Ф 95mm and interior week are Ф 25mm, in following examples and comparative example, this grinding substrate is ground evaluation.
Example I-1～I-9 and Comparative Example I-1～I-5
As shown in table 1, (E.I.Du Pont Company makes with colloidal silica I-A, the median size of primary particle is 27nm, D90/D50=3.1), (E.I.Du Pont Company makes I-B, the median size of primary particle is 15nm, D90/D50=2.2), (E.I.Du Pont Company makes I-C, the median size of primary particle is 19nm, D90/D50=1.6) or be equivalent to the I-A of example I-4 and the mixture of I-B (E.I.Du Pont Company makes, the median size of primary particle is 18nm, D90/D50=3.0) as abrasive substance, the HEDP aqueous solution with 60 weight %, the sulfuric acid of 98 weight %, and/or citric acid is as the zeta-potential conditioning agent, and as required with the aqueous hydrogen peroxide solution of 35 weight % as other component, preparation has composition as shown in table 1, the pH value, and the grinding Liquid composition of abrasive substance zeta-potential.In addition, surplus is an ion exchanged water.
Each component blended is in proper order: will be as HEDP and the sulfuric acid or the citric acid dilute with water of zeta-potential conditioning agent, in this aqueous solution, add aqueous hydrogen peroxide solution, then add remaining composition, after mixing and the adjusting, under agitation it is little by little joined in the colloidal silica slip, the preparation of grinding Liquid composition is promptly accused and is finished like this.
For resulting grinding Liquid composition among example I-1～I-9 and the Comparative Example I-1～I-5,, measure its zeta-potential, nanometer cut and surfaceness (Ra) and estimate based on method as described below.The result of gained is as shown in table 1.
I-1. grinding condition
Rub tester: the 9B type twin grinder that SPEEDFAM company makes
Abrasive cloth: the smooth grinding that FUJIBO company makes is with filling up (thickness 0.9mm, opening diameter: 30 μ m, 60 ° of Xiao A hardness)
Platen (platen) speed of rotation: 32.5r/min
The feed speed of grinding Liquid composition: 100ml/min
Milling time: 4min
Grind load: 7.8kPa
The number of the substrate that drops into: 10.
I-2. the test condition of zeta-potential
" ELS-8000 " (dull and stereotyped program control type) that testing tool: Da mound electronics corporation makes
Impressed voltage: 80V
Probe temperature: 25 ℃
Specimen: preparation as follows the grinding Liquid composition of dilution as specimen: use can be adjusted into the pH value of dilution back grinding Liquid composition and dilute the preceding identical zeta-potential conditioning agent aqueous solution (zeta-potential conditioning agent in the grinding Liquid composition and water form the aqueous solution) accordingly, makes that the concentration of abrasive substance is 0.05 weight %
Testing time: same sample is tested 3 times under the same conditions repeatedly, with its mean value of 3 times as zeta-potential.
I-3. the test condition of nanometer cut
" the MicroMax VMX-2100CSP " that testing tool VISION PSYTEC company makes
Light source: 2S λ (250W) and 3P λ (250W) are 100%
Inclination angle :-6 °
Multiplying power: maximum (angular field of view: the total area is 1/120)
Angular field of view: whole area (substrate of periphery φ 95mm and interior all φ 25mm)
Aperture (iris): notch
Estimate: 4 substrates that grind through rub tester of picked at random divided by 8, just calculate the nanometer cut number of each real estate with the existing total nanometer cut number (root) of the pros and cons separately of these 4 substrates.The evaluation of the nanometer cut of putting down in writing in the table in addition, is promptly to carry out with respect to the nanometer cut number (root/face) of comparative example 1 with the relative evaluation method.
I-4. the test condition of surfaceness (Ra)
Testing tool: " NanoscopeIII, the Dimension 3000 " that Digital Equipment Corporation (Digital Instrument) makes
Sweep velocity: 1.0Hz
Scanning area: 2 * 2 μ m
Estimate: every 120 ° of 3 points equally spaced measuring on the inner periphery and the outer periphery, test simultaneously on the two sides of this substrate and carry out, obtain the mean value that amounts to 6 points.
By the result shown in the table 1 as can be known: use the resulting substrate of grinding Liquid composition of example I-1～I-9, compare with the substrate of Comparative Example I-1～I-5, the generation of nanometer cut is suppressed, and has reduced surfaceness.
(test condition of zeta-potential)
The test condition of the described zeta-potential in back is as follows:
Testing tool: NICOMP Model 1380 ZLS (manufacturing of Particle Sizing Systems company)
Impressed voltage: 1.0～5.0V
Specimen: (centrifugal force 35000g 30min), takes out supernatant liquor to use separating centrifuge that the grinding Liquid composition of each embodiment/comparative example is carried out centrifugation.This grinding Liquid composition that in this supernatant liquor, add to mix 0.2 weight %, with it as specimen.
Testing time: same sample is tested 3 times under identical condition determination repeatedly, with its mean value of 3 times as zeta-potential.
Example II-1
The grinding Liquid composition that preparation is made up of following compositions (zeta-potential: 26.5mV, pH value: 1.5): the colloidal silica slip II-A of 20 weight % (median size of E.I.Du Pont Company's manufacturing, primary particle is 37nm, D90/D50=2.2) as silicon oxide particle, 0.25 the hydrochloric acid as 36 weight % of zeta-potential conditioning agent of weight %, surplus is an ion exchanged water.
The order by merging of each component is: will little by little join under agitation condition among the colloidal silica slip II-A and prepare as the aqueous hydrochloric acid through water-reducible 36 weight % of zeta-potential conditioning agent.Use the grinding Liquid composition of these preparations, grind evaluation according to following condition, grinding rate is that 0.197 μ m/min, surface smoothness (Ra) are 0.23nm as a result.
II-1, quilt are ground substrate
The storage hard disk substrate that crystallized glass is made, periphery 65mm, interior all 20mm, thickness 0.65mm, surfaceness (Ra) 0.2～0.3nm.
II-2, grinding condition
Milling apparatus: " Musasino Denshi MA-300 " (carrier (carrier) is forced driving for single face shredder, platen diameter 300mm)
Platen speed of rotation: 90r/min
Carrier speed of rotation: 90r/min
The feed speed of grinding Liquid composition: 50ml/min (every 1cm
2Ground substrate 1.7ml/min)
Milling time: 10min
Grind load: 14.7kPa
Grinding pad: " chamois leather type, Bellatrix N0012 " (manufacturing of Kanebo company)
Method for trimming: every grinding once repaired for 30 seconds with brush.
The method of calculation of II-3, grinding rate
Suppose that the proportion that is ground substrate is 2.41, calculate grinding rate (μ m/min) by the weight reduction before and after grinding.
[evaluation method of the smooth finish of substrate]
The surface smoothness of substrate is estimated by the average surface roughness (Ra) of measuring substrate.Condition determination is as follows:
Instrument: Zygo New View5032
Lens: 10 times
Zoom ratio: 1
Camera: 320 * 240 is common
Move (remove): right cylinder
Filter: FFT Fixed Band Pass0.005～0.1mm
Area: 0.85mm * 0.64mm
Example II-2～II-4, Comparative Example I I-1
The grinding Liquid composition the same with example II-1, that preparation has the zeta-potential of composition as shown in table 2, pH value and silicon oxide particle grinds evaluation to it.Its result (grinding rate, zeta-potential) is as shown in table 2.
Table 2
As shown in Table 2: the zeta-potential of silicon oxide particle is adjusted to-example II-2～II-4 in the scope of 15～40mV in the grinding Liquid composition, and I-1 compares with Comparative Example I, and grinding rate is significantly improved.
Example II-5～II-6, Comparative Example I I-2
As shown in table 3, (E.I.Du Pont Company makes with colloidal silica slip II-B, the median size of primary particle is 17nm, D90/D50=1.6) as silicon oxide particle, the hydrochloric acid of 36 weight % is used as the zeta-potential conditioning agent, preparation has the grinding Liquid composition of the zeta-potential of composition as shown in table 3, pH value and silicon oxide particle, and surplus is an ion exchanged water.
The order by merging of each component is: will as the zeta-potential conditioning agent through water-reducible aqueous hydrochloric acid, under agitation condition, little by little join in the colloidal silica slip and prepare.Use these grinding Liquid compositions of preparation, grind evaluation under the following conditions.Resulting result (grinding rate, zeta-potential) is as shown in table 3.Ground the method for calculation of substrate, grinding condition, grinding rate, identical with example I-1～II～4.
Table 3
As shown in Table 3: the zeta-potential of silicon oxide particle is adjusted to-example II-5, II-6 in the scope of 15～40mV in the grinding Liquid composition, and I-2 compares with Comparative Example I, and grinding rate is significantly improved.
Example II-7～II-8, Comparative Example I I-3
As shown in table 4, colloidal silica slip II-A is used as silicon oxide particle, the hydrochloric acid of 36 weight % is used as the zeta-potential conditioning agent, and preparation has the grinding Liquid composition of the zeta-potential of composition as shown in table 4, pH value and silicon oxide particle, and surplus is an ion exchanged water.The order by merging of each component is: will as the zeta-potential conditioning agent through water-reducible aqueous hydrochloric acid, under agitation condition, little by little join in the colloidal silica slip and prepare.Use the grinding Liquid composition of these preparations, grind evaluation under the following conditions.Resulting result (grinding rate, zeta-potential) is as shown in table 4.Ground the method for calculation of substrate, grinding condition, grinding rate, identical with example I-1～II～4.
Table 4
As shown in Table 4: the zeta-potential of silicon oxide particle is adjusted to-example II-7, II-8 in the scope of 15～40mV in the grinding Liquid composition, and I-3 compares with Comparative Example I, and grinding rate is significantly improved.
Example II-9～II-10, Comparative Example I I-4
As shown in table 5, colloidal silica slip II-A is used as silicon oxide particle, the hydrochloric acid of 36 weight % is used as the zeta-potential conditioning agent, and preparation has the grinding Liquid composition of the zeta-potential of composition as shown in table 5, pH value and silicon oxide particle, and surplus is an ion exchanged water.The order by merging of each component is: will as the zeta-potential conditioning agent through water-reducible aqueous hydrochloric acid, under agitation condition, little by little join in the colloidal silica slip and prepare.Use the grinding Liquid composition of these preparations, grind evaluation under the following conditions.Resulting result (grinding rate, zeta-potential) is as shown in table 5.
II-4, quilt are ground substrate
Be formed with the PE-TEOS film of 2000nm on 8 inches (200mm) silicon substrates, and then be cut to the square of 40mm * 40mm.
II-5, grinding condition
The feed speed of grinding Liquid composition, milling time, grinding pad and method for trimming are as follows, and remaining condition is identical with example II-1～II-4.
The feed speed of grinding Liquid composition: 200ml/min (every 1cm
2Ground substrate 0.6ml/min)
Milling time: 5min
Grinding pad: " IC1000 050 (P)/Suba 400 " (manufacturing of RODEL NITTA company)
Method for trimming: " Diamond Dresser#100 " finishing 30 seconds is once used in every grinding.
The method of calculation of II-6, grinding rate
Difference by the remaining film thickness of PE-TEOS before and after grinding is calculated grinding rate (nm/min).Wherein, use light interference type film thickness gauge (" LAMBDA ACE VM-1000 " that DAINIPPON SCREEN MFG. company makes) to measure remaining film thickness.
Table 5
As shown in Table 5: the zeta-potential of silicon oxide particle is adjusted to-example II-9, II-10 in the scope of 15～40mV in the grinding Liquid composition, and I-4 compares with Comparative Example I, and grinding rate has improved.
Grinding Liquid composition of the present invention is applicable in the grinding of precise part substrates such as the substrate, photomask base plate, optical lens, optical mirror, optical prism, semiconductor substrate of magnetic recording mediums such as disk, CD, magneto-optic disk for example.
Therefore, for the present invention discussed above, it is conspicuous obtaining identical content by multiple transformable method.This variation is not thought to have broken away from purpose of the present invention and scope, and those skilled in the art know that this class of understanding changes and will all comprise within the scope of the claims.
Claims (12)
1. storage polishing composition for hard disk substrate that comprises water-medium and silicon oxide particle, the zeta-potential of the silicon oxide particle in the wherein said grinding Liquid composition is-10～10mV, and the median size of the primary particle of silicon oxide particle is for being not less than 1nm but not enough 40nm, is 1～5 as the D90/D50 of the size distribution of silicon oxide particle.
2. grinding Liquid composition as claimed in claim 1, wherein silicon oxide is a colloidal silica.
3. grinding Liquid composition as claimed in claim 1, it comprises more than one the zeta-potential conditioning agent that is selected among acid, alkali, salt and the tensio-active agent.
4. Ginding process of storing hard disk substrate, it uses the described grinding Liquid composition of claim 1.
5. Ginding process as claimed in claim 4, wherein said storage hard disk substrate are substrate or the glass storage hard disk substrate that plating has Ni-P coating.
6. manufacture method of storing hard disk substrate, it comprises the operation of using grinding Liquid composition that quilt grinding substrate is ground, described grinding Liquid composition comprises water-medium and silicon oxide particle, wherein, the zeta-potential of silicon oxide particle is adjusted to-10～10mV, and the median size of the primary particle of silicon oxide particle is set to and is not less than 1nm but not enough 40nm, is set to 1～5 as the D90/D50 of the size distribution of silicon oxide particle.
7. one kind is improved conduct by the method for the grinding rate of the storage hard disk substrate of grinding substrate, the zeta-potential that wherein will comprise the silicon oxide particle in the grinding Liquid composition of water-medium and silicon oxide particle is adjusted to-10～10mV, and the median size of the primary particle of silicon oxide particle is set at is not less than 1nm but not enough 40nm, will be set at 1～5 as the D90/D50 of the size distribution of silicon oxide particle.
8. method as claimed in claim 7 is wherein ground substrate and is contained silicon at it at least by lapped face.
9. method as claimed in claim 7, it further comprises with the grinding load of 0.5～20kPa grinding pad by being pressed in the operation of being ground on the substrate.
10. the manufacture method of a substrate, it comprises the operation that the described method of claim 7 is used for being ground substrate.
11. method that reduces as the cut of the storage hard disk substrate that is ground substrate, the zeta-potential that wherein will comprise the silicon oxide particle in the grinding Liquid composition of water-medium and silicon oxide particle is adjusted to-10～10mV, and the median size of the primary particle of silicon oxide particle is set at is not less than 1nm but not enough 40nm, will be set at 1～5 as the D90/D50 of the size distribution of silicon oxide particle.
12. method as claimed in claim 11, it is to every 1cm
2Ground substrate and supplied with grinding Liquid composition, simultaneously grinding pad is pressed into this and is ground on the substrate with the speed of 0.01～3ml/min.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP081768/2004 | 2004-03-22 | ||
| JP2004081768A JP4286168B2 (en) | 2004-03-22 | 2004-03-22 | How to reduce nanoscratches |
| JP191782/2004 | 2004-06-29 | ||
| JP2004191782A JP4414292B2 (en) | 2004-06-29 | 2004-06-29 | Polishing speed improvement method |
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| CN1673306A CN1673306A (en) | 2005-09-28 |
| CN1673306B true CN1673306B (en) | 2011-08-10 |
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| CN2005100590654A Expired - Fee Related CN1673306B (en) | 2004-03-22 | 2005-03-22 | Polishing composition |
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| US (2) | US20050208883A1 (en) |
| CN (1) | CN1673306B (en) |
| GB (1) | GB2412917B (en) |
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- 2005-03-08 TW TW094106992A patent/TW200613485A/en unknown
- 2005-03-11 GB GB0505057A patent/GB2412917B/en not_active Expired - Fee Related
- 2005-03-17 US US11/081,560 patent/US20050208883A1/en not_active Abandoned
- 2005-03-18 MY MYPI20051185A patent/MY141876A/en unknown
- 2005-03-22 CN CN2005100590654A patent/CN1673306B/en not_active Expired - Fee Related
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2007
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| CN1307079C (en) * | 2003-09-30 | 2007-03-28 | 明基电通股份有限公司 | Panel display |
Also Published As
| Publication number | Publication date |
|---|---|
| US20050208883A1 (en) | 2005-09-22 |
| CN1673306A (en) | 2005-09-28 |
| GB2412917B (en) | 2009-06-10 |
| GB0505057D0 (en) | 2005-04-20 |
| GB2412917A (en) | 2005-10-12 |
| US20070167116A1 (en) | 2007-07-19 |
| MY141876A (en) | 2010-07-16 |
| TW200613485A (en) | 2006-05-01 |
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