TWI623612B - Sapphire plate slurry composition - Google Patents
Sapphire plate slurry composition Download PDFInfo
- Publication number
- TWI623612B TWI623612B TW104133754A TW104133754A TWI623612B TW I623612 B TWI623612 B TW I623612B TW 104133754 A TW104133754 A TW 104133754A TW 104133754 A TW104133754 A TW 104133754A TW I623612 B TWI623612 B TW I623612B
- Authority
- TW
- Taiwan
- Prior art keywords
- polishing
- sapphire
- sapphire plate
- cerium oxide
- oxide particles
- Prior art date
Links
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 185
- 239000010980 sapphire Substances 0.000 title claims abstract description 185
- 239000000203 mixture Substances 0.000 title claims abstract description 153
- 239000002002 slurry Substances 0.000 title claims description 11
- 238000005498 polishing Methods 0.000 claims abstract description 256
- 239000002245 particle Substances 0.000 claims abstract description 196
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 137
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 135
- 239000007788 liquid Substances 0.000 claims abstract description 74
- 229910052816 inorganic phosphate Inorganic materials 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 40
- 150000001875 compounds Chemical class 0.000 claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 claims abstract description 23
- 239000012736 aqueous medium Substances 0.000 claims abstract description 13
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims abstract description 12
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 claims abstract description 10
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical class O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000007494 plate polishing Methods 0.000 claims abstract description 3
- 239000004615 ingredient Substances 0.000 claims description 33
- 238000000227 grinding Methods 0.000 claims description 32
- -1 alkali metal salt Chemical class 0.000 claims description 17
- 150000003863 ammonium salts Chemical class 0.000 claims description 6
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 4
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 20
- 230000003746 surface roughness Effects 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- 239000003002 pH adjusting agent Substances 0.000 description 12
- 239000000758 substrate Substances 0.000 description 12
- 239000006185 dispersion Substances 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 239000006061 abrasive grain Substances 0.000 description 7
- 239000011164 primary particle Substances 0.000 description 7
- 239000011163 secondary particle Substances 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 6
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 6
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000000634 powder X-ray diffraction Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 5
- 235000019838 diammonium phosphate Nutrition 0.000 description 5
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000007800 oxidant agent Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 229910052684 Cerium Inorganic materials 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- GJYJYFHBOBUTBY-UHFFFAOYSA-N alpha-camphorene Chemical compound CC(C)=CCCC(=C)C1CCC(CCC=C(C)C)=CC1 GJYJYFHBOBUTBY-UHFFFAOYSA-N 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 238000004630 atomic force microscopy Methods 0.000 description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 4
- 238000007865 diluting Methods 0.000 description 4
- 238000002296 dynamic light scattering Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 125000004383 glucosinolate group Chemical group 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000005696 Diammonium phosphate Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000005819 Potassium phosphonate Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000006059 cover glass Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- YXXXKCDYKKSZHL-UHFFFAOYSA-M dipotassium;dioxido(oxo)phosphanium Chemical compound [K+].[K+].[O-][P+]([O-])=O YXXXKCDYKKSZHL-UHFFFAOYSA-M 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 238000010979 pH adjustment Methods 0.000 description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 2
- 229910001380 potassium hypophosphite Inorganic materials 0.000 description 2
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 241000218628 Ginkgo Species 0.000 description 1
- 235000011201 Ginkgo Nutrition 0.000 description 1
- 235000008100 Ginkgo biloba Nutrition 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- AXTYOFUMVKNMLR-UHFFFAOYSA-N dioxobismuth Chemical compound O=[Bi]=O AXTYOFUMVKNMLR-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001139 pH measurement Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- KOUDKOMXLMXFKX-UHFFFAOYSA-N sodium oxido(oxo)phosphanium hydrate Chemical compound O.[Na+].[O-][PH+]=O KOUDKOMXLMXFKX-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- DWZJIMWMBCWAPW-UHFFFAOYSA-N trisodium;phosphite;pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].[Na+].[O-]P([O-])[O-] DWZJIMWMBCWAPW-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
本發明之藍寶石板用研磨液組合物含有二氧化矽粒子、選自由正磷酸鹽、亞磷酸鹽、及次磷酸鹽所組成之群中之1種以上之無機磷酸鹽化合物及水系介質，且25℃下之pH為8以上。上述無機磷酸鹽化合物較佳為選自由正磷酸鹽、亞磷酸鹽、及次磷酸鹽所組成之群中之1種以上之無機磷酸鹽化合物。本發明之藍寶石板之製造方法之一例包括如下步驟：對被研磨藍寶石板供給上述藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨。本發明之被研磨藍寶石板之研磨方法之一例包括如下步驟：對被研磨藍寶石板供給上述藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨。 The polishing liquid composition for sapphire sheets according to the present invention contains cerium oxide particles, one or more inorganic phosphate compounds selected from the group consisting of orthophosphates, phosphites, and hypophosphites, and an aqueous medium, and The pH at ° C is 8 or more. The inorganic phosphate compound is preferably one or more inorganic phosphate compounds selected from the group consisting of orthophosphates, phosphites, and hypophosphites. An example of the method for producing a sapphire plate according to the present invention includes the step of supplying the polishing liquid composition for a sapphire plate to a ground sapphire plate, and polishing the ground sapphire plate. An example of the method for polishing a sapphire plate to be polished according to the present invention includes the step of supplying the sapphire plate polishing composition to the ground sapphire plate, and polishing the sapphire plate to be polished.
Description
本發明係關於一種藍寶石板用研磨液組合物、及使用其之藍寶石板之製造方法以及被研磨藍寶石板之研磨方法。 The present invention relates to a polishing composition for a sapphire plate, a method for producing a sapphire plate using the same, and a method for polishing a sapphire plate to be polished.
藍寶石等硬脆材料作為光學材料、電子材料或機械材料不可或缺。 Hard and brittle materials such as sapphire are indispensable as optical materials, electronic materials or mechanical materials.
例如，人工藍寶石板被用作積體電路基盤、紅外線探測用透鏡、時鐘、智慧型手機等移動終端裝置等各種用途之材料。尤其隨著LED(Light Emitting Diode，發光二極體)之急速普及，用作其基板之藍寶石板之需求急速增加。關於LED用藍寶石板，為了提高LED元件之發光效率而期待其表面平滑性較高。 For example, an artificial sapphire board is used as a material for various uses such as an integrated circuit base, an infrared detecting lens, a clock, and a mobile terminal device such as a smart phone. In particular, with the rapid spread of LEDs (Light Emitting Diodes), the demand for sapphire panels used as substrates thereof has rapidly increased. The sapphire panel for LED is expected to have high surface smoothness in order to improve the luminous efficiency of the LED element.
為了滿足藍寶石板之表面平滑性，進行使用包含二氧化矽粒子之研磨液組合物之精研磨。藉由使用硬度低於藍寶石(α-氧化鋁、莫氏硬度9)板之二氧化矽(莫氏硬度7)粒子作為研磨粒，不會於藍寶石板表面上產生凹坑或刮痕。然而，藍寶石雖然機械、化學、熱穩定性優異，但存在於使用二氧化矽粒子之精研磨中研磨速度較低之問題。 In order to satisfy the surface smoothness of the sapphire plate, fine polishing using a polishing liquid composition containing cerium oxide particles is performed. By using particles of cerium oxide (Mohs hardness 7) having a hardness lower than that of sapphire (α-alumina, Mohs hardness 9) as the abrasive grains, pits or scratches are not generated on the surface of the sapphire plate. However, although sapphire is excellent in mechanical, chemical, and thermal stability, it has a problem that the polishing speed is low in the fine polishing using the cerium oxide particles.
針對研磨速度之問題，例如於專利文獻1中揭示有包含氯化鈉或氯化鉀等具有鹼性pH且經溶解之氯化物的藍寶石板用之研磨液組合物。於專利文獻6中揭示有以同時實現高速研磨與表面粗糙度降低為目的、包含特定之無機硼化合物的藍寶石板用之研磨液組合物。於專利文獻2、3中揭示有以提高研磨速度為目的、使用氧化鋁粒子作為研磨粒且包含磷化合物等添加劑之研磨液組合物。於專利文獻4中揭示 有pH為酸性區域且可藉由包含磷酸或膦酸系之化合物而提高研磨速度之研磨液組合物。於專利文獻5中揭示有研磨對象為SiC基板、pH為8.5-12、包含氧化劑作為必需成分且包含無機鹽作為任意成分之研磨液組合物，但並未記載SiC基板以外之研磨對象。 For the problem of the polishing rate, for example, Patent Document 1 discloses a polishing liquid composition for a sapphire plate having a basic pH and dissolved chloride such as sodium chloride or potassium chloride. Patent Document 6 discloses a polishing liquid composition for a sapphire plate containing a specific inorganic boron compound for the purpose of simultaneously achieving high-speed polishing and surface roughness reduction. Patent Literatures 2 and 3 disclose a polishing liquid composition containing an alumina particle as an abrasive particle and an additive such as a phosphorus compound for the purpose of increasing the polishing rate. Revised in Patent Document 4 A polishing liquid composition having a pH in an acidic region and capable of increasing the polishing rate by a compound containing a phosphoric acid or a phosphonic acid system. Patent Document 5 discloses a polishing liquid composition in which a polishing target is a SiC substrate, a pH of 8.5-12, an oxidizing agent as an essential component, and an inorganic salt as an optional component. However, the polishing target other than the SiC substrate is not described.
專利文獻1：日本專利特表2008-531319號公報 Patent Document 1: Japanese Patent Laid-Open Publication No. 2008-531319
專利文獻2：日本專利特表2006-524583號公報 Patent Document 2: Japanese Patent Laid-Open Publication No. 2006-524583
專利文獻3：日本專利特開2011-62815號公報 Patent Document 3: Japanese Patent Laid-Open No. 2011-62815
專利文獻4：日本專利特表2009-538236號公報 Patent Document 4: Japanese Patent Laid-Open Publication No. 2009-538236
專利文獻5：WO2012/036087號公報 Patent Document 5: WO2012/036087
專利文獻6：日本專利特開2012-206183號公報 Patent Document 6: Japanese Patent Laid-Open Publication No. 2012-206183
另一方面，期待以提高生產性為目的而進一步提高藍寶石板之研磨速度，同時確保良好之表面平滑性。 On the other hand, it is expected to further improve the polishing speed of the sapphire sheet for the purpose of improving productivity while ensuring good surface smoothness.
本發明提供一種可同時實現高速研磨與低表面粗糙度之藍寶石板用研磨液組合物、及使用其之藍寶石板之製造方法以及被研磨藍寶石板之研磨方法。 The present invention provides a polishing liquid composition for sapphire sheets capable of simultaneously achieving high-speed polishing and low surface roughness, a method for producing a sapphire sheet using the same, and a method for polishing a sapphire plate to be polished.
本發明之藍寶石板用研磨液組合物含有二氧化矽粒子、選自由正磷酸鹽、亞磷酸鹽、及次磷酸鹽所組成之群中之1種以上之無機磷酸鹽化合物以及水系介質，且25℃下之pH為8以上。 The polishing liquid composition for sapphire sheets according to the present invention contains cerium oxide particles, one or more inorganic phosphate compounds selected from the group consisting of orthophosphates, phosphites, and hypophosphites, and an aqueous medium, and The pH at ° C is 8 or more.
本發明之藍寶石板之製造方法之一例包括如下步驟：對被研磨藍寶石板供給本發明之藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨。 An example of the method for producing a sapphire plate according to the present invention includes the step of supplying the polishing sapphire plate composition of the present invention to the ground sapphire plate, and polishing the ground sapphire plate.
本發明之藍寶石板之製造方法之另一例包括如下步驟：供給本發明之藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨；及使用上述步驟中使用之上述藍寶石板用研磨液組合物，對上述被研磨藍寶石板以外之被研磨藍寶石板進行研磨。 Another example of the method for producing a sapphire plate according to the present invention includes the steps of: supplying the polishing composition for sapphire plate of the present invention, grinding the sapphire plate to be polished; and using the above-described sapphire plate polishing liquid used in the above step The ground sapphire plate other than the ground sapphire plate is ground.
本發明之被研磨藍寶石板之研磨方法之一例包括如下步驟：對被研磨藍寶石板供給本發明之藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨。 An example of the method for polishing a sapphire plate to be polished according to the present invention includes the step of supplying the sapphire plate for polishing the sapphire plate of the present invention to the sapphire plate to be ground.
本發明之被研磨藍寶石板之研磨方法之另一例包括如下步驟：供給本發明之藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨；及使用上述步驟中使用之上述藍寶石板用研磨液組合物，對上述被研磨藍寶石板以外之被研磨藍寶石板進行研磨。 Another example of the method for polishing a ground sapphire plate according to the present invention comprises the steps of: supplying the polishing composition for sapphire plate of the present invention, grinding the sapphire plate to be polished; and using the sapphire plate for polishing used in the above step The liquid composition is ground on the ground sapphire plate other than the ground sapphire plate.
本發明之藍寶石板用研磨液組合物之用途係將本發明之藍寶石板用研磨液組合物用於被研磨藍寶石板之研磨。 The use of the polishing liquid composition for sapphire sheets of the present invention is to use the polishing composition for sapphire sheets of the present invention for polishing a ground sapphire sheet.
根據本發明，可提供一種可同時實現高速研磨與低表面粗糙度之藍寶石板用研磨液組合物、及使用其之藍寶石板之製造方法以及被研磨藍寶石板之研磨方法。 According to the present invention, it is possible to provide a polishing liquid composition for a sapphire plate which can simultaneously realize high-speed polishing and low surface roughness, a method for producing a sapphire plate using the same, and a polishing method for a sapphire plate to be polished.
本發明係基於如下見解：包含二氧化矽粒子與水系介質之研磨液組合物於其pH為8以上之情形時，藉由包含特定之無機磷酸鹽化合物，可同時實現高速研磨與低表面粗糙度。 The present invention is based on the insight that when a slurry composition comprising cerium oxide particles and an aqueous medium has a pH of 8 or more, high-speed grinding and low surface roughness can be simultaneously achieved by including a specific inorganic phosphate compound. .
本發明之藍寶石板用研磨液組合物(以下亦存在簡稱為「研磨液組合物」之情形)包含二氧化矽粒子(成分A)、選自由正磷酸鹽、亞磷酸鹽、及次磷酸鹽所組成之群中之1種以上之無機磷酸鹽化合物(成分 B)、以及水系介質(成分C)。藉由本發明之研磨液組合物包含特定之無機磷酸鹽化合物(成分B)而可同時實現高速研磨與低表面粗糙度之理由雖不確定，但推測如下。 The polishing liquid composition for sapphire sheets of the present invention (hereinafter also referred to simply as "the polishing liquid composition") contains cerium oxide particles (ingredient A) selected from the group consisting of orthophosphates, phosphites, and hypophosphites. One or more inorganic phosphate compounds (components) B), and the aqueous medium (ingredient C). Although the reason why the high-speed polishing and the low surface roughness can be simultaneously achieved by the polishing liquid composition of the present invention containing a specific inorganic phosphate compound (component B) is uncertain, it is presumed as follows.
若對被研磨藍寶石板表面供給鹼性之研磨液組合物，則藉由藍寶石之鹼性水解，被研磨藍寶石板表面之結晶結構軟質化。於對經軟質化之被研磨藍寶石板表面進行研磨之情形時，與對未經軟質化之被研磨藍寶石板表面進行研磨之情形相比，更可實現高速研磨及表面粗糙度之降低。若於包含二氧化矽粒子與水系介質且25℃下之pH為8以上之研磨液組合物中包含無機磷酸鹽化合物(成分B)，則藍寶石與無機磷酸鹽化合物(成分B)反應而生成磷酸鋁。推測隨著磷酸鋁之生成而產生鹼作為副產物，至被研磨藍寶石板之更深部為止其結晶結構因該鹼而軟質化，其結果，可同時實現高速研磨與低表面粗糙度。但是，本發明並不限定於該等推定。 When the alkaline polishing composition is supplied to the surface of the ground sapphire plate, the crystal structure of the surface of the polished sapphire plate is softened by alkaline hydrolysis of sapphire. In the case of polishing the surface of the softened sapphire plate, the high-speed grinding and the reduction of the surface roughness can be achieved compared with the case where the surface of the sapphire plate which has not been softened is ground. When an inorganic phosphate compound (ingredient B) is contained in a polishing liquid composition containing cerium oxide particles and an aqueous medium and having a pH of 8 or more at 25 ° C, sapphire reacts with an inorganic phosphate compound (ingredient B) to form phosphoric acid. aluminum. It is presumed that a base is produced as a by-product by the formation of aluminum phosphate, and the crystal structure is softened by the alkali until the deeper portion of the sapphire plate is polished. As a result, high-speed polishing and low surface roughness can be simultaneously achieved. However, the present invention is not limited to the above assumptions.
<二氧化矽粒子> <cerium oxide particles>
本發明之研磨液組合物所包含之二氧化矽粒子(成分A)係作為研磨粒而發揮作用。作為該等二氧化矽粒子，可列舉膠體二氧化矽、薰製二氧化矽等，就提高經研磨之被研磨對象物之平滑性之觀點而言，更佳為膠體二氧化矽。 The cerium oxide particles (component A) contained in the polishing liquid composition of the present invention function as abrasive grains. Examples of the cerium oxide particles include colloidal cerium oxide, cerium oxide, and the like, and colloidal cerium oxide is more preferable from the viewpoint of improving the smoothness of the object to be polished.
作為上述二氧化矽粒子之使用形態，就操作性之觀點而言，較佳為漿料狀。於本發明之研磨液組合物所包含之二氧化矽粒子為膠體二氧化矽之情形時，就製造容易性及經濟性之觀點而言，膠體二氧化矽較佳為自水玻璃或烷氧基矽烷之水解物獲得者，更佳為自水玻璃獲得者。自水玻璃獲得之二氧化矽粒子可利用自先前以來公知之方法製作。 The form of use of the above-mentioned cerium oxide particles is preferably in the form of a slurry from the viewpoint of workability. In the case where the cerium oxide particles contained in the polishing composition of the present invention are colloidal cerium oxide, the colloidal cerium oxide is preferably self-water glass or alkoxy group from the viewpoint of easiness of production and economy. The obtained hydrolyzate of decane is more preferably obtained from a water glass. The cerium oxide particles obtained from water glass can be produced by a method known from the prior art.
上述二氧化矽粒子亦可為利用矽烷偶合劑等對粒子表面進行了表面處理之二氧化矽粒子，但就提高研磨速度之觀點而言，較佳為未經表面處理之二氧化矽粒子。上述二氧化矽粒子中亦可包含Al或Zr等 Si以外之無機元素，但就提高研磨速度之觀點而言，較佳為固形物成分之主成分為SiO2，且SiO2以無水氧化物換算計較佳為90質量%以上，更佳為95質量%以上，進而較佳為99質量%以上。 The cerium oxide particles may be cerium oxide particles which have been surface-treated with a decane coupling agent or the like. However, from the viewpoint of improving the polishing rate, cerium oxide particles which have not been surface-treated are preferred. The cerium oxide particles may contain an inorganic element other than Si such as Al or Zr. However, from the viewpoint of improving the polishing rate, it is preferred that the main component of the solid content component is SiO 2 and SiO 2 is converted into anhydrous oxide. The amount is preferably 90% by mass or more, more preferably 95% by mass or more, and still more preferably 99% by mass or more.
關於本發明之研磨液組合物中之上述二氧化矽粒子之含量，就提高研磨速度之觀點而言，以SiO2換算濃度計較佳為1質量%以上，更佳為5質量%以上，進而較佳為10質量%以上。又，關於本發明之研磨液組合物中之二氧化矽粒子之含量，就降低研磨液組合物之成本及提高保存穩定性之觀點而言，以SiO2換算濃度計較佳為40質量%以下，更佳為30質量%以下，進而較佳為25質量%以下。 The content of the silicon dioxide particles of the above polishing liquid composition of the present invention, on the viewpoint of improving the polishing rate, the concentration of SiO 2 in terms of good care at least 1% by mass, more preferably not less than 5% by mass, and further more Preferably, it is 10% by mass or more. In addition, the content of the cerium oxide particles in the polishing liquid composition of the present invention is preferably 40% by mass or less in terms of SiO 2 conversion concentration from the viewpoint of lowering the cost of the polishing liquid composition and improving storage stability. It is more preferably 30% by mass or less, further preferably 25% by mass or less.
關於本發明之研磨液組合物中之上述二氧化矽粒子之藉由動態光散射法而測定之平均二次粒徑，就提高研磨速度之觀點而言，較佳為10nm以上，更佳為50nm以上，進而較佳為80nm以上，就提高經研磨之被研磨對象物之平滑性之觀點而言，較佳為500nm以下，更佳為300nm以下，進而較佳為200nm以下。再者，上述二氧化矽粒子之平均二次粒徑可藉由下述實施例所記載之方法而求出。 The average secondary particle diameter measured by the dynamic light scattering method of the above-mentioned ceria particles in the polishing composition of the present invention is preferably 10 nm or more, and more preferably 50 nm from the viewpoint of increasing the polishing rate. The above is more preferably 80 nm or more, and from the viewpoint of improving the smoothness of the object to be polished to be polished, it is preferably 500 nm or less, more preferably 300 nm or less, still more preferably 200 nm or less. Further, the average secondary particle diameter of the above cerium oxide particles can be determined by the method described in the following examples.
關於本發明之研磨液組合物中之上述二氧化矽粒子之BET比表面積，就提高研磨速度之觀點而言，較佳為10m2/g以上，更佳為20m2/g以上，進而較佳為30m2/g以上，就相同之觀點而言，較佳為200m2/g以下，更佳為100m2/g以下，進而較佳為60m2/g以下。 The BET specific surface area of the above-mentioned ceria particles in the polishing composition of the present invention is preferably 10 m 2 /g or more, more preferably 20 m 2 /g or more, and further preferably from the viewpoint of increasing the polishing rate. is 30m 2 / g or more, the same viewpoint, is preferably 200m 2 / g or less, more preferably 100m 2 / g or less, further preferably 60m 2 / g or less.
關於本發明之研磨液組合物中之上述二氧化矽粒子之平均一次粒徑，就提高經研磨之基板表面之平滑性之觀點而言，較佳為500nm以下，更佳為300nm以下，進而較佳為200nm以下，進而更佳為150nm以下，就確保高研磨速度之觀點而言，較佳為45nm以上，更佳為70nm以上。再者，上述二氧化矽粒子之平均一次粒徑如下述實施例所記載般，係於電子顯微鏡(TEM)觀察圖像中作為圓當量徑而求出之粒徑之數量平均。 The average primary particle diameter of the above-mentioned ceria particles in the polishing composition of the present invention is preferably 500 nm or less, more preferably 300 nm or less, from the viewpoint of improving the smoothness of the surface of the substrate to be polished. The thickness is preferably 200 nm or less, more preferably 150 nm or less, and from the viewpoint of ensuring a high polishing rate, it is preferably 45 nm or more, and more preferably 70 nm or more. Further, the average primary particle diameter of the above-mentioned cerium oxide particles is the number average of the particle diameters obtained as a circle-equivalent diameter in an electron microscope (TEM) observation image as described in the following examples.
關於本發明之研磨液組合物中之上述二氧化矽粒子之平均一次粒徑之下述變動係數，就提高研磨速度之觀點而言，較佳為1~50%，更佳為1~30%，進而較佳為1~10%。 The following coefficient of variation of the average primary particle diameter of the above-mentioned ceria particles in the polishing composition of the present invention is preferably from 1 to 50%, more preferably from 1 to 30%, from the viewpoint of increasing the polishing rate. Further preferably, it is 1 to 10%.
變動係數=(標準偏差/平均一次粒徑) Coefficient of variation = (standard deviation / average primary particle size)
本發明之研磨液組合物所包含之二氧化矽粒子(成分A)之粒子形狀可為球狀、金平糖型、締合型、異形型等任一種，就提高研磨速度之觀點而言，較佳為球狀或金平糖型，就同時實現研磨速度之提高與刮痕數之減少之觀點而言，更佳為球狀。再者，所謂「球狀二氧化矽粒子」，係指接近圓球之球形狀之粒子(通常市售之膠體二氧化矽)。 The particle shape of the cerium oxide particles (component A) contained in the polishing liquid composition of the present invention may be any of a spherical shape, a ginkgoose type, an associative type, and a profiled type, and is preferably a viewpoint of improving the polishing rate. In the case of a spherical or gold-plated sugar type, it is more preferably spherical in view of achieving an increase in the polishing rate and a reduction in the number of scratches. Further, the term "spherical cerium oxide particles" means particles having a spherical shape close to a sphere (commonly commercially available colloidal cerium oxide).
於本發明之研磨液組合物所包含之研磨粒(成分A)之粒子形狀為金平糖型、締合型、異形型之任一種之情形時，就提高研磨速度之觀點而言，本發明之研磨液組合物較佳為包含選自由金平糖型二氧化矽粒子A1、異形型二氧化矽粒子A2、及異形且金平糖型二氧化矽粒子A3所組成之群中之至少1種二氧化矽粒子。 When the particle shape of the abrasive grains (component A) contained in the polishing liquid composition of the present invention is any one of a ginkgoose type, an association type, and a profiled type, the polishing of the present invention is obtained from the viewpoint of improving the polishing rate. The liquid composition preferably contains at least one type of cerium oxide particle selected from the group consisting of a gold saccharide type cerium oxide particle A1, a heteromorphic cerium oxide particle A2, and a heteromorphic and gold glucoside cerium oxide particle A3.
就提高研磨速度之觀點而言，二氧化矽粒子(成分A)較佳為金平糖型二氧化矽粒子A1。於本說明書中，所謂「金平糖型二氧化矽粒子」，係指於球狀之粒子表面上具有特異之疣狀突起之二氧化矽粒子。二氧化矽粒子A1於一個或複數個實施形態中，係以最小之二氧化矽粒子之粒徑為基準而粒徑相差5倍以上的2個以上之粒子凝聚或融合而成之形狀。再者，上述粒徑可於電子顯微鏡(TEM等)觀察圖像中作為於1個粒子內所測定之圓當量徑而求出。二氧化矽粒子A2及二氧化矽粒子A3之粒徑亦能以相同之方式求出。 From the viewpoint of increasing the polishing rate, the cerium oxide particles (ingredient A) are preferably the glyphosic cerium oxide particles A1. In the present specification, the term "golden saccharide cerium oxide particles" refers to cerium oxide particles having a specific ridge-like protrusion on the surface of spherical particles. In one or a plurality of embodiments, the cerium oxide particles A1 have a shape in which two or more particles having a particle diameter differing by 5 or more are aggregated or fused, based on the particle diameter of the smallest cerium oxide particles. In addition, the particle diameter can be obtained as an equivalent circle diameter measured in one particle in an observation image of an electron microscope (TEM or the like). The particle diameters of the cerium oxide particles A2 and the cerium oxide particles A3 can also be determined in the same manner.
又，就提高研磨速度之觀點而言，二氧化矽粒子(成分A)較佳為異形型二氧化矽粒子A2。於本說明書中，所謂「異形型二氧化矽粒子」，係指2個以上之粒子、較佳為2~10個粒子凝聚或融合而成之形狀之二氧化矽粒子。二氧化矽粒子A2於一個或複數個實施形態中， 係以最小之二氧化矽粒子之粒徑為基準而粒徑相差1.5倍以內的2個以上之粒子凝聚或融合而成之形狀。 Further, from the viewpoint of increasing the polishing rate, the cerium oxide particles (component A) are preferably shaped cerium oxide particles A2. In the present specification, the "heteromorphic cerium oxide particles" means cerium oxide particles having a shape in which two or more particles, preferably 2 to 10 particles are aggregated or fused. The cerium oxide particles A2 are in one or more embodiments, A shape obtained by agglomerating or fusing two or more particles having a particle diameter of 1.5 or less based on the particle diameter of the smallest cerium oxide particles.
又，就提高研磨速度之觀點而言，二氧化矽粒子(成分A)較佳為異形且金平糖型之二氧化矽粒子A3。於本說明書中，所謂「異形且金平糖型二氧化矽粒子」，係指2個以上之粒子凝聚或融合而成之形狀之粒子、且具備上述金平糖型與上述異形型之中間之形狀及/或上述金平糖型與上述異形型兩者之特徵之二氧化矽粒子。二氧化矽粒子A3於一個或複數個實施形態中，係以凝聚或融合前之二氧化矽粒子1粒為基準而粒徑為1/5以下之較小粒子進而凝聚或融合於粒徑為1.5倍以內的2個以上之粒子凝聚或融合而成之粒子上而成之形狀。 Further, from the viewpoint of increasing the polishing rate, the cerium oxide particles (ingredient A) are preferably the bismuth dioxide particles A3 having a heterogeneous shape and a ginkgoose type. In the present specification, the "heteromorphic and glyphosic cerium oxide particles" are particles having a shape in which two or more particles are aggregated or fused, and have a shape and/or a shape between the above-mentioned ginkgoose type and the above-mentioned profiled type. The cerium oxide particles characterized by both the above-mentioned ginkgoose type and the above-mentioned profiled type. In one or more embodiments, the ceria particle A3 is a small particle having a particle diameter of 1/5 or less based on one particle of agglomerated or fused ceria particles, and is further aggregated or fused to a particle size of 1.5. A shape formed by agglomerated or fused particles of two or more particles within a multiple.
二氧化矽粒子(成分A)於一個或複數個實施形態中，包含二氧化矽粒子A1、A2、A3之任一種，二氧化矽粒子A1、A2、A3之任2種或二氧化矽粒子A1、A2、及A3之全部。關於二氧化矽粒子(成分A)中之二氧化矽粒子A1、A2、及A3之合計所占之比率(質量比)，就同時實現提高研磨速度與減少刮痕之觀點而言，較佳為50質量%以上，更佳為70質量%以上，進而較佳為80質量%以上，進而更佳為90質量%以上，進而更佳為實質上為100質量%，進而更佳為100質量%。 The cerium oxide particles (ingredient A) comprise, in one or more embodiments, any of the cerium oxide particles A1, A2, and A3, and two of the cerium oxide particles A1, A2, and A3 or the cerium oxide particles A1. All of A2, A2 and A3. The ratio (mass ratio) of the total of the cerium oxide particles A1, A2, and A3 in the cerium oxide particles (component A) is preferably from the viewpoint of simultaneously increasing the polishing rate and reducing scratches. 50% by mass or more, more preferably 70% by mass or more, further preferably 80% by mass or more, more preferably 90% by mass or more, still more preferably 100% by mass or more, still more preferably 100% by mass.
於二氧化矽粒子(成分A)包含二氧化矽粒子A1及A2之情形時，A1/A2之質量比率於一個或複數個實施形態中較佳為5/95~95/5之範圍。就同時實現提高研磨速度與減少刮痕之觀點而言，A1/A2之質量比率更佳為20/80~80/20，進而較佳為20/80~60/40，進而更佳為20/80~40/60，進而更佳為20/80~30/70。 In the case where the cerium oxide particles (ingredient A) contain the cerium oxide particles A1 and A2, the mass ratio of A1/A2 is preferably in the range of 5/95 to 95/5 in one or a plurality of embodiments. The mass ratio of A1/A2 is more preferably 20/80 to 80/20, and further preferably 20/80 to 60/40, and more preferably 20/, from the viewpoint of simultaneously improving the polishing speed and reducing scratches. 80~40/60, and more preferably 20/80~30/70.
於本發明之研磨液組合物所包含之二氧化矽粒子(成分A)之粒子形狀為金平糖型、締合型、異形型之任一種之情形時，於本說明書中，所謂粒子之絕對最大長度，係指粒子之輪廓線上之任意2點間之距離之最大值之長度。關於二氧化矽粒子(成分A)之絕對最大長度之 平均值(以下亦稱為「平均絕對最大長度」)，就提高研磨速度之觀點而言，較佳為80nm以上，更佳為90nm以上，進而較佳為100nm以上，進而更佳為110nm以上，進而更佳為120nm以上。關於二氧化矽粒子A之平均絕對最大長度，就相同之觀點而言，較佳為500nm以下，更佳為400nm以下，進而較佳為300nm以下，進而更佳為200nm以下，進而更佳為150nm以下。又，關於二氧化矽粒子(成分A)之平均絕對最大長度，就相同之觀點而言，較佳為80~500nm，更佳為90~400nm，進而較佳為90~300nm，進而更佳為90~150nm。若二氧化矽粒子(成分A)之平均絕對最大長度為上述範圍內，則可認為研磨切削時之物理研磨力較強，墊之研磨粒保持性提高，故而研磨速度有效地提高。再者，平均絕對最大長度可藉由實施例所記載之方法而求出。 In the case where the particle shape of the cerium oxide particles (component A) contained in the polishing composition of the present invention is any one of a ginkgoose type, an association type, and a profiled type, in the present specification, the absolute maximum length of the particles Is the length of the maximum of the distance between any two points on the contour of the particle. About the absolute maximum length of the cerium oxide particles (ingredient A) The average value (hereinafter also referred to as "average absolute maximum length") is preferably 80 nm or more, more preferably 90 nm or more, still more preferably 100 nm or more, and still more preferably 110 nm or more from the viewpoint of increasing the polishing rate. More preferably, it is 120 nm or more. The average absolute maximum length of the cerium oxide particles A is preferably 500 nm or less, more preferably 400 nm or less, still more preferably 300 nm or less, still more preferably 200 nm or less, and still more preferably 150 nm from the same viewpoint. the following. Further, the average absolute maximum length of the cerium oxide particles (component A) is preferably from 80 to 500 nm, more preferably from 90 to 400 nm, still more preferably from 90 to 300 nm, and still more preferably from the same viewpoint. 90~150nm. When the average absolute maximum length of the cerium oxide particles (component A) is within the above range, it is considered that the physical polishing force at the time of polishing cutting is strong, and the abrasive grain retainability of the mat is improved, so that the polishing rate is effectively improved. Further, the average absolute maximum length can be obtained by the method described in the examples.
[二氧化矽粒子(成分A)之面積比(b/a×100)] [Area ratio of cerium oxide particles (ingredient A) (b/a × 100)]
於本發明之研磨液組合物所包含之二氧化矽粒子(成分A)之粒子形狀為金平糖型、締合型、異形型之任一種之情形時，於本說明書中，所謂面積比(b/a×100)，係指將以粒子之絕對最大長度為直徑之圓之面積b除以由電子顯微鏡觀察所獲得之該粒子之投影面積a後乘以100所得之值(%)。 When the particle shape of the cerium oxide particles (component A) contained in the polishing liquid composition of the present invention is any one of a ginkgoose type, an association type, and a profiled type, in the present specification, the area ratio (b/) a × 100) is a value (%) obtained by dividing the area b of the circle having the absolute maximum length of the particle by the projection area a of the particle obtained by observation with an electron microscope and multiplying by 100.
於本發明之研磨液組合物所包含之二氧化矽粒子(成分A)之粒子形狀為金平糖型、締合型、異形型之任一種之情形時，關於二氧化矽粒子(成分A)，就同時實現提高研磨速度與減少刮痕之觀點而言，較佳為於所有二氧化矽粒子(成分A)中含有30質量%以上之構成二氧化矽粒子(成分A)之各二氧化矽粒子之面積比(b/a×100)為110~200%之二氧化矽粒子，更佳為含有30~100質量%，進而較佳為含有50~100質量%，進而更佳為含有70~100質量%，進而更佳為含有80~100質量%，進而更佳為含有90~100質量%。再者，構成二氧化矽粒子(成 分A)之各二氧化矽粒子之質量係將由電子顯微鏡觀察所獲得之該粒子之投影面積a作為球截面積換算成球而求出體積，進而將二氧化矽粒子之密度設為2.2g/cm3進行計算而獲得。 When the particle shape of the cerium oxide particles (component A) contained in the polishing composition of the present invention is any one of a ginkgoose type, an association type, and a profiled type, the cerium oxide particles (component A) are In view of the improvement of the polishing rate and the reduction of the scratches, it is preferable that all of the cerium oxide particles (component A) contain 30% by mass or more of each of the cerium oxide particles constituting the cerium oxide particles (ingredient A). The area ratio (b/a×100) is 110 to 200% of cerium oxide particles, more preferably 30 to 100% by mass, further preferably 50 to 100% by mass, and even more preferably 70 to 100% by mass. More preferably, it is 80 to 100% by mass, and more preferably 90 to 100% by mass. Further, the mass of each of the cerium oxide particles constituting the cerium oxide particles (component A) is obtained by converting the projected area a of the particles obtained by electron microscopic observation into a sphere as a spherical cross-sectional area, and obtaining a volume, thereby further oxidizing The density of the cerium particles was set to 2.2 g/cm 3 to obtain a calculation.
[若二氧化矽粒子(成分A)關於面積比(b/a×100)滿足上述條件，則可認為研磨切削時之物理研磨力較強，墊之研磨粒保持性提高，故而研磨速度有效地提高。再者，絕對最大長度可藉由實施例所記載之方法而求出。 [If the cerium oxide particles (component A) satisfy the above conditions with respect to the area ratio (b/a × 100), it is considered that the physical polishing force at the time of polishing cutting is strong, and the abrasive grain retention property of the pad is improved, so the polishing rate is effectively improve. Further, the absolute maximum length can be obtained by the method described in the examples.
關於二氧化矽粒子(成分A)之面積比(b/a×100)之平均值，就提高研磨速度之觀點而言，較佳為110%以上。又，就相同之觀點而言，二氧化矽粒子(成分A)之面積比(b/a×100)之平均值較佳為200%以下，更佳為180%以下，進而較佳為150%以下，進而更佳為140%以下。關於二氧化矽粒子(成分A)之面積比(b/a×100)之平均值，就提高研磨速度之觀點而言，較佳為110~200%，更佳為110~180%，進而較佳為110~150%，進而更佳為110~140%。又，關於二氧化矽粒子(成分A)之面積比(b/a×100)之平均值，就同時實現提高研磨速度與減少刮痕之觀點而言，較佳為110~200%，更佳為120~200%，進而較佳為130~200%，進而更佳為140~200%。再者，二氧化矽粒子(成分A)之面積比(b/a×100)之平均值係將平均絕對最大長度之圓面積b除以上述投影面積a之平均值後乘以100所得之值。 The average value of the area ratio (b/a × 100) of the cerium oxide particles (component A) is preferably 110% or more from the viewpoint of increasing the polishing rate. Further, from the same viewpoint, the average ratio of the area ratio (b/a × 100) of the cerium oxide particles (component A) is preferably 200% or less, more preferably 180% or less, still more preferably 150%. Hereinafter, it is more preferably 140% or less. The average value of the area ratio (b/a × 100) of the cerium oxide particles (component A) is preferably from 110 to 200%, more preferably from 110 to 180%, from the viewpoint of increasing the polishing rate. Good is 110~150%, and even better is 110~140%. Further, the average value of the area ratio (b/a × 100) of the cerium oxide particles (component A) is preferably from 110 to 200%, more preferably from the viewpoint of simultaneously increasing the polishing rate and reducing scratches. It is 120 to 200%, more preferably 130 to 200%, and still more preferably 140 to 200%. Further, the average value of the area ratio (b/a × 100) of the cerium oxide particles (component A) is obtained by dividing the circular area b of the average absolute maximum length by the average value of the projected area a and multiplying by 100. .
若二氧化矽粒子(成分A)關於面積比(b/a×100)滿足上述2個條件，則可認為研磨切削時之物理研磨力更強，墊之研磨粒保持性進一步提高，故而研磨速度進一步有效地提高。 When the cerium oxide particles (component A) satisfy the above two conditions with respect to the area ratio (b/a × 100), it is considered that the physical polishing force at the time of polishing cutting is stronger, and the polishing grain retention of the pad is further improved, so the polishing speed is increased. Further effectively improve.
<無機磷酸鹽化合物(成分B)> <Inorganic phosphate compound (ingredient B)>
就同時實現高速研磨與低表面粗糙度之觀點而言，本發明之研磨液組合物含有選自由正磷酸鹽、亞磷酸鹽、及次磷酸鹽所組成之群中之1種以上之無機磷酸鹽化合物(成分B)。作為無機磷酸鹽化合物， 就同時實現高速研磨與低表面粗糙度之觀點而言，更佳為選自正磷酸鹽及亞磷酸鹽中之1種以上。又，無機磷酸鹽化合物較佳為鹼金屬鹽、鹼土金屬鹽或銨鹽。作為鹼金屬鹽或鹼土金屬，較佳為鎂、鈣、鈉、及鉀。該等之中，就抑制二氧化矽粒子之凝聚之觀點而言，無機磷酸鹽化合物更佳為選自鈉鹽、鉀鹽及銨鹽中之至少1種。 The polishing liquid composition of the present invention contains at least one inorganic phosphate selected from the group consisting of orthophosphates, phosphites, and hypophosphites, from the viewpoint of achieving both high-speed polishing and low surface roughness. Compound (ingredient B). As an inorganic phosphate compound, From the viewpoint of achieving high-speed polishing and low surface roughness at the same time, it is more preferably one or more selected from the group consisting of orthophosphates and phosphites. Further, the inorganic phosphate compound is preferably an alkali metal salt, an alkaline earth metal salt or an ammonium salt. As the alkali metal salt or alkaline earth metal, magnesium, calcium, sodium, and potassium are preferable. Among these, the inorganic phosphate compound is more preferably at least one selected from the group consisting of a sodium salt, a potassium salt, and an ammonium salt from the viewpoint of suppressing aggregation of the cerium oxide particles.
作為無機磷酸鹽化合物(成分B)之具體例，就同時實現高速研磨與低表面粗糙度之觀點而言，可列舉：磷酸鈉(Na3PO4)、磷酸鉀(K3PO4)、磷酸氫二鈉(Na2HPO4)、磷酸二氫鈉(NaH2PO4)、磷酸二氫鉀(KH2PO4)、磷酸二氫銨(NH4H2PO4)、磷酸氫二鉀(K2HPO4)、磷酸氫二銨((NH4)2HPO4)等正磷酸鹽；亞磷酸鈉(Na2HPO3)、亞磷酸鉀(K2HPO3)等亞磷酸鹽；次磷酸鈉(NaH2PO2)、次磷酸鉀(KH2PO2)、次磷酸銨(NH4H2PO2)等次磷酸鹽，該等之中，就同時實現高速研磨與低表面粗糙度之觀點而言，較佳為選自由磷酸氫二鈉、磷酸氫二鉀、磷酸氫二銨、亞磷酸鈉、次磷酸鈉及次磷酸銨所組成之群中之1種以上之無機磷酸鹽化合物。又，該等無機鹽亦可呈水合物結構。 Specific examples of the inorganic phosphate compound (ingredient B) include sodium phosphate (Na 3 PO 4 ), potassium phosphate (K 3 PO 4 ), and phosphoric acid from the viewpoint of achieving high-speed polishing and low surface roughness at the same time. Disodium hydrogen (Na 2 HPO 4 ), sodium dihydrogen phosphate (NaH 2 PO 4 ), potassium dihydrogen phosphate (KH 2 PO 4 ), ammonium dihydrogen phosphate (NH 4 H 2 PO 4 ), dipotassium hydrogen phosphate ( Orthophosphorous acid such as K 2 HPO 4 ), diammonium phosphate ((NH 4 ) 2 HPO 4 ); phosphite such as sodium phosphite (Na 2 HPO 3 ), potassium phosphite (K 2 HPO 3 ); hypophosphorous acid a hypophosphite such as sodium (NaH 2 PO 2 ), potassium hypophosphite (KH 2 PO 2 ) or ammonium hypophosphite (NH 4 H 2 PO 2 ), among which high-speed grinding and low surface roughness are simultaneously achieved. In view of the above, one or more inorganic phosphate compounds selected from the group consisting of disodium hydrogen phosphate, dipotassium hydrogen phosphate, diammonium hydrogen phosphate, sodium phosphite, sodium hypophosphite, and ammonium hypophosphite are preferred. Further, the inorganic salts may also have a hydrate structure.
關於本發明之研磨液組合物所包含之無機磷酸鹽化合物(成分B)之含量，就同時實現高速研磨與低表面粗糙度之觀點而言，較佳為1質量ppm以上，更佳為10質量ppm以上，進而較佳為100質量ppm以上，進而更佳為200質量ppm以上，進而更佳為500質量ppm以上，進而更佳為800ppm以上。又，關於本發明之研磨液組合物所包含之無機磷酸鹽化合物(成分B)之含量，就降低經研磨之被研磨對象之表面粗糙度之觀點而言，較佳為5000質量ppm以下，更佳為4000質量ppm以下，進而較佳為3000質量ppm以下，進而更佳為2000質量ppm以下。 The content of the inorganic phosphate compound (ingredient B) contained in the polishing composition of the present invention is preferably 1 mass ppm or more, more preferably 10 mass, from the viewpoint of achieving high-speed polishing and low surface roughness at the same time. The ppm or more is more preferably 100 ppm by mass or more, still more preferably 200 ppm by mass or more, still more preferably 500 ppm by mass or more, and still more preferably 800 ppm or more. In addition, the content of the inorganic phosphate compound (ingredient B) contained in the polishing composition of the present invention is preferably 5,000 ppm by mass or less from the viewpoint of lowering the surface roughness of the object to be polished to be polished. It is preferably 4,000 ppm by mass or less, more preferably 3,000 ppm by mass or less, and still more preferably 2,000 ppm by mass or less.
關於本發明之研磨液組合物中之二氧化矽粒子(成分A)與無機磷酸鹽化合物(成分B)之含量比[二氧化矽粒子之含量(質量ppm)/無機磷 酸鹽化合物之含量(質量ppm)]，就降低經研磨之被研磨對象之表面粗糙度之觀點而言，較佳為2以上，更佳為20以上，進而較佳為100以上，且較佳為10000以下，更佳為5000以下，進而較佳為2000以下。 Content ratio of cerium oxide particles (ingredient A) to inorganic phosphate compound (ingredient B) in the polishing composition of the present invention [content of cerium oxide particles (ppm by mass) / inorganic phosphorus The content of the acid salt compound (ppm by mass) is preferably 2 or more, more preferably 20 or more, still more preferably 100 or more, from the viewpoint of lowering the surface roughness of the object to be polished. It is 10,000 or less, more preferably 5,000 or less, further preferably 2,000 or less.
[水系介質(成分C)] [aqueous medium (ingredient C)]
作為本發明之研磨液組合物所包含之水系介質(成分C)，可列舉離子交換水或超純水等水或水與溶劑之混合介質等，作為上述溶劑，較佳為可與水混合之溶劑(例如乙醇等醇)。作為水系介質，其中更佳為離子交換水或超純水，進而較佳為超純水。於本發明之成分C為水與溶劑之混合介質之情形時，水相對於混合介質整體之比率並未特別限定，就經濟性之觀點而言，較佳為95質量%以上，更佳為98質量%以上，進而較佳為實質上為100質量%，進而更佳為100質量%。 The aqueous medium (component C) to be contained in the polishing composition of the present invention may, for example, be water such as ion-exchanged water or ultrapure water or a mixed medium of water and a solvent, and the solvent is preferably mixed with water. Solvent (for example, an alcohol such as ethanol). As the aqueous medium, it is more preferably ion-exchanged water or ultrapure water, and further preferably ultrapure water. In the case where the component C of the present invention is a mixed medium of water and a solvent, the ratio of the water to the entire mixed medium is not particularly limited, and from the viewpoint of economy, it is preferably 95% by mass or more, and more preferably 98. The mass% or more is further preferably substantially 100% by mass, and more preferably 100% by mass.
本發明之研磨液組合物中之水系介質(成分C)之含量並未特別限定，只要為成分A、成分B、下述任意成分之剩餘部分即可。 The content of the aqueous medium (ingredient C) in the polishing liquid composition of the present invention is not particularly limited, and may be any of the component A, the component B, and the remainder of any of the following components.
關於本發明之研磨液組合物之25℃下之pH，就提高研磨速度之觀點而言，pH為8以上，較佳為9以上，更佳為10以上，就抑制膠體二氧化矽之溶解、提高穩定性之觀點而言，較佳為未達14。 The pH of the polishing composition of the present invention at 25 ° C is such that the pH is 8 or more, preferably 9 or more, and more preferably 10 or more, from the viewpoint of increasing the polishing rate, thereby suppressing the dissolution of colloidal cerium oxide. From the viewpoint of improving stability, it is preferably less than 14.
本發明之研磨液組合物亦可根據其使用用途進而包含自先前以來公知之任意成分。於本發明之研磨液組合物為例如半導體元件等電子零件用藍寶石基板用研磨液組合物(例如LED用藍寶石基板用研磨液組合物)之情形時，本發明之研磨液組合物亦可進而包含界面活性劑、防銹劑、分散劑、pH調整劑、抗菌劑、抗靜電劑等。本發明之研磨液組合物亦可含有微量之過氧化氫等氧化劑，但就提高研磨速度之觀點而言，較佳為不含過氧化氫等氧化劑。 The polishing composition of the present invention may further contain any component known from the prior art depending on the intended use thereof. In the case where the polishing liquid composition of the present invention is a polishing liquid composition for a sapphire substrate for an electronic component such as a semiconductor device (for example, a polishing liquid composition for sapphire substrates for LEDs), the polishing composition of the present invention may further comprise Surfactant, rust inhibitor, dispersant, pH adjuster, antibacterial agent, antistatic agent, and the like. The polishing composition of the present invention may contain a trace amount of an oxidizing agent such as hydrogen peroxide. However, from the viewpoint of increasing the polishing rate, it is preferred that the oxidizing agent such as hydrogen peroxide is not contained.
[研磨液組合物之製備方法] [Preparation method of polishing liquid composition]
本發明之研磨液組合物可藉由利用公知之方法將各成分混合而製備。就經濟性之觀點而言，研磨液組合物通常大多情況下係以濃縮 液之形式製造，並於使用時將其稀釋。上述研磨液組合物可直接使用，若為濃縮液則稀釋後使用即可。於將濃縮液稀釋之情形時，其稀釋倍率並無特別限制，可根據上述濃縮液中之各成分之濃度或研磨條件等適當決定。再者，上述各成分之含量係使用時之含量。 The polishing composition of the present invention can be produced by mixing the components by a known method. From the standpoint of economy, the slurry composition is usually concentrated in most cases. It is manufactured in the form of a liquid and diluted at the time of use. The above polishing liquid composition can be used as it is, and if it is a concentrated liquid, it can be used after dilution. In the case where the concentrate is diluted, the dilution ratio is not particularly limited, and may be appropriately determined depending on the concentration of each component in the concentrate, the polishing conditions, and the like. Further, the content of each of the above components is the content at the time of use.
繼而，對使用本發明之研磨液組合物的本發明之藍寶石板之製造方法之一例、及本發明之被研磨藍寶石板之研磨方法之一例進行說明。 Next, an example of a method for producing a sapphire plate of the present invention using the polishing composition of the present invention and an example of a method for polishing a sapphire plate to be polished according to the present invention will be described.
[被研磨對象] [Abraded object]
於本發明之藍寶石板之製造方法之一例(亦存在簡稱為「本發明之製造方法之一例」之情形)、及本發明之被研磨藍寶石板之研磨方法之一例(亦存在簡稱為「本發明之研磨方法之一例」之情形)中，經研磨之被研磨對象之形狀並無特別限制，例如不僅可為圓盤狀、平板狀、塊狀、角柱狀等具有平面部之形狀，亦可為透鏡等具有曲面部之形狀。又，上述被研磨對象係被用作智慧型手機等移動終端裝置之覆蓋玻璃之藍寶石板、LED用藍寶石基板等各式各樣，本發明之研磨液組合物適合作為LED用藍寶石基板、被用作智慧型手機等移動終端裝置之覆蓋玻璃之藍寶石板之製造方法之研磨步驟中所使用之研磨液組合物。 An example of a method for producing a sapphire board according to the present invention (there is also a case where it is simply referred to as "an example of the manufacturing method of the present invention"), and an example of a method for polishing a sapphire sheet to be polished according to the present invention (also referred to as "the present invention" In the case of an example of the polishing method, the shape of the object to be polished to be polished is not particularly limited, and may be, for example, a disk shape, a flat plate shape, a block shape, a prismatic shape, or the like, or a flat portion. The lens or the like has a shape of a curved surface portion. In addition, the above-mentioned object to be polished is used as a sapphire plate for a cover glass of a mobile terminal device such as a smart phone, or a sapphire substrate for LED, and the polishing composition of the present invention is suitable as a sapphire substrate for LEDs. A polishing liquid composition used in a polishing step of a method for producing a sapphire sheet covering a glass of a mobile terminal device such as a smart phone.
因此，本發明之藍寶石板之製造方法之一例係LED用藍寶石基板或智慧型手機等移動終端裝置之覆蓋玻璃用藍寶石板等藍寶石板之製造方法，且包括使用本發明之研磨液組合物對被研磨藍寶石板進行研磨之步驟。又，本發明之被研磨藍寶石板之研磨方法之一例係LED用藍寶石基板或智慧型手機等移動終端裝置之覆蓋玻璃用藍寶石板等藍寶石板之研磨方法，且包括使用本發明之研磨液組合物對被研磨藍寶石板進行研磨之步驟。 Therefore, an example of the method for producing a sapphire plate according to the present invention is a method for producing a sapphire plate such as a sapphire plate for a mobile terminal device such as a sapphire substrate for a LED or a smart phone, and includes using the polishing liquid composition of the present invention. The step of grinding the sapphire plate for grinding. Further, an example of the method for polishing a sapphire plate to be polished according to the present invention is a method for polishing a sapphire plate such as a sapphire plate for a mobile terminal device such as a sapphire substrate for LED or a smart phone, and includes the use of the polishing composition of the present invention. The step of grinding the ground sapphire plate.
對上述被研磨藍寶石板進行研磨之步驟分為：第一研磨步驟(粗 研磨步驟)，其使將藍寶石單晶錠切割為薄圓板狀而獲得之晶圓平面化；及第二研磨步驟(精研磨)，其於對經粗研磨之晶圓進行蝕刻後，使晶圓表面鏡面化；本發明之研磨液組合物可於第一研磨步驟及第二研磨步驟之任一步驟中使用。然而，就提高藍寶石板之表面平滑性及生產性之觀點而言，本發明之研磨液組合物較佳為於第二研磨步驟中使用。通常於第一研磨步驟中使用包含金剛石作為研磨粒之研磨液組合物。 The step of grinding the above-mentioned ground sapphire plate is divided into: a first grinding step (thick a polishing step), which planarizes the wafer obtained by cutting the sapphire single crystal ingot into a thin circular plate shape; and a second polishing step (fine polishing), which is performed after etching the rough-polished wafer The round surface is mirrored; the polishing composition of the present invention can be used in any of the first grinding step and the second grinding step. However, the polishing composition of the present invention is preferably used in the second grinding step from the viewpoint of improving the surface smoothness and productivity of the sapphire sheet. A slurry composition comprising diamond as abrasive particles is typically used in the first milling step.
作為本發明之製造方法之一例及本發明之研磨方法之一例中所使用之研磨裝置，並無特別限制，可使用具備保持被研磨藍寶石板之夾具(載體：玻璃環氧製材料等)與研磨布(研磨墊)之研磨裝置，且可為兩面研磨裝置及單面研磨裝置之任一種。 The polishing apparatus used in an example of the production method of the present invention and the polishing method of the present invention is not particularly limited, and a jig (carrier: glass epoxy material, etc.) and polishing having a sapphire plate to be polished can be used. A polishing device for a cloth (polishing pad), and may be any of a double-sided polishing device and a single-sided polishing device.
上述研磨墊並無特別限制，可使用先前公知者。作為研磨墊之材質，可列舉有機高分子等，作為上述有機高分子，可列舉聚胺基甲酸酯等。上述研磨墊之形狀較佳為不織布狀。例如，作為不織布研磨墊，可較佳地使用SUBA800(Nitta Haas製造)。 The polishing pad described above is not particularly limited, and those known in the art can be used. The material of the polishing pad is, for example, an organic polymer, and examples of the organic polymer include a polyurethane. The shape of the polishing pad is preferably a non-woven fabric. For example, as a non-woven polishing pad, SUBA800 (manufactured by Nitta Haas) can be preferably used.
使用該研磨裝置之本發明之製造方法之一例及本發明之研磨方法之一例中包括如下步驟：利用載體保持被研磨藍寶石板並利用貼附有研磨墊之研磨壓盤夾持被研磨藍寶石板，將本發明之研磨液組合物供給至研磨墊與被研磨藍寶石板之間，一面使被研磨藍寶石板與上述研磨墊接觸，一面移動研磨墊及/或被研磨藍寶石板，藉此對被研磨藍寶石板進行研磨。 An example of the manufacturing method of the present invention using the polishing apparatus and an example of the polishing method of the present invention include the steps of holding a ground sapphire plate with a carrier and holding the ground sapphire plate with a polishing platen to which a polishing pad is attached, The polishing composition of the present invention is supplied between the polishing pad and the ground sapphire plate, and the polished sapphire plate is brought into contact with the polishing pad to move the polishing pad and/or the sapphire plate to be polished, thereby polishing the sapphire The plate is ground.
關於本發明之製造方法之一例及研磨方法之一例中之研磨負載，就提高研磨速度之觀點而言，較佳為50g/cm2以上，更佳為100g/cm2以上，進而較佳為150g/cm2以上，進而更佳為200g/cm2以上。又，若考慮到裝置、墊等之耐久性，則上述研磨負載較佳為400g/cm2以下，更佳為350g/cm2以下。上述研磨負載之調整可藉由對壓 盤或被研磨藍寶石板等之空氣壓或砝碼之負荷而進行。研磨負載意指於研磨時施加於被研磨藍寶石板之研磨面之壓盤之壓力。 About one case of one case and method for manufacturing the polishing method of the present invention in the polishing load, to improving the polishing speed, it is preferably 50g / cm 2 or more, more preferably 100g / cm 2 or more, and further preferably 150g /cm 2 or more, and more preferably 200 g/cm 2 or more. Moreover, in consideration of the durability of the device, the mat, and the like, the polishing load is preferably 400 g/cm 2 or less, and more preferably 350 g/cm 2 or less. The adjustment of the grinding load can be performed by a load on the air pressure or weight of the platen or the sapphire plate to be polished. The grinding load means the pressure applied to the platen of the abrasive surface of the ground sapphire plate during grinding.
本發明之研磨液組合物之供給方法可使用如下方法等：於研磨液組合物之構成成分預先經充分混合之狀態下利用泵等供給至研磨墊與被研磨藍寶石板之間之方法；及於即將進行研磨之前之供給線內等將上述構成成分混合後供給之方法。就提高研磨速度之觀點及減少裝置負荷之觀點而言，較佳為於研磨液組合物之構成成分預先經充分混合之狀態下利用泵等將研磨液組合物供給至研磨墊與被研磨藍寶石板之間之方法。 The method of supplying the polishing composition of the present invention may be a method in which a component of the polishing composition is supplied to a polishing pad and a ground sapphire plate by a pump or the like in a state where the components of the polishing composition are sufficiently mixed in advance; A method in which the above constituent components are mixed and supplied in a supply line immediately before polishing. From the viewpoint of increasing the polishing rate and reducing the load on the device, it is preferred that the polishing composition is supplied to the polishing pad and the ground sapphire plate by a pump or the like while the constituent components of the polishing liquid composition are sufficiently mixed in advance. The method between.
關於研磨液組合物之供給速度，就降低成本之觀點而言，較佳為對被研磨藍寶石板每1cm2為20mL/min以下，更佳為10mL/min以下，進而較佳為5mL/min以下。又，關於上述供給速度，就提高研磨速度之觀點而言，較佳為對被研磨藍寶石板每1cm2為0.01mL/min以上，更佳為0.1mL/min以上，進而較佳為0.5mL/min以上。 The supply rate of the polishing liquid composition is preferably 20 mL/min or less, more preferably 10 mL/min or less, and still more preferably 5 mL/min or less per 1 cm 2 of the sapphire plate to be polished. . Further, the supply speed is preferably 0.01 mL/min or more, more preferably 0.1 mL/min or more, and still more preferably 0.5 mL per 1 cm 2 of the sapphire plate to be polished. Min or above.
於本發明之製造方法之一例及本發明之研磨方法之一例中使用本發明之研磨液組合物，因此被研磨藍寶石板之研磨速度較快，且可降低研磨後之基板表面之表面粗糙度。 Since the polishing liquid composition of the present invention is used in an example of the production method of the present invention and an example of the polishing method of the present invention, the polishing rate of the ground sapphire plate is fast, and the surface roughness of the surface of the substrate after polishing can be reduced.
於本發明之製造方法之另一例中包括如下步驟：對被研磨藍寶石板供給本發明之研磨液組合物，對上述被研磨藍寶石板進行研磨；及使用上述步驟中使用之上述研磨液組合物，對上述被研磨藍寶石板以外之被研磨藍寶石板進行研磨。 Another example of the production method of the present invention includes the steps of: supplying the polishing composition of the present invention to the ground sapphire plate, grinding the ground sapphire plate; and using the above-mentioned polishing liquid composition used in the above step, The ground sapphire plate other than the ground sapphire plate is ground.
本發明進而揭示以下<1>~<22>。 The present invention further discloses the following <1> to <22>.
<1>一種藍寶石板用研磨液組合物，其含有二氧化矽粒子(成分A)、選自由正磷酸鹽、亞磷酸鹽、及次磷酸鹽所組成之群中之1種以上之無機磷酸鹽化合物(成分B)及水系介質(成分C)，且25℃下之pH為8以上。 <1> A polishing liquid composition for sapphire sheets, comprising cerium oxide particles (ingredient A), one or more inorganic phosphates selected from the group consisting of orthophosphates, phosphites, and hypophosphites The compound (ingredient B) and the aqueous medium (ingredient C) had a pH of 8 or more at 25 °C.
<2>如上述<1>之藍寶石板用研磨液組合物，其中上述無機磷酸鹽化合物較佳為選自由正磷酸鹽及亞磷酸鹽所組成之群中之1種以上之無機磷酸鹽化合物。 <2> The polishing liquid composition for sapphire sheets according to the above <1>, wherein the inorganic phosphate compound is preferably one or more inorganic phosphate compounds selected from the group consisting of orthophosphates and phosphites.
<3>如上述<1>或<2>之藍寶石板用研磨液組合物，其中上述無機磷酸鹽化合物較佳為選自鹼金屬鹽、鹼土金屬鹽、及銨鹽中之1種以上，更佳為選自鎂鹽、鈣鹽、鈉鹽、鉀鹽及銨鹽中之1種以上，進而較佳為選自鈉鹽、鉀鹽及銨鹽中之1種以上。 (3) The polishing liquid composition for sapphire sheets according to the above <1>, wherein the inorganic phosphate compound is preferably one or more selected from the group consisting of an alkali metal salt, an alkaline earth metal salt, and an ammonium salt. It is preferably one or more selected from the group consisting of a magnesium salt, a calcium salt, a sodium salt, a potassium salt, and an ammonium salt, and more preferably one or more selected from the group consisting of a sodium salt, a potassium salt, and an ammonium salt.
<4>如上述<1>至<3>中任一項之藍寶石板用研磨液組合物，其中上述無機磷酸鹽化合物較佳為選自由磷酸鈉(Na3PO4)、磷酸鉀(K3PO4)、磷酸氫二鈉(Na2HPO4)、磷酸二氫鈉(NaH2PO4)、磷酸二氫鉀(KH2PO4)、磷酸二氫銨(NH4H2PO4)、磷酸氫二鉀(K2HPO4)、磷酸氫二銨((NH4)2HPO4)、亞磷酸鈉(Na2HPO3)、亞磷酸鉀(K2HPO3)、次磷酸鈉(NaH2PO2)、次磷酸鉀(KH2PO2)、及次磷酸銨(NH4H2PO2)所組成之群中之1種以上之無機磷酸鹽化合物，更佳為選自由磷酸氫二鈉、磷酸氫二鉀、磷酸氫二銨、亞磷酸鈉、次磷酸鈉、及次磷酸銨所組成之群中之1種以上之無機磷酸鹽化合物。 The polishing composition for sapphire sheets according to any one of the above aspects, wherein the inorganic phosphate compound is preferably selected from the group consisting of sodium phosphate (Na 3 PO 4 ) and potassium phosphate (K 3 ). PO 4 ), disodium hydrogen phosphate (Na 2 HPO 4 ), sodium dihydrogen phosphate (NaH 2 PO 4 ), potassium dihydrogen phosphate (KH 2 PO 4 ), ammonium dihydrogen phosphate (NH 4 H 2 PO 4 ), Dipotassium hydrogen phosphate (K 2 HPO 4 ), diammonium phosphate ((NH 4 ) 2 HPO 4 ), sodium phosphite (Na 2 HPO 3 ), potassium phosphite (K 2 HPO 3 ), sodium hypophosphite (NaH) One or more inorganic phosphate compounds of the group consisting of 2 PO 2 ), potassium hypophosphite (KH 2 PO 2 ), and ammonium hypophosphite (NH 4 H 2 PO 2 ) are more preferably selected from the group consisting of hydrogen phosphate One or more inorganic phosphate compounds of the group consisting of sodium, dipotassium hydrogen phosphate, diammonium hydrogen phosphate, sodium phosphite, sodium hypophosphite, and ammonium hypophosphite.
<5>如上述<1>至<4>中任一項之藍寶石板用研磨液組合物，其中上述藍寶石板用研磨液組合物中之上述無機磷酸鹽化合物(成分B)之含量較佳為1質量ppm以上，更佳為10質量ppm以上，進而較佳為100質量ppm以上，進而更佳為200質量ppm以上，進而更佳為500質量ppm以上，進而更佳為800ppm以上，且較佳為5000質量ppm以下，更佳為4000質量ppm以下，進而較佳為3000質量ppm以下，進而更佳為2000質量ppm以下，進而更佳為1500質量ppm以下。 The polishing composition for sapphire sheets according to any one of the above aspects, wherein the content of the inorganic phosphate compound (ingredient B) in the polishing composition for sapphire sheets is preferably 1 ppm by mass or more, more preferably 10 ppm by mass or more, still more preferably 100 ppm by mass or more, still more preferably 200 ppm by mass or more, still more preferably 500 ppm by mass or more, still more preferably 800 ppm or more, and more preferably It is 5,000 ppm by mass or less, more preferably 4,000 ppm by mass or less, further preferably 3,000 ppm by mass or less, further preferably 2,000 ppm by mass or less, and still more preferably 1,500 ppm by mass or less.
<6>如上述<1>至<5>中任一項之藍寶石板用研磨液組合物，其中上述二氧化矽粒子(成分A)與無機磷酸鹽化合物(成分B)之含量比[二氧化矽粒子之含量(質量ppm)/無機磷酸鹽化合物之含量(質量 ppm)]較佳為2以上，更佳為20以上，進而較佳為100以上，且較佳為10000以下，更佳為5000以下，進而較佳為2000以下。 The polishing composition for sapphire sheets according to any one of the above-mentioned <1> to <5> wherein the content ratio of the above-mentioned cerium oxide particles (ingredient A) to inorganic phosphate compound (ingredient B) is [2. Content of cerium particles (ppm by mass) / content of inorganic phosphate compounds (mass The ppm) is preferably 2 or more, more preferably 20 or more, still more preferably 100 or more, and is preferably 10,000 or less, more preferably 5,000 or less, still more preferably 2,000 or less.
<7>如上述<1>至<6>中任一項之藍寶石板用研磨液組合物，其中上述藍寶石基板用研磨液組合物中之上述二氧化矽粒子之含量以SiO2換算濃度計較佳為1質量%以上，更佳為5質量%以上，進而較佳為10質量%以上，且較佳為40質量%以下，更佳為30質量%以下，進而較佳為25質量%以下。 The polishing composition for a sapphire plate according to any one of the above aspects, wherein the content of the cerium oxide particles in the polishing composition for sapphire substrate is preferably SiO 2 . It is 1% by mass or more, more preferably 5% by mass or more, further preferably 10% by mass or more, and more preferably 40% by mass or less, more preferably 30% by mass or less, and still more preferably 25% by mass or less.
<8>如上述<1>至<7>中任一項之藍寶石板用研磨液組合物，其中上述二氧化矽粒子之利用動態光散射法而測定之平均二次粒徑較佳為10nm以上，更佳為50nm以上，進而較佳為80nm以上，且較佳為500nm以下，更佳為300nm以下，進而較佳為200nm以下。 The polishing liquid composition for sapphire sheets according to any one of the above-mentioned items, wherein the average particle diameter of the cerium oxide particles measured by a dynamic light scattering method is preferably 10 nm or more. More preferably, it is 50 nm or more, further preferably 80 nm or more, and is preferably 500 nm or less, more preferably 300 nm or less, still more preferably 200 nm or less.
<9>如上述<1>至<8>中任一項之藍寶石板用研磨液組合物，其中上述二氧化矽粒子之平均一次粒徑較佳為500nm以下，更佳為300nm以下，進而較佳為200nm以下，進而更佳為150nm以下，且較佳為45nm以上，更佳為70nm以上。 The polishing liquid composition for sapphire sheets according to any one of the above-mentioned items, wherein the cerium oxide particles have an average primary particle diameter of preferably 500 nm or less, more preferably 300 nm or less, and further It is preferably 200 nm or less, more preferably 150 nm or less, and is preferably 45 nm or more, and more preferably 70 nm or more.
<10>如上述<1>至<9>中任一項之藍寶石板用研磨液組合物，其中上述二氧化矽粒子之BET比表面積較佳為10m2/g以上，更佳為20m2/g以上，進而較佳為30m2/g以上，且較佳為200m2/g以下，更佳為100m2/g以下，進而較佳為60m2/g以下。 The polishing composition for sapphire sheets according to any one of the above-mentioned items, wherein the cerium oxide particles have a BET specific surface area of preferably 10 m 2 /g or more, more preferably 20 m 2 / g or more is more preferably 30 m 2 /g or more, and is preferably 200 m 2 /g or less, more preferably 100 m 2 /g or less, still more preferably 60 m 2 /g or less.
<11>如上述<1>至<10>中任一項之藍寶石板用研磨液組合物，其中上述二氧化矽粒子(成分A)包含選自由金平糖型二氧化矽粒子A1、異形型二氧化矽粒子A2、及異形且金平糖型二氧化矽粒子A3所組成之群中之至少1種二氧化矽粒子。 The polishing composition for sapphire sheets according to any one of the above-mentioned <1>, wherein the cerium oxide particles (ingredient A) are selected from the group consisting of a gold-separated cerium oxide particle A1 and a hetero-type oxidizing agent. At least one type of cerium oxide particles of the group consisting of cerium particles A2 and heterogeneous and glucosinolate cerium oxide particles A3.
<12>如上述<11>之藍寶石板用研磨液組合物，其中上述二氧化矽粒子(成分A)中之金平糖型二氧化矽粒子A1、異形型二氧化矽粒子A2、及異形且金平糖型二氧化矽粒子A3之合計所占之比率(質量比) 較佳為50質量%以上，更佳為70質量%以上，進而較佳為80質量%以上，進而更佳為90質量%以上，進而更佳為實質上為100質量%，進而更佳為100質量%。 <12> The polishing liquid composition for sapphire sheets according to the above <11>, wherein the cerium oxide particles (component A) are the glucosinolate type cerium oxide particles A1, the shaped cerium oxide particles A2, and the heteromorphic and glucosinolate type. Ratio of mass of cerium oxide particles A3 (mass ratio) It is preferably 50% by mass or more, more preferably 70% by mass or more, still more preferably 80% by mass or more, still more preferably 90% by mass or more, still more preferably substantially 100% by mass, and still more preferably 100% by mass. quality%.
<13>如上述<11>或<12>之藍寶石板用研磨液組合物，其中於上述二氧化矽粒子(成分A)包含金平糖型二氧化矽粒子A1與異形型二氧化矽粒子A2兩者之情形時，質量比率(金平糖型二氧化矽粒子A1/異形型二氧化矽粒子A2)較佳為5/95~95/5，更佳為20/80~80/20，進而較佳為20/80~60/40，進而更佳為20/80~40/60，進而更佳為20/80~30/70。 <13> The polishing composition for sapphire sheets according to the above <11> or <12>, wherein the cerium oxide particles (component A) comprise both the gold saccharide type cerium oxide particle A1 and the heteromorphic cerium oxide particle A2. In the case of the case, the mass ratio (Ginkgo saccharide cerium oxide particle A1/shaped cerium oxide particle A2) is preferably 5/95 to 95/5, more preferably 20/80 to 80/20, and still more preferably 20 /80~60/40, and more preferably 20/80~40/60, and even better 20/80~30/70.
<14>如上述<11>至<13>中任一項之藍寶石板用研磨液組合物，其中上述二氧化矽粒子(成分A)之平均絕對最大長度較佳為80nm以上，更佳為90nm以上，進而較佳為100nm以上，進而更佳為110nm以上，進而更佳為120nm以上，且較佳為500nm以下，更佳為400nm以下，進而較佳為300nm以下，進而更佳為200nm以下，進而更佳為150nm以下。 The polishing composition for sapphire sheets according to any one of the above-mentioned <11>, wherein the average absolute maximum length of the cerium oxide particles (component A) is preferably 80 nm or more, more preferably 90 nm. The above is more preferably 100 nm or more, still more preferably 110 nm or more, still more preferably 120 nm or more, further preferably 500 nm or less, more preferably 400 nm or less, further preferably 300 nm or less, and still more preferably 200 nm or less. More preferably, it is 150 nm or less.
<15>如上述<11>至<14>中任一項之藍寶石板用研磨液組合物，其中較佳為於所有二氧化矽粒子(成分A)中含有30質量%以上之構成上述二氧化矽粒子(成分A)之各二氧化矽粒子之面積比(b/a×100)為110~200%之二氧化矽粒子，更佳為含有30~100質量%，進而較佳為含有50~100質量%，進而更佳為含有70~100質量%，進而更佳為含有80~100質量%，進而更佳為含有90~100質量%。 The polishing composition for sapphire sheets according to any one of the above-mentioned <11> to <14>, wherein it is preferable that the cerium oxide particles (component A) contain 30% by mass or more of the above-mentioned oxidizing agent. The area ratio (b/a×100) of each of the cerium oxide particles (component A) is 110 to 200% of cerium oxide particles, more preferably 30 to 100% by mass, and even more preferably 50%. 100% by mass, more preferably 70 to 100% by mass, still more preferably 80 to 100% by mass, still more preferably 90 to 100% by mass.
<16>如上述<11>至<15>中任一項之藍寶石板用研磨液組合物，其中上述面積比(b/a×100)之平均值較佳為110%以上，且較佳為200%以下，更佳為180%以下，進而較佳為150%以下，進而更佳為140%以下。 The polishing composition for sapphire sheets according to any one of the above-mentioned items, wherein the average ratio of the area ratio (b/a × 100) is preferably 110% or more, and preferably 200% or less, more preferably 180% or less, further preferably 150% or less, and still more preferably 140% or less.
<17>如上述<11>至<15>中任一項之藍寶石板用研磨液組合 物，其中上述面積比(b/a×100)之平均值較佳為110~200%，更佳為120~200%，進而較佳為130~200%，進而更佳為140~200%。 <17> A polishing liquid combination for a sapphire plate according to any one of the above <11> to <15> The average value of the above area ratio (b/a × 100) is preferably from 110 to 200%, more preferably from 120 to 200%, still more preferably from 130 to 200%, and still more preferably from 140 to 200%.
<18>一種藍寶石板之製造方法，其包括如下步驟：對被研磨藍寶石板供給如上述<1>至<17>中任一項之藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨。 <18> A method for producing a sapphire sheet, comprising the step of: supplying a polishing composition for a sapphire plate according to any one of the above <1> to <17> to a ground sapphire plate, and performing the above-described ground sapphire plate Grinding.
<19>一種藍寶石板之製造方法，其包括如下步驟：對被研磨藍寶石板供給如上述<1>至<17>中任一項之藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨；及使用上述步驟中使用之上述藍寶石板用研磨液組合物，對上述被研磨藍寶石板以外之被研磨藍寶石板進行研磨。 <19> A method for producing a sapphire plate, comprising the step of: supplying a polishing composition for a sapphire plate according to any one of the above <1> to <17> to a ground sapphire plate, and performing the above-described ground sapphire plate Grinding; and polishing the ground sapphire plate other than the ground sapphire plate by using the polishing composition for sapphire sheets used in the above step.
<20>一種被研磨藍寶石板之研磨方法，其包括如下步驟：對被研磨藍寶石板供給如上述<1>至<17>中任一項之藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨。 <20> A method of grinding a sapphire plate to be ground, comprising the step of supplying the sapphire plate sapphire composition according to any one of the above <1> to <17> to the ground sapphire plate The plate is ground.
<21>一種被研磨藍寶石板之研磨方法，其包括如下步驟：對被研磨藍寶石板供給如上述<1>至<17>中任一項之藍寶石板用研磨液組合物，對上述被研磨藍寶石板進行研磨；及使用上述步驟中使用之上述藍寶石板用研磨液組合物，對上述被研磨藍寶石板以外之被研磨藍寶石板進行研磨。 <21> A method of grinding a sapphire plate to be ground, comprising the step of supplying the sapphire plate sapphire composition according to any one of the above <1> to <17> to the ground sapphire plate The plate is subjected to polishing; and the ground sapphire plate other than the ground sapphire plate is ground using the polishing composition for sapphire plate used in the above step.
<22>一種藍寶石板用研磨液組合物之用途，其係用於被研磨藍寶石板之研磨，且該藍寶石板用研磨液組合物係如上述<1>至<17>中任一項之含有二氧化矽粒子、選自由正磷酸鹽、亞磷酸鹽、及次磷酸鹽所組成之群中之1種以上之無機磷酸鹽化合物及水系介質且25℃下之pH為8以上。 <22> A use of a polishing composition for a sapphire plate, which is used for polishing a ground sapphire plate, and the polishing composition for a sapphire plate is contained in any one of the above <1> to <17> The cerium oxide particles, one or more inorganic phosphate compounds selected from the group consisting of orthophosphates, phosphites, and hypophosphites, and an aqueous medium have a pH of 8 or more at 25 °C.
如下所述，製備實施例1~13、比較例1~9之研磨液組合物。實施例1~13、比較例1~9之研磨液組合物中之二氧化矽粒子、無機磷 酸鹽化合物或其比較對象化合物之含量分別係設為如表1所記載。剩餘之成分為離子交換水。 The polishing liquid compositions of Examples 1 to 13 and Comparative Examples 1 to 9 were prepared as described below. The cerium oxide particles and inorganic phosphorus in the polishing liquid compositions of Examples 1 to 13 and Comparative Examples 1 to 9 The content of the acid salt compound or the compound to be compared thereof is as shown in Table 1, respectively. The remaining component is ion exchange water.
[實施例1~5] [Examples 1 to 5]
<實施例1> <Example 1>
於裝有離子交換水858.47g之燒杯內，以磷酸氫二鈉之有效成分之濃度成為特定值之方式添加作為無機磷酸鹽化合物之磷酸氫二鈉12水合物(和光純藥工業(股)公司製造)0.25g後，添加40質量%膠體二氧化矽(日揮觸媒化成(股)製造，CATALOID SI-80P)水分散液(球狀二氧化矽粒子水分散液)141.0g並對該等進行攪拌，獲得添加有無機磷酸鹽之二氧化矽水分散液。其後，立刻使用以水將48質量%氫氧化鈉水溶液(關東化學公司製造)稀釋至0.1質量%而成之溶液0.28g作為pH調整劑，將25℃下之添加有無機磷酸鹽之二氧化矽水分散液之pH調整為10.5，獲得研磨液組合物。 Adding disodium hydrogen phosphate 12 hydrate as an inorganic phosphate compound to a specific value of the concentration of the active ingredient of disodium hydrogen phosphate in a beaker containing 858.47 g of ion-exchanged water (Wako Pure Chemical Industries Co., Ltd.) After 0.25 g of the product was added, 40% by mass of colloidal cerium oxide (manufactured by Nisko Catalyst Co., Ltd., CATALOID SI-80P) aqueous dispersion (spherical cerium oxide particle aqueous dispersion) was added and 141.0 g was added. Stirring was carried out to obtain an aqueous dispersion of cerium oxide added with an inorganic phosphate. Immediately thereafter, 0.28 g of a solution obtained by diluting a 48% by mass aqueous sodium hydroxide solution (manufactured by Kanto Chemical Co., Ltd.) with water to 0.1% by mass as a pH adjuster was used, and an inorganic phosphate-doped dioxide was added at 25 ° C. The pH of the hydrophobic dispersion was adjusted to 10.5 to obtain a slurry composition.
<實施例2~5> <Examples 2 to 5>
變更磷酸氫二鈉12水合物之添加量，除此以外，以與實施例1相同之方法獲得實施例2~5之研磨液組合物。 The polishing liquid compositions of Examples 2 to 5 were obtained in the same manner as in Example 1 except that the amount of addition of disodium hydrogen phosphate 12 hydrate was changed.
<實施例6> <Example 6>
準備以水將62.5%硫酸(Tayca製造)以成為0.1質量%之方式稀釋而成者作為pH調整劑，並使用該pH調整劑將研磨液組合物之25℃下之pH調整為9，除此以外，以與實施例4相同之方法獲得實施例6之研磨液組合物。 Prepared as a pH adjuster by diluting 62.5% of sulfuric acid (manufactured by Tayca) to 0.1% by mass in water, and adjusting the pH of the polishing composition at 25 ° C to 9 using the pH adjuster. The polishing liquid composition of Example 6 was obtained in the same manner as in Example 4 except for the same procedure as in Example 4.
<實施例7> <Example 7>
使用以水將48質量%氫氧化鈉水溶液(關東化學公司製造)稀釋至0.1質量%而成之溶液，將研磨液組合物之25℃下之pH調整為11.2，除此以外，以與實施例4相同之方法獲得實施例7之研磨液組合物。 A solution obtained by diluting a 48% by mass aqueous sodium hydroxide solution (manufactured by Kanto Chemical Co., Ltd.) with water to 0.1% by mass was used, and the pH of the polishing composition at 25 ° C was adjusted to 11.2, and the examples were 4 The same method was used to obtain the slurry composition of Example 7.
<實施例8> <Example 8>
使用亞磷酸鈉五水合物(和光純藥工業公司製造)作為無機磷酸鹽化合物(成分B)，且以研磨液組合物之25℃下之pH成為表1所記載之值之方式調整pH調整劑之使用量，除此以外，以與實施例4相同之方法獲得實施例8之研磨液組合物。 Sodium phosphite pentahydrate (manufactured by Wako Pure Chemical Industries, Ltd.) was used as the inorganic phosphate compound (ingredient B), and the pH adjuster was adjusted so that the pH of the polishing composition at 25 ° C became the value described in Table 1. A polishing liquid composition of Example 8 was obtained in the same manner as in Example 4 except for the amount used.
<實施例9> <Example 9>
使用次磷酸鈉一水合物(米山化學工業公司製造)作為無機磷酸鹽化合物(成分B)，且以研磨液組合物之25℃下之pH成為表1所記載之值之方式調整pH調整劑之使用量，除此以外，以與實施例4相同之方法獲得實施例9之研磨液組合物。 Sodium hypophosphite monohydrate (manufactured by Mishan Chemical Industry Co., Ltd.) was used as the inorganic phosphate compound (ingredient B), and the pH adjusting agent was adjusted so that the pH of the polishing composition at 25 ° C became the value described in Table 1. The polishing liquid composition of Example 9 was obtained in the same manner as in Example 4 except for the amount used.
<實施例10> <Example 10>
使用磷酸氫二鉀(和光純藥工業公司製造)作為無機磷酸鹽化合物(成分B)，且以研磨液組合物之25℃下之pH成為表1所記載之值之方式調整pH調整劑之使用量，除此以外，以與實施例4相同之方法獲得實施例10之研磨液組合物。 The use of dipotassium hydrogen phosphate (manufactured by Wako Pure Chemical Industries, Ltd.) as an inorganic phosphate compound (ingredient B), and adjustment of the pH adjusting agent in such a manner that the pH of the polishing composition at 25 ° C became the value described in Table 1 The polishing liquid composition of Example 10 was obtained in the same manner as in Example 4 except for the amount.
<實施例11> <Example 11>
使用磷酸氫二銨(和光純藥工業公司製造)作為無機磷酸鹽化合物(成分B)，且以研磨液組合物之25℃下之pH成為表1所記載之值之方式調整pH調整劑之使用量，除此以外，以與實施例4相同之方法獲得實施例11之研磨液組合物。 The use of diammonium hydrogen phosphate (manufactured by Wako Pure Chemical Industries, Ltd.) as an inorganic phosphate compound (ingredient B), and adjustment of the pH adjusting agent in such a manner that the pH of the polishing composition at 25 ° C became the value described in Table 1 The polishing liquid composition of Example 11 was obtained in the same manner as in Example 4 except for the amount.
<實施例12> <Example 12>
使用次磷酸銨(富山藥品工業公司製造)作為無機磷酸鹽化合物(成分B)，且以研磨液組合物之25℃下之pH成為表1所記載之值之方式調整pH調整劑之使用量，除此以外，以與實施例4相同之方法獲得實施例12之研磨液組合物。 The ammonium phosphate (manufactured by Toyama Pharmaceutical Co., Ltd.) was used as the inorganic phosphate compound (component B), and the amount of the pH adjuster was adjusted so that the pH of the polishing composition at 25 ° C became the value described in Table 1. A polishing liquid composition of Example 12 was obtained in the same manner as in Example 4 except the above.
<實施例13> <Example 13>
使用異形二氧化矽粒子水分散液代替球狀二氧化矽粒子水分散 液，除此以外，以與實施例8相同之方法獲得實施例13之研磨液組合物。再者，異形二氧化矽粒子之平均絕對最大長度為122.6nm，面積比(b/a×100)之平均值為137.4%，面積比(b/a×100)為110~200%之二氧化矽粒子相對於所有二氧化矽粒子之比率為93.2質量%。 Replace the spherical cerium oxide particle water dispersion with the dissimilar cerium oxide particle aqueous dispersion A polishing liquid composition of Example 13 was obtained in the same manner as in Example 8 except for the liquid. Furthermore, the average absolute maximum length of the shaped cerium oxide particles is 122.6 nm, the average of the area ratio (b/a×100) is 137.4%, and the area ratio (b/a×100) is 110-200%. The ratio of the cerium particles to all of the cerium oxide particles was 93.2% by mass.
<比較例1> <Comparative Example 1>
不使用磷酸氫二鈉，且以研磨液組合物之25℃下之pH成為表1所記載之值之方式調整pH調整劑之使用量，除此以外，以與實施例4相同之方法獲得比較例1之研磨液組合物。 A comparison was made in the same manner as in Example 4 except that disodium hydrogen phosphate was not used and the pH adjustment agent was adjusted so that the pH of the polishing composition at 25 ° C became the value described in Table 1. The slurry composition of Example 1.
<比較例2~5> <Comparative Examples 2 to 5>
使用表1所記載之比較對象化合物代替磷酸氫二鈉，且以研磨液組合物之25℃下之pH成為表1所記載之值之方式調整pH調整劑之使用量，除此以外，以與實施例4相同之方法分別獲得比較例2~5之研磨液組合物。 The comparative target compound described in Table 1 was used instead of disodium hydrogen phosphate, and the pH adjustment agent was adjusted so that the pH of the polishing composition at 25 ° C became the value described in Table 1, and In the same manner as in Example 4, the polishing liquid compositions of Comparative Examples 2 to 5 were respectively obtained.
<比較例6> <Comparative Example 6>
使用62.5%硫酸(Tayca製造)作為pH調整劑，將研磨液組合物之25℃下之pH調整為2，除此以外，以與實施例4相同之方法獲得比較例6之研磨液組合物。 A polishing liquid composition of Comparative Example 6 was obtained in the same manner as in Example 4 except that 62.5% sulfuric acid (manufactured by Tayca) was used as the pH adjuster and the pH of the polishing composition at 25 ° C was adjusted to 2.
<比較例7> <Comparative Example 7>
使用62.5%硫酸(Tayca製造)作為pH調整劑，將研磨液組合物之25℃下之pH調整為7，除此以外，以與實施例4相同之方法獲得比較例7之研磨液組合物。 A polishing liquid composition of Comparative Example 7 was obtained in the same manner as in Example 4 except that 62.5% sulfuric acid (manufactured by Tayca) was used as the pH adjuster and the pH of the polishing composition at 25 ° C was adjusted to 7.
<比較例8> <Comparative Example 8>
不使用無機磷酸(鹽)化合物，除此以外，以與實施例13相同之方法獲得比較例8之研磨液組合物。 The polishing liquid composition of Comparative Example 8 was obtained in the same manner as in Example 13 except that the inorganic phosphoric acid (salt) compound was not used.
<比較例9> <Comparative Example 9>
於裝有離子交換水之燒杯內，以磷酸氫二鈉之有效成分之濃度 成為特定值之方式添加作為無機磷酸鹽化合物之磷酸氫二鈉12水合物(和光純藥工業(股)公司製造)2.59g後，添加45質量%氧化鋁粒子(平均二次粒徑0.8μm、α化率90%、微晶尺寸32nm)水分散液455.56g並對該等進行攪拌，獲得添加有無機磷酸鹽之氧化鋁粒子水分散液。其後，立刻使用以水將48質量%氫氧化鈉水溶液(關東化學公司製造)稀釋至0.1%而成之溶液0.17g作為pH調整劑，將25℃下之添加有無機磷酸鹽之氧化鋁粒子水分散液之pH調整為10.5，獲得研磨液組合物。 Concentration of active ingredient of disodium hydrogen phosphate in a beaker containing ion-exchanged water Addition of 2.59 g of disodium hydrogen phosphate 12 hydrate (manufactured by Wako Pure Chemical Industries, Ltd.) as an inorganic phosphate compound, and adding 45 mass% of alumina particles (average secondary particle diameter of 0.8 μm, 455.56 g of an aqueous dispersion was obtained by agitation rate of 90% and a crystallite size of 32 nm), and the aqueous dispersion of the alumina particle to which the inorganic phosphate was added was obtained. Immediately thereafter, 0.17 g of a solution obtained by diluting a 48% by mass aqueous sodium hydroxide solution (manufactured by Kanto Chemical Co., Ltd.) to 0.1% with water as a pH adjuster was used, and an inorganic phosphate-added alumina particle at 25 ° C was added. The pH of the aqueous dispersion was adjusted to 10.5 to obtain a slurry composition.
[氧化鋁粒子之體積平均粒徑(D50)之測定方法] [Method for Measuring Volume Average Particle Diameter (D50) of Alumina Particles]
關於比較例9之研磨液組合物中之氧化鋁粒子(研磨粒)之體積平均粒徑(平均二次粒徑)，將0.5%POIZ530(花王公司製造；特殊多羧酸型高分子界面活性劑)水溶液作為分散介質，將該分散介質投入下述測定裝置內，繼而以透過率成為75~95%之方式投入樣本(氧化鋁粒子)，其後施加5分鐘超音波後測定粒徑。 Regarding the volume average particle diameter (average secondary particle diameter) of the alumina particles (abrasive grains) in the polishing liquid composition of Comparative Example 9, 0.5% POIZ530 (manufactured by Kao Corporation; special polycarboxylic acid type polymer surfactant) The aqueous solution was used as a dispersion medium, and the dispersion medium was placed in a measuring apparatus described below, and then a sample (alumina particles) was introduced so that the transmittance was 75 to 95%, and then ultrasonic waves were applied for 5 minutes, and then the particle diameter was measured.
測定機器：堀場製作所製造，雷射繞射/散射式粒度分佈測定裝置LA920 Measuring machine: manufactured by Horiba, Ltd., laser diffraction/scattering particle size distribution measuring device LA920
循環強度：4 Cycle strength: 4
超音波強度：4 Ultrasonic intensity: 4
將所獲得之體積分佈粒徑之累積體積頻度成為50%之粒徑作為氧化鋁粒子之體積平均粒徑(D50)。 The particle size at which the cumulative volume frequency of the obtained volume distribution particle diameter is 50% is taken as the volume average particle diameter (D50) of the alumina particles.
[氧化鋁粒子之α化率及微晶尺寸之測定方法] [Method for Measuring the Gelation Rate and Crystallite Size of Alumina Particles]
使氧化鋁漿料20g於105℃下乾燥5小時，利用研缽將所獲得之乾燥物解碎而獲得粉末x射線繞射用樣本。利用粉末X射線繞射法對各樣本進行分析，將104面中之峰面積與α化率99.9%之α-氧化鋁(昭和電工公司製造，WA-1000)之峰面積進行比較。粉末X射線繞射法之測定條件如下所述。 20 g of the alumina slurry was dried at 105 ° C for 5 hours, and the obtained dried product was pulverized with a mortar to obtain a sample for powder x-ray diffraction. Each sample was analyzed by a powder X-ray diffraction method, and the peak area in the 104 plane was compared with the peak area of α-alumina (manufactured by Showa Denko KK, WA-1000) having a gelation rate of 99.9%. The measurement conditions of the powder X-ray diffraction method are as follows.
測定條件： Determination conditions:
裝置：(股)Rigaku製造，粉末X射線分析裝置RINT2500VC Device: (share) Rigaku manufacture, powder X-ray analysis device RINT2500VC
X射線產生電壓：40kV X-ray generation voltage: 40kV
放射線：Cu-Kα1線(λ=0.154050nm) Radiation: Cu-Kα1 line (λ = 0.154050 nm)
電流：120mA Current: 120mA
Scan Speed(掃描速度)：10度/分鐘 Scan Speed: 10 degrees / minute
測定步進：0.02度/分鐘 Measuring step: 0.02 degrees / minute
α化率(%)=α氧化鋁特有峰面積÷WA-1000之峰面積×100 Alphaization rate (%) = alpha alumina specific peak area ÷ WA-1000 peak area × 100
又，微晶尺寸係根據所獲得之粉末X射線繞射光譜，使用粉末X射線繞射裝置所附帶之粉末X射線繞射圖案綜合分析軟體JADE(MDI公司，基於謝樂之式之自動計算)而算出。利用上述軟體之算出處理係基於上述軟體之操作說明書(Jade(Ver.5)軟體、操作說明書Manual No.MJ13133E02、理學電機股份有限公司)而進行。 Further, the crystallite size is calculated based on the obtained powder X-ray diffraction spectrum using the powder X-ray diffraction pattern comprehensive analysis software JADE (MDI, based on Xie Le's formula) attached to the powder X-ray diffraction device. . The calculation processing by the above-described software is performed based on the above-described software operation manual (Jade (Ver. 5) software, operation manual Manual No. MJ13133E02, and Science Machinery Co., Ltd.).
<二氧化矽粒子之平均一次粒徑之測定> <Measurement of average primary particle size of cerium oxide particles>
二氧化矽粒子之平均一次粒徑如下所述，係以於電子顯微鏡(TEM)觀察圖像中所測定之圓當量徑之形式求出之粒徑的數量平均。利用掃描儀將利用日本電子製造之透射型電子顯微鏡(TEM)(商品名「JEM-2000FX」，80kV，1~5萬倍)對二氧化矽粒子進行觀察而得之照片以圖像資料之形式輸入電腦，使用分析軟體「WinROOF(Ver.3.6)」(銷售商：三谷商事)對1000~2000個二氧化矽粒子資料求出一個一個二氧化矽粒子之以圓當量徑之形式求出之粒徑，藉由數量平均而求出平均一次粒徑。 The average primary particle diameter of the cerium oxide particles is as follows, and is the number average of the particle diameters obtained as a circle-equivalent diameter measured in an electron microscope (TEM) observation image. A photograph of the cerium oxide particles observed by a transmission electron microscope (TEM) (trade name "JEM-2000FX", 80 kV, 10,000 to 50,000 times) manufactured by JEOL was carried out in the form of image data by a scanner. Enter the computer and use the analysis software "WinROOF (Ver.3.6)" (seller: Mitani Corporation) to find the particles of a cerium oxide particle in the form of a circle equivalent diameter for 1000 to 2000 cerium oxide particles. The average diameter of the primary diameter was determined by the number average.
[二氧化矽粒子之平均二次粒徑之測定] [Determination of average secondary particle size of cerium oxide particles]
比較例1之研磨液組合物中之膠體二氧化矽(研磨粒)之平均二次粒徑(分散粒徑)係使用動態光散射(DLS)粒度分佈計(Malvern公司製造，Zetasizer Nano S)於下述條件下進行測定，求出所獲得之體積換算平均粒徑作為平均二次粒徑(分散粒徑)。 The average secondary particle diameter (dispersion particle diameter) of the colloidal cerium oxide (abrasive particles) in the polishing composition of Comparative Example 1 was measured by a dynamic light scattering (DLS) particle size distribution meter (manufactured by Malvern, Zetasizer Nano S). The measurement was performed under the following conditions, and the obtained volume-converted average particle diameter was determined as an average secondary particle diameter (dispersion particle diameter).
溶劑：水(折射率1.333) Solvent: water (refractive index 1.333)
研磨粒：膠體二氧化矽(折射率1.45，衰減係數0.02) Abrasive grain: colloidal cerium oxide (refractive index 1.45, attenuation coefficient 0.02)
測定溫度：25℃ Measuring temperature: 25 ° C
[二氧化矽粒子之BET比表面積之測定] [Determination of BET specific surface area of cerium oxide particles]
關於二氧化矽粒子之比表面積，對於在100℃下乾燥24小時之粉末樣本，以小數點以後4位數精確稱量測定樣本約0.1g至測定池中，於即將進行比表面積之測定之前於200℃之環境下乾燥30分鐘，然後使用比表面積測定裝置(Micromeritic自動比表面積測定裝置Flowsorb III2305，島津製作所製造)藉由氮吸附法(BET法)進行測定。實施例1~13、比較例1~7之研磨液組合物之製備所使用之二氧化矽粒子之BET比表面積為40m2/g。 Regarding the specific surface area of the cerium oxide particles, for the powder sample dried at 100 ° C for 24 hours, about 0.1 g of the sample is accurately weighed by 4 digits after the decimal point into the measuring cell, immediately before the measurement of the specific surface area. The mixture was dried in an environment of 200 ° C for 30 minutes, and then measured by a nitrogen adsorption method (BET method) using a specific surface area measuring device (Micromeritic automatic specific surface area measuring device Flowsorb III2305, manufactured by Shimadzu Corporation). The cerium oxide particles used in the preparation of the polishing composition of Examples 1 to 13 and Comparative Examples 1 to 7 had a BET specific surface area of 40 m 2 /g.
[二氧化矽粒子之平均絕對最大長度及面積比(b/a×100)之平均值] [Average absolute maximum length and area ratio of cerium oxide particles (b/a × 100)]
利用掃描儀將利用日本電子製造之透射型電子顯微鏡(TEM)(商品名「JEM-2000FX」，80kV，1~5萬倍)對二氧化矽粒子進行觀察而得之照片以圖像資料之形式輸入至電腦，使用分析軟體「WinROOF(Ver.3.6)」(銷售商：三谷商事)對1000~2000個二氧化矽粒子資料求出一個一個二氧化矽粒子之絕對最大長度，獲得絕對最大長度之平均值(平均絕對最大長度)。將以絕對最大長度為直徑之圓之面積b除以由電子顯微鏡觀察而獲得之該粒子之投影面積a並乘以100，算出面積比(b/a×100)(%)。又，算出面積比(b/a×100)為110~200%之二氧化矽粒子相對於所有二氧化矽粒子之比率。進而，算出平均絕對最大長度之圓面積b除以上述投影面積a之平均值並乘以100所得之值作為面積比(b/a×100)之平均值。 A photograph of the cerium oxide particles observed by a transmission electron microscope (TEM) (trade name "JEM-2000FX", 80 kV, 10,000 to 50,000 times) manufactured by JEOL was carried out in the form of image data by a scanner. Enter the computer and use the analysis software "WinROOF (Ver.3.6)" (seller: Mitani Corporation) to calculate the absolute maximum length of one cerium oxide particle from 1000 to 2000 cerium oxide particles, and obtain the absolute maximum length. Average (average absolute maximum length). The area b of the circle having the absolute maximum length as the diameter was divided by the projected area a of the particle obtained by observation with an electron microscope and multiplied by 100, and the area ratio (b/a × 100) (%) was calculated. Further, the ratio of the cerium oxide particles having an area ratio (b/a × 100) of 110 to 200% with respect to all of the cerium oxide particles was calculated. Further, a value obtained by dividing the circle area b of the average absolute maximum length by the average value of the projected area a and multiplying by 100 is calculated as the average value of the area ratio (b/a × 100).
<研磨液組合物之pH測定> <Measurement of pH of polishing liquid composition>
使用pH計(東亞電波工業公司製造，HM-30G)於25℃下測定研磨液組合物之pH。 The pH of the polishing composition was measured at 25 ° C using a pH meter (manufactured by Toa Telecommunications Co., Ltd., HM-30G).
<研磨評價> <grinding evaluation>
於下述研磨條件下使用實施例1~13、比較例1~9之研磨液組合物對3吋之藍寶石板(c面)進行3小時循環研磨。繼而，求出藍寶石板之研磨前後之重量變化，根據藍寶石密度(3.98g/cm3)、藍寶石板面積(45.6c m2)算出研磨速度(μm/h)。使用實施例1~13、比較例1~9之研磨液組合物之情形時之研磨速度係以將使用比較例1之研磨液組合物之情形時之研磨速度設為「100」之情形時之相對值示於表1。 The sapphire plate (c surface) of 3 Å was subjected to cycle polishing for 3 hours under the following polishing conditions using the polishing composition of Examples 1 to 13 and Comparative Examples 1 to 9. Then, the weight change before and after polishing of the sapphire plate was determined, and the polishing rate (μm/h) was calculated from the sapphire density (3.98 g/cm 3 ) and the sapphire plate area (45.6 cm 2 ). When the polishing liquid compositions of Examples 1 to 13 and Comparative Examples 1 to 9 were used, the polishing rate was set to "100" when the polishing liquid composition of Comparative Example 1 was used. The relative values are shown in Table 1.
(研磨條件) (grinding conditions)
單面研磨機(Techno Rise製造之TR15M-TRK1，壓盤直徑38cm) Single-side grinding machine (TR15M-TRK1 manufactured by Techno Rise, pressure plate diameter 38cm)
不織布研磨墊(Nitta Haas製造之SUBA800) Non-woven abrasive pad (SUBA800 by Nitta Haas)
研磨負載300g/cm2 Grinding load 300g/cm 2
壓盤轉速120rpm Platen speed 120rpm
載體轉速120rpm Carrier speed 120rpm
研磨液流量80mL/min(循環) Grinding fluid flow rate 80mL/min (cycle)
[表面粗糙度之測定方法] [Method for measuring surface roughness]
使用AFM(Atomic Force Microscopy，原子力顯微鏡)(Digital Instrument NanoScope IIIa Multi Mode AFM)於以下所示之條件下對洗淨後之藍寶石板於正反面之各1個部位測定內周緣與外周緣之中央部分，測定中心線平均粗糙度AFM-Ra。將2點之平均值作為「表面粗糙度」示於表1。值越小表示越抑制表面粗糙度之惡化。 The center portion of the inner circumference and the outer circumference of each of the front and back surfaces of the washed sapphire plate was measured using an AFM (Atomic Force Microscopy, Atomic Force Microscope) (Digital Instrument NanoScope IIIa Multi Mode AFM) under the conditions shown below. , the center line average roughness AFM-Ra was measured. The average value of the two points is shown in Table 1 as "surface roughness". The smaller the value, the more the deterioration of the surface roughness is suppressed.
〔AFM之測定條件〕 [Measurement conditions of AFM]
Mode(模式)：Tapping mode(間歇接觸式) Mode: Tapping mode (intermittent contact)
Area(面積)：5×5μm Area: 5 × 5 μm
Scan rate(掃描速率)：1.0Hz Scan rate: 1.0Hz
Cantilever(懸臂)：OMCL-AC160TS-C3 Cantilever (cantilever): OMCL-AC160TS-C3
Line(線)：512×512 Line (line): 512 × 512
如表1所示，於使用實施例之研磨液組合物之情形時，與使用比較例之研磨液組合物之情形相比，更能同時實現高速研磨與低表面粗糙度。 As shown in Table 1, in the case of using the polishing liquid composition of the example, high-speed polishing and low surface roughness were more simultaneously achieved than in the case of using the polishing liquid composition of the comparative example.
如以上所說明般，於使用本發明之研磨液組合物之被研磨藍寶石板之研磨中，研磨速度較快，且研磨後之藍寶石板可確保良好之表面平滑性。因此，只要使用本發明之研磨液組合物，則例如LED之製造或智慧型手機等移動終端裝置之覆蓋玻璃之製造所使用之藍寶石板等之生產性提高。 As described above, in the polishing of the ground sapphire plate using the polishing composition of the present invention, the polishing speed is fast, and the polished sapphire plate ensures good surface smoothness. Therefore, as long as the polishing liquid composition of the present invention is used, the productivity of a sapphire board or the like used for the manufacture of a cover glass of a mobile terminal device such as an LED or a smart phone is improved.
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| JP6846193B2 (en) * | 2016-12-26 | 2021-03-24 | ニッタ・デュポン株式会社 | Polishing slurry |
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| US20060196849A1 (en) * | 2005-03-04 | 2006-09-07 | Kevin Moeggenborg | Composition and method for polishing a sapphire surface |
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| JP5940754B1 (en) | 2016-06-29 |
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